Note: Descriptions are shown in the official language in which they were submitted.
1
HAIR-MENDING COMPOSITIONS AND ASSOCIATED METHODS
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This patent application claims the benefit of U.S. Provisional
Patent Application
No. 61/394,966, filed October 20, 2010 and International Application No.
PCT/US10/53360,
filed October 20, 2010.
BACKGROUND OF THE INVENTION
[0002] Hair care compositions are often formulated to have multiple
properties. For
example, a hair conditioner may be formulated to condition hair and also may
be formulated
to repair hair. Hair care compositions with multiple properties are attractive
to a consumer in
that fewer compositions need be applied to the hair to achieve a desired
effect. However, to
formulate such a hair care composition, multiple ingredients are often
necessary. As the
number of ingredients increases, the complexity of the composition increases.
The long term
stability of such a composition can become compromised due to
incompatibilities among the
many ingredients.
[0003] Furthermore, due to the large number of ingredients in many hair
care
compositions, formulators are not only faced with the challenges of finding
the proper
ingredients to provide the desired cosmetic properties but are also faced with
the challenge of
manufacturing these complicated compositions. Such challenges include
developing
production protocols to produce a composition both on a small scale for
initial testing and on
a large scale for commercial marketing. A greater number of ingredients may
translate into a
greater number of manufacturing containers required, which itself translates
into more time
and expense to produce the composition. Cosmetic compositions thus are
complicated
mixtures of ingredients, and with such complexity, require careful
consideration when
developing production protocols.
[0004] Hair care composition ingredients include conditioning agents,
which are often
positively charged compounds. Hair fibers have a net negative charge. The
positive charge
of the conditioning agents is attracted to the overall negative charge of the
hair fibers, making
the positively charged conditioning agents substantive to the hair. This
substantive nature
allows the conditioning agent to interact with the hair in order for the
conditioning agent to
provide its conditioning effect. The conditioning effect can include restoring
the hair fiber
CA 2812991 2017-11-27
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
2
after damage to the hair, such as repairing split-ends.
[00051 Conditioning agents known in the art include quaternary ammonium
nitrogen
compounds, known as "quats," and polymers comprising moieties of such
compounds,
known as "polyquats." The polyquats include polyquaternium-28, a
vinylpyrrolidone/methacrylamidopropyl trimethylammonium chloride copolymer. It
has
been found that the combination of polyquat-28 and methylvinylether/maleie
acid copolymer
(PVMMA) at particular ratios produces a polyelectrolyte complex (PEC) that
repairs split-
end damage (U.S. Patent Application Publication Nos. 2005/0089494 and
2006/0251603,
both assigned to ISP Investments Inc.). However, within the context of
complicated hair care
formulations, the stability of PECs may be compromised due to the presence of
other
ingredients, especially charged compounds and polymers that could disrupt the
PEC
structure. Thus, the usefulness of PECs may be limited by their compatibility
with other
ingredients that may be desirable to include in a hair care composition. Since
multiple
properties are often desired in hair care compositions, it would be desirable
to formulate hair
care compositions that include stable combinations of PECs with other hair
care ingredients
that provide additional desirable properties.
[0006] Also, although PVMMA:polyquat-28 PECs consist of only two component
ingredients, the method of producing these PECs is described in the ISP
Investments
applications as comprising two or three separate containers. Such a method is
cumbersome,
especially in view of any additional containers required to incorporate
additional ingredients.
The dedication of two or three containers in a large-scale production facility
for the making
of one complex is inefficient and costly.
[0007] Additionally, when a consumer purchases hair care products, the
consumer does
so based on the properties of the hair care product. For example, a consumer
with frizzy hair
may purchase a product to de-frizz the hair, and a consumer with split-ends
may purchase a
product to repair the split-ends. Thus, consumers may purchase hair care
products having
properties desirable for a particular hair type or hair problem. In order for
consumers to
compare hair care product compositions to make a decision regarding which to
purchase, the
beneficial properties of the compositions should be clearly communicated to
the consumers.
One method is to use still photography, such as described in the ISP
Investments applications.
However, additional methods arc needed.
[0008] It would therefore be desirable to formulate a stable hair care
composition that
includes intact PECs in combination with other hair benefit agents, especially
charged hair
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
3
benefit agents. Also, there is a need for a more efficient process for making
PECs and hair
care compositions containing PECs. Further, there is a need for the
development of test
methods that can show improved results of split-end mending of a hair care
composition such
that the benefits of the hair care composition can then be effectively
communicated to
consumers. There also is a need for the development of additional methods that
can show the
benefits of a hair care composition such that the benefits can then be
effectively
communicated to consumers. The present invention provides these advantages.
Additional
advantages of the invention, as well as additional inventive features, will be
apparent from
the description of the invention provided herein.
BRIEF SUMMARY OF THE INVENTION
[0009] In one aspect, the present invention provides a hair care
composition comprising a
polyelectrolyte complex of a cationic polymer and an anionic polymer in the
form of an
emulsion with improved freeze-thaw stability relative to comparative
compositions
containing such polyelectrolyte complexes.
[0010] In another aspect, the present invention provides a hair care
composition
comprising a polyelectrolyte complex of a cationic polymer and an anionic
polymer, wherein
the viscosity of the composition is greater than 3000 cps.
[0011] In another aspect, the present invention provides a hair care
composition
comprising a polyelectrolyte complex of a cationic polymer and an anionic
polymer; from
about 1% to about 5% of a thickening agent; about 10% or greater of propylene
glycol; and
about 5% or greater of an emollient; wherein the percentages are based on the
total weight of
the composition.
100121 In yet another aspect, the present invention provides a hair care
composition
comprising a polyelectrolyte complex of a cationic polymer and an anionic
polymer; from
about 3% to about 5% of a thickening agent; and about 2% or less of an
emollient; wherein
the percentages are based on the total weight of the composition.
[0013] The present invention also provides methods of using the
compositions described
herein, including a method of conditioning a hair fiber and a method of
repairing a split-end
of a hair fiber.
[0014] Furthermore, the present invention provides a method for improving
the freeze-
thaw stability of a hair care composition comprising a polyelectrolyte complex
of a cationic
polymer and an anionic polymer, the method comprising adding to the hair care
composition
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
4
from about 1% to about 5% of a thickening agent, wherein the percentage is
based on the
total weight of the composition.
[0015] Additionally, the present invention provides a method for improving
the freeze-
thaw stability of a hair care composition comprising a polyelectrolyte
complex, the method
comprising adding to the hair care composition from about 10% or greater of
propylene
glycol, wherein the percentage is based on the total weight of the
composition.
[0016] The present invention also provides a method for thermally
protecting hair by
applying to the hair compositions as described herein.
[0017] Furthermore, an aspect of the present invention provides a method of
producing a
polyelectrolyte complex, the method comprising hydrating a
methylvinylethcr/maleic acid
copolymer having repeating units of the formula (Formula I)
iCH3
so
ICH2¨CH¨p-1H
OH OH
in a container; reacting the methylvinylether/maleic acid copolymer with a
base, in the
container in an amount sufficient to at least partially neutralize the acidic
groups thereof, to
form an intermediate mixture; heating the intermediate mixture in the
container; adding to the
intermediate mixture in the container a cationic copolymer of a
vinylpyrrolidone of the
formula (Formula H)
¨c14177H.
and a methacrylamidopropyl trimethylammonium chloride of the formula (Formula
III)
043,
¨CH2¨ c _____________________________
NH
(GN'S
Cr
CHa
; and
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
mixing the polymers in the container at high shear force and at a temperature
of at least about
50-60 C to produce the polyelectrolytc complex.
[0018] The present invention also provides a method of producing a
polyelectrolyte
complex, the method comprising hydrating a methylvinylether/maleic acid
copolymer having
repeating units of the formula Tin a container; reacting the
methylvinylether/maleic acid
copolymer with, e.g., a 20% sodium hydroxide solution in the container,
wherein the sodium
hydroxide is added in an amount sufficient to achieve a pH of, e.g., from
about 6.5 to about
7.5 or from about 6.9 to about 7.0, to form an intermediate mixture; heating
the intermediate
mixture in the container to a temperature of from about 50 C to about 60 C;
adding to the
intermediate mixture in the container a cationic copolymer of a
vinylpyrrolidone of the
formula II and a methacrylamidopropyl trimethylammonium chloride of the
foimula III; and
mixing the polymers in the container for at least about 10 minutes at high
shear force and at a
temperature of at least about 50-60 C to produce the polyelectrolyte complex.
In an
embodiment, the method further comprises the step of mixing the
polyelectrolyte complex
with one or more components selected from aqueous carriers, surfactants,
fragrances,
conditioning agents, emollients, emulsifiers, thickening agents,
preservatives, gelling agents,
silicones, hair fixatives, humectants and moisturizers to form a hair care
composition. In an
embodiment, the mixing is sufficient to allow adequate incorporation of the
one or more
components.
[0019] The present invention also provides a method of producing a hair
care
composition comprising producing a polyelectrolyte complex, comprising the
steps of
hydrating a methylvinylether/maleic acid copolymer having repeating units of
the formula I
in a container; reacting the methylvinylether/maleic acid copolymer with a
base, such as, e.g.,
20% sodium hydroxide, in the container in an amount sufficient to at least
partially neutralize
the acidic groups thereof, e.g., wherein the sodium hydroxide is added in an
amount sufficient
to achieve a pH of, e.g., from about 6.5 to about 7.5 or from about 6.9 to
about 7.0, to form an
intermediate mixture; heating the intermediate mixture in the container, e.g.,
to a temperature
of from about 50 C to about 60 C; adding to the intermediate mixture in the
container a
cationic copolymer of a vinylpyrrolidone of the formula II and a
methacrylamidopropyl
trimethylammonium chloride of the thimula Ill; mixing the polymers in the
container at high
shear force and at a temperature of at least about 50-60 C to produce the
polyelectrolyte
complex; adding to the polyelectrolyte complex in the container one or more
additional
components selected from aqueous carriers, surfactants, fragrances,
conditioning agents,
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
6
emollients, emulsifiers, thickening agents, preservatives, gelling agents,
silicones, hair
fixatives, humectants and moisturizers; and mixing the resulting composition
in the container.
In an embodiment, the method produces a hair care composition in the form of a
shampoo,
conditioner, leave-in treatment, creme, gel, mousse, serum, oil treatment,
glaze, or spray.
[0020] The present invention also provides a method of producing a hair
care
composition comprising producing a polyelectrolyte complex between a
methylvinylether/maleic acid copolymer and a cationic copolymer of a
vinylpyrrolidone and
a methacrylamidopropyl trimethylammonium chloride, comprising the steps of
hydrating a
methylvinylether/malcic acid copolymer having repeating units of the formula I
in a first
container; reacting the methylvinylether/maleic acid copolymer with a base,
such as, e.g.,
20% sodium hydroxide, in the first container in an amount sufficient to at
least partially
neutralize the acidic groups thereof, e.g., wherein the sodium hydroxide is
added in an
amount sufficient to achieve a pH of, e.g., from about 6.5 to about 7.5 or
from about 6.9 to
about 7.0, to form an intermediate mixture; heating the inteimediatc mixture
in the first
container, e.g., to a temperature of from about 50 C to about 60 C; adding
to the
intermediate mixture in the first container a cationic copolymer of a
vinylpyrrolidone of the
formula II and a methacrylamidopropyl trimethylammonium chloride of the
formula III;
mixing the polymers in the first container at high shear force and at a
temperature of at least
about 50-60 C to produce the polyelectrolyte complex; mixing in a second
container one or
more components selected from aqueous carriers, surfactants, fragrances,
conditioning
agents, emollients, emulsifiers, thickening agents, preservatives, gelling
agents, silicones, hair
fixatives, humectants and moisturizers; and mixing together in the first or
second container
the polyelectrolyte complex of the first container and the mixed components of
the second
container. In an embodiment, the method produces a hair care composition in
the form of a
shampoo, conditioner, leave-in treatment, crème, gel, mousse, or spray.
[0021] Furthermore, the present invention provides a method of graphically
reconstructing a repair of a split-end of a hair fiber, the method comprising
securing a hair
fiber to a surface, wherein the hair fiber secured to the surface has a split-
end or is damaged
while on the surface to produce a split-end; associating the surface with a
magnifying device,
wherein the split-end is positioned within the field of view of the magnifying
device;
associating an image capture device with the magnifying device so as to
capture an enlarged
image of the field of view of the magnifying device; treating the split-end
with a composition,
wherein the composition repairs the split-end and wherein the split-end fuses
together; and
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
7
via the image capture device associated with the magnifying device, capturing
an image of
the repair of the split-end during treatment with the composition, and storing
a representation
of the captured image of the repair for subsequent retrieval. In an
embodiment, the
composition comprises, e.g., from about 1% to about 5% of a thickening agent,
about 10% or
greater of propylene glycol, and about 5% or greater of an emollient, wherein
the percentages
are based on the total weight of the composition. In another embodiment, the
composition
comprises from about 3% to about 5% of a thickening agent, and about 2% or
less of an
emollient, wherein the percentages are based on the total weight of the
composition. In
another embodiment, the degree of split-end hair fiber repair is communicated
to consumers.
[0022] The present invention also provides a method of quantitatively
assessing the
degree of split-end hair fiber repair, the method comprising obtaining a tress
of hair, wherein
the hair is twice-bleached hair; combing and blow drying the tress of hair to
produce at least
one split-end in at least one hair fiber; removing at least one hair fiber
having a split-end from
the tress; optionally marking the at least one hair fiber; capturing a first
image of the split-end
of the at least one hair fiber and storing a representation, e.g., an
electronic representation, of
the image; associating the hair fiber with the tress from which the hair fiber
was removed;
treating the tress and the hair fiber with a composition; removing the hair
fiber from the
treated tress; capturing a second image of the end of the hair fiber removed
from the treated
tress; assigning a value of 0 for no repair of the split-end, 1/2 for partial
repair, or 1 for
complete repair with respect to the hair fiber to assess the degree of split-
end repair of the
hair fiber; and if more than one hair fiber is assessed, optionally
determining an average value
with respect to the assessed hair fibers. In an embodiment, the composition
comprises, e.g.,
from about 1% to about 5% of a thickening agent, about 10% or greater of
propylene glycol,
and about 5% or greater of an emollient, wherein the percentages are based on
the total
weight of the composition. In another embodiment, the composition comprises
from about
3% to about 5% of a thickening agent, and about 2% or less of an emollient,
wherein the
percentages are based on the total weight of the composition. In another
embodiment, the
degree of split-end hair fiber repair is communicated to consumers.
[0023] One embodiment of the present invention provides a method of
quantitatively
assessing the degree of split-end hair fiber repair, the method comprising
obtaining a tress of
hair; producing at least one hair fiber of the tress to have a spilt-end;
removing at least one
hair fiber having a split-end from the tress; optionally marking the at least
one hair fiber;
capturing a first image of the split-end of the at least one hair fiber and
storing a
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
8
representation, e.g., an electronic representation, of the image; associating
the hair fiber with
the tress from which the hair fiber was removed; treating the tress and the
hair fiber with a
composition, wherein the composition comprises a hair care composition
comprising a
polyelectrolyte complex of a cationic polymer and an anionic polymer, from
about 1% to
about 5% of a thickening agent, about 10% or greater of propylene glycol, and
about 5% or
greater of an emollient, wherein the percentages are based on the total weight
of the
composition; removing the hair fiber from the treated tress; capturing a
second image of the
end of the hair fiber removed from the treated tress; assigning a value of 0
for no repair of the
split-end, 'A for partial repair, or 1 for complete repair with respect to the
hair fiber to assess
the degree of split-end repair of the hair fiber; and if more than one hair
fiber is assessed,
optionally determining an average value with respect to the assessed hair
fibers.
[0024] Another embodiment of the present invention provides a method of
quantitatively
assessing the degree of split-end hair fiber repair, the method comprising
obtaining a tress of
hair; producing at least one hair fiber of the tress to have a spilt-end;
removing at least one
hair fiber having a split-end from the tress; optionally marking the at least
one hair fiber;
capturing a first image of the split-end of the at least one hair fiber and
storing a
representation, e.g., an electronic representation, of the image; associating
the hair fiber with
the tress from which the hair fiber was removed; treating the tress and the
hair fiber with a
composition, wherein the composition comprises a hair care composition
comprising a
polyelectrolyte complex of a cationic polymer and an anionic polymer, from
about 3% to
about 5% of a thickening agent, and about 2% or less of an emollient, wherein
the
percentages are based on the total weight of the composition; removing the
hair fiber from
the treated tress; capturing a second image of the end of the hair fiber
removed from the
treated tress; assigning a value of 0 for no repair of the split-end, 1/2 for
partial repair, or 1 for
complete repair with respect to the hair fiber to assess the degree of split-
end repair of the
hair fiber; and if more than one hair fiber is assessed, optionally
determining an average value
with respect to the assessed hair fibers.
[0025] Another embodiment of the present invention provides a method of
quantitatively
assessing the degree of split-end hair fiber repair, the method comprising
obtaining a tress of
hair; producing at least one hair fiber of the tress to have a spilt-end;
removing at least one
hair fiber having a split-end from the tress; optionally marking the at least
one hair fiber;
capturing a first image of the split-end of the at least one hair fiber and
storing a
representation, e.g., an electronic representation, of the image; associating
the hair fiber with
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
9
the tress from which the hair fiber was removed; treating the tress and the
hair fiber with a
composition, wherein the composition comprises a hair care composition
comprising a
polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein
the viscosity
of the composition is greater than 3000 cps; removing the hair fiber from the
treated tress;
capturing a second image of the end of the hair fiber removed from the treated
tress, ;
assigning a value of 0 for no repair of the split-end, 'A for partial repair,
or 1 for complete
repair with respect to the hair fiber to assess the degree of split-end repair
of the hair fiber;
and if more than one hair fiber is assessed, optionally determining an average
value with
respect to the assessed hair fibers.
[0026] Another embodiment of the present invention provides a method of
quantitatively
assessing the degree of split-end hair fiber repair, the method comprising
obtaining a tress of
hair; producing at least one hair fiber of the tress to have a spilt-end;
removing at least one
hair fiber having a split-end from the tress; optionally marking the at least
one hair fiber;
capturing a first image of the split-end of the at least one hair fiber and
storing a
representation, e.g., an electronic representation, of the image; associating
the hair fiber with
the tress from which the hair fiber was removed; treating the tress and the
hair fiber with a
composition, wherein the composition comprises a hair care composition
comprising a
polyelectrolyte complex of a cationic polymer and an anionic polymer in the
folin of an
emulsion with improved freeze-thaw stability relative to comparative
compositions
containing such polyelectrolyte complexes; removing the hair fiber from the
treated tress;
capturing a second image of the end of the hair fiber removed from the treated
tress;
assigning a value of 0 for no repair of the split-end, 'A for partial repair,
or 1 for complete
repair with respect to the hair fiber to assess the degree of split-end repair
of the hair fiber;
and if more than one hair fiber is assessed, optionally determining an average
value with
respect to the assessed hair fibers.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 is a bar graph that shows percent mending determined using
a method of
the present invention with rinse-off conditioners in three cycles. Numbers in
parentheses are
percent polyelectrolyte complex (PEC). The number of fibers tested for the
various
compositions were 20, 100, and/or 50.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
[0028] Figure 2 is a bar graph that shows percent mending determined using
a method of
the present invention with leave-in compositions in one treatment. Twenty
fibers were tested
for each composition.
[0029] Figure 3 is a drawing showing the mending of a split-end using
polyelectrolyte
complexes (PECs). The drawing shows a possible mechanism of split-end repair
by PECs:
PECs attach to the site of the split-end, form a network with themselves and
the fiber
assembly, and shrink as they dry, binding the split end from within.
[0030] Figures 4A-4D show still photography of the mending of a variety of
split-end
types.
[0031] Figure 5 shows still photography taken from video of the mending of
split-ends
during the process of mending.
[0032] Figure 6 is a schematic diagram of an image data capture system in
accordance
with an embodiment of the invention.
[0033] Figure 7 shows a line graph comparing high humidity curl retention
of exemplary
compositions of the present invention.
[0034] Figure 8 shows thermal protection of hair using exemplary
compositions of the
present invention.
[0035] Figures 9-19 show freeze/thaw comparisons of compositions described
herein.
[0036] Figure 20 shows split-ends mended by exemplary compositions of the
present
invention.
DETAILED DESCRIPTION OF THE INVENTION
[0037] The present invention is predicated on the surprising and unexpected
discovery of
stable compositions containing polyelectrolyte complexes (PECs) and other hair
benefit
agents, particularly charged species, wherein the PECs remain intact and
exhibit hair repair
efficacy. It was unexpectedly found that the PECs can be combined with other
charged hair
benefit agents, i.e., substances that have beneficial properties for hair or
that impart beneficial
properties to hair, such as, e.g., cationic conditioning agents, without
disrupting the complex
that defines the PEC structure. Due to this unexpected discovery, the present
invention
provides compositions that not only provide the hair mending effect of PECs
but also
provides the advantages of other hair benefit agents. Thus, the present
invention provides
compositions and methods that include, e.g., charged hair benefit agents,
e.g., quaternary
ammonium salts, cationic conditioning polymers, and the like. Suitable hair
benefit agents
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
11
that can be combined with PECs in accordance with the present invention
include, for
example, stearamidopropyl dimethylamine, cocamidopropyl betaine, polyquatemium-
37,
polyquatemium-7, polyquaternium-39, DC 5-7113 (silicone quatemium-16 and
undeceth-11
and butyloctanol and undeceth-5), Abil T Quat 60 (silicone quatemium-22),
quatemium-80,
Merquat 2001 (polyquaternium-47), and acrylic acid/VP crosspolymer. Other
suitable
charged hair benefit agents arc described herein.
[0038] The present invention also provides a one-container process for
producing a PEC.
The process of the present invention also allows for the production of PECs of
the same
particle size distribution as those prepared using conventional processes
requiring two or
more separate containers. Thus, the present invention provides a more
efficient and cost
effective process for manufacturing PECs and hair care compositions containing
PECs.
[0039] The present invention also allows for concentrations of PECs greater
than 4 wt. %,
e.g., 8 wt. %.
[0040] Additionally, the present invention has the advantage of providing
methods that
can graphically demonstrate the benefits of a hair care composition such that
the benefits can
then be effectively communicated to consumers. Consumers purchase hair care
products
based on the properties of the hair care products. Effectively communicating
to these
consumers the beneficial properties of a hair care product composition, then,
is very
important so that the consumers can make informed purchasing decisions when
comparing
competing hair care products.
[0041] The present invention further has the advantage of providing a test
method that
allows for showing improved results of split-end mending of a hair care
composition such
that the benefits of the hair care composition can then be effectively
communicated to
consumers. Most split-end mending test methods use virgin hair where the split-
ends are
mechanically induced. It is likely that virgin hair is used in order for the
ingredients of a
split-end mending composition to act solely on the mechanically induced
damage. In other
words, in virgin hair, there is no other damage to the hair besides the split-
ends. Therefore,
the mending composition directs its mending capabilities only to the split-end
damage. The
mending ingredients of such a composition, then, would not be wasted on other
parts of the
hair. However, it has been unexpectedly found that the use of hair with
additional damage,
e.g., due to bleaching, can be used instead of virgin hair in a split-end
mending test method.
This is counterintuitive since it would be expected that any mending
composition would have
its mending ingredients attracted to other damage of the hair and not just the
split-ends,
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
12
reducing the amount of split-end repair. It has been found by Applicants that
the more
damaged the hair, the better the mending of split-ends. Further, it has been
found that, using
more damaged hair, a high mending percentage can be achieved in a rinse-out
product, e.g.,
greater than 50%, a level achievable with leave-in products. In one aspect,
the present
invention provides a hair care composition comprising a polyelectrolyte
complex of a
cationic polymer and an anionic polymer in the form of an emulsion with
improved freeze-
thaw stability relative to comparative compositions, e.g., made by formulating
the PECs
described in U.S. Patent Application Publication Nos. 2005/0089494 and
2006/0251603 in
conventional hair care base formulations. In an embodiment, the composition
comprises,
e.g., from about 1% to about 5% of a thickening agent, about 10% or greater of
propylene
glycol, and about 5% or greater of an emollient, wherein the percentages are
based on the
total weight of the composition. In another embodiment, the composition
comprises from
about 3% to about 5% of a thickening agent, and about 2% or less of an
emollient, wherein
the percentages are based on the total weight of the composition.
[0042] The compositions of the present invention provide unexpected freeze-
thaw
stability. Freeze-thaw stability is an important property of hair care
compositions particularly
for purposes of transport and storage which often exposes the compositions to
low
temperature extremes. Freeze-thaw stability is also important for products
which remain on
the hair and are thus exposed to temperature extremes outdoors. A composition
containing
PECs is not inherently unstable under freeze/thaw conditions. However, when
combined
with one or more fatty alcohols (e.g., cetyl, stearyl, etc.), which have been
used in the art to
thicken conditioner compositions, at e.g, about 3 wt. % or higher (e.g., about
5 wt. %), the
formulation will be unstable during freeze/thaw. The composition will get
grainy and
chunky, which is unsatisfactory to a consumer, and will likely be rejected by
the consumer.
[0043] In addition to freeze/thaw instability, conventional compositions
with PECs that
contain about 5% fatty alcohol do not have long term high temperature
stability. The
viscosity of such a composition continues to increase over time (e.g., over
100,000 cps after
2-3 months at 45 C), which is unsatisfactory to a consumer since it will be
too thick and hard
to spread throughout the hair, and will likely be rejected by the consumer.
The present
inventors have found that the addition of Salcare improves viscosity control;
that is,
viscosity is controlled to stay within, e.g., about 20,000-40,000 cps.
[0044] The compositions and methods of the present invention can include a
thickening
agent. Thickening agents add viscosity to a composition such that a
composition with a
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
13
greater amount of a given thickening agent has a higher viscosity. The
thickening agent can
be, for example a quaternary ammonium nitrogen compound or polymer, for
example
polyquaternium-37, and for example where polyquaternium-37 is in a mixture
with propylene
glycol dicaprylate/dicaprate and polypropylene glycol-1 trideceth-6. Salcare
SC 96 from
Ciba /BASF, Basel, Switzerland is an example of such a mixture. Salcare SC 96
is 65%
polyquatemium-37, 25% propylene glycol dicaprylate/dicaprate, 10% PPG-1
trideceth-6.
Other suitable thickening agents also can be added to the compositions of the
present
invention including, for example, xanthan gum, acrylic acid/VP crosspolymer
(e.g.,
UltrathixTM P-100; ISP, Wayne, NJ, USA), PVP, PVP K-90, PEG-90M, and
styrene/VP
copolymer.
100451 In another aspect, the present invention provides a hair care
composition
comprising a polyelectrolyte complex of a cationic polymer and an anionic
polymer, wherein
the viscosity of the composition is greater than 3000 cps. In an embodiment,
such a
composition can include, e.g., from about 1% to about 5% of a thickening
agent, about 10%
or greater of propylene glycol, and about 5% or greater of an emollient,
wherein the
percentages are based on the total weight of the composition. In another
embodiment, such a
composition can include, e.g., from about 3% to about 5% of a thickening
agent, and about
2% or less of an emollient, wherein the percentages arc based on the total
weight of the
composition.
100461 The viscosity of the compositions of the present invention can be
varied based on
the amount of thickening agent and/or other ingredients added. The
compositions of the
present invention may comprise thickening agents in a concentration of from
about 1 wt. % to
about 10 wt. %. The thickening agent may be present in an amount in wt. %,
e.g., as listed in
the table below. In the table, an "X" represents the range "from
[corresponding value in first
row] to [corresponding value in first column]." For example, the first "X" is
the range "from
about 1 wt.% to about 2 wt.%."
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
14
[0047] Table 1
about about about about about about about about
about
1 wt.% 2 wt.% 3 wt.% 4 wt.% 5 wt.% 6 wt.% 7 wt.% 8
wt.% 9 wt.%
about X
2 wt.%
about X X
3 wt.%
about X X X
4 wt.%
about
X X X X
wt.%
about X X X X X
about X X X X X X
about
X X X X X X X
about X X X X X X X X
9 wt.%
about X X X X X X X X X
wt.%
Thus, the viscosity can have a range between any aforementioned endpoints.
[0048] The
viscosity of the compositions of the present invention can range, e.g., from
about 3000 cps to about 100,000 cps, or, e.g., from about 20,000 cps to about
40,000 cps, as
measured by RV T-B, 10 rpm, 1 mm, at 25 C for viscosities under 50,000 cps or
RV T-C, 5
rpm, 1 mm, at 25 C for viscosities above 50,000 cps, but below 100,000 cps.
The viscosity
of the compositions of the present invention can range, e.g., as listed in the
table below. In
the table, an "X" represents the range "from [corresponding value in first
row] to
[corresponding value in first column]." For example, the first "X" is the
range "from about
3000 cps to about 10,000 cps."
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
[0049] Table 2
about about about about about about about about
about about
3000 10,000 20,000 30,000 40,000 50,000 60,000 70,000 80,000 90,000
cps cps cps cps cps cps cps cps cps cps
about
X
10,000
about
20,000 X X
cps
about
30,000 X X X
cps
about
40,000 X X X X
cps
about
50,000 X X X X X
cps
about
60,000 X X X X X X
cps
about
70,000 X X X X X X X
cps
about
80,000 X X X X X X X X
cps
about
90,000 X X X X X X X X X
cps
about
100,000 X X X X X X X X X X
cps
Thus, the viscosity can have a range bounded by any two of the aforementioned
endpoints.
[0050] In one aspect of the invention, the composition contains a
thickening agent,
propylene glycol, and a relatively high concentration of an emollient, e.g.,
in an amount of 5
wt. % or greater. Suitable emollients can include, e.g., one or more fatty
alcohols.
Consumers may find hair care products containing 10 wt. cYo or more of
propylene glycol to
be unacceptable in that they may think such products would be heavy or sticky
feeling, may
notice hair taking too long to dry (due to the humectant properties of
glycols), or may notice
hair is hard to comb or is not shiny. Surprisingly, however, it was found that
including
propylene glycol at 10% or greater in accordance with the present invention
not only
provided acceptable freeze-thaw stability but also may provide a composition
that is more
likely to be found acceptable by consumers. Additionally, Applicants have
found that an
emulsion in such compositions can accept a high level of glycol and not be
affected (e.g.,
viscosity change, etc.). Applicants found that other polyhydric alcohols such
as sorbitol and
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
16
glycerin at 5 wt. %, did not provide for acceptable freeze-thaw stability.
[0051] In some embodiments, the compositions and methods of the present
invention
may include propylene glycol, e.g., in concentrations of about 10 wt. % or
greater, about 20
wt. % or greater, about 30 wt. % or greater, about 40 wt. c1/0 or greater, or
about 50 wt. % or
greater.
[0052] The present invention also provides a hair care composition
comprising a
polyelectrolyte complex of a cationic polymer and an anionic polymer; from
about 1% to
about 5% of a thickening agent; about 10% or greater of propylene glycol; and
about 5% or
greater of an emollient; wherein the percentages are based on the total weight
of the
composition.
[0053] In another aspect, the present invention provides a hair care
composition that
includes a polyelectrolyte complex of a cationic polymer and an anionic
polymer, in
combination with from about 3% to about 5% of a thickening agent, and about 2%
or less of
an emollient, wherein the percentages are based on the total weight of the
composition. In
this aspect, the composition of the present invention is preferably
substantially free of
propylene glycol. As used herein, "substantially free of propylene glycol"
means that the
composition of the present invention contains less than about 1 wt. %
propylene glycol, less
than about 0.5 wt. % propylene glycol, less than about 0.1 wt. % propylene
glycol, and more
preferably 0 wt. % or no propylene glycol.
[0054] The compositions and methods of the present invention can include
the presence
of one or more emollients. Emollients can, e.g., soften and/or soothe skin.
Suitable
emollients can include, for example, fatty alcohols. Fatty alcohols include,
e.g., cetyl
alcohol, stearyl alcohol, and combinations thereof. Fatty alcohols can
sometimes be used to
thicken compositions as well as provide emollient properties. Applicants have
surprisingly
found that compositions of the present invention, e.g., 5% fatty alcohol/1%
Salcare SC 96
and 1% fatty alcohol/5% Salcare SC 96, exhibit roughly the same emulsion
properties (e.g.,
viscosity, rheology, yield value, appearance, color). This was unexpected at
cetyl alcohol
concentrations down to only about 1 wt. %. Furthermore, it has been found that
the emollient
concentration can be reduced to about 1 wt. % or less in a composition with 2
wt. % PECs
where the composition also has from about 3 wt. % to about 5 wt. % of a
thickening agent.
The wt. % range of fatty alcohols can be expanded when the concentration of
PECs is lower.
Even with a low concentration of emollient fatty alcohols, PEC compositions
have been
found to still provide an acceptable sensory experience. This is unexpected in
that most hair
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
17
care compositions, especially conditioners, have higher concentrations of
emollient fatty
alcohols to provide a sensory experience for the consumer. Also, coupled with
the thickening
agent, the PEC composition retains an acceptable viscosity. Additionally, the
combination of
a low concentration of emollient fatty alcohol and PECs with from about 3 wt.
% to about 5
wt. % thickening agent provides for a rich, white opacity not observed with
any of these
ingredients individually.
[0055] The concentration of the emollient in the compositions of the
present invention
desirably can be tailored based on the concentration of thickening agent. With
the thickening
agent at 3-5 wt. %, For example, the emollient concentration can range, e.g.,
as listed in the
table below. In the table, an "X" represents the range "from [corresponding
value in first
row] to [corresponding value in first column]." For example, the first "X" is
the range "from
about 0 wt.% to about 0.1 wt.%."
[0056] Table 3
about about about about about about about about about
about about about about about about about about
about about ' about
0 wt.% 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
wt.% 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 0
l,)
wt.% wt.% wt.% wt.% wt.% wt.% wt.%
wt.% . wt.% wt.% wt.% wt.% wt.% wt.% wt.% wt.% wt.%
wt.% o
1-
about
--.....
0.! X
CJI
wt.%
about i
C.4
.1.
0.2 X X ,
(....)
,
,
wt.% .
.
about
0.3 X X X
wt.%
about
0.4 X X X X
wt.%
.
about
a
0.5 X X X X X
wt.%
. o
about
to
co
0.6 X X X X X X
i-
n)
wt.%
about
00 1-`
0.7 X X X X X X X
n)
wt.%
0
I-.
about
w
0.8 X X X X X X X X
O
1
w
wt.%
1
1 about
i-
ko
i 0.9 X X X X X X X X X
' wt.% .
.
about X X X X X X X X X X
1 wt.%
about
1.1 X X X X X X X X X X X
wt.%
about
01:1
1.2 X X X X X X X X X X X X
cn
1-3
wt.%
.
about
1.3 X X X X X X X X X X X X X
r..)
, i
1-,
wt.%
about
- e-
1.4 X X X i X X X X X X X X X X
X vi
vi
wt.% I
,
(...)
--.4
o
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
19
x
x x
x x x
x x x x
x x x x x
x x x x x x
x x x x x x
x 8 X X X X
X X X X X X
X X X X X X
X X X X X X
X X X X X X
X X X X X X
X X X X X X
X X X X X X
X X X X X X
X X X x X x
X X X X X X
x X x X x X
X X X X x X
,;,,
JR ,,- JRJR ,--- .- JR .0JR <,,JR
20
Thus, the concentration of emollient can have a range bounded by any two of
the
aforementioned endpoints. Alternatively, with the thickening agent at 1-5 wt.
%, for
example, the emollient concentration can be, e.g., from about 5 wt. % or
greater, about 6 wt.
% or greater, about 7 wt. % or greater, about 8 wt. % or greater, about 9 wt.
% or greater,
about 10 wt. % or greater, about 20 wt. % or greater, about 30 wt. % or
greater, about 40 wt.
% or greater, or about 50 wt. % or greater.
100571 Some PECs are described in U.S. Patent Application Publication
Nos.
2005/0089494 and 2006/0251603.
As outlined in these publications, the formation of PECs is not simply due to
the
presence of oppositely charged polymers in a composition. A phase diagram may
be
produced to show the polymer-polymer species present when concentrations of
the oppositely
charged polymers are varied (thus varying the ratios of the polymers to each
other). Based on
the phase diagram, the ratio of polymers in terms of weight percent, moles,
etc. at which
PECs are formed can be determined. For PVMMA/polyquat-28 PECs, a preferred
weight
ratio is 1:9 PVMMA:polyquat-28. However, PECs may exist at other weight
percent ratios.
For example, PVMMA/polyquat-28 PECs can be formed around the 1:9 weight
percent ratio,
such that a ratio slightly higher or lower than 1:9 will have some amount of
PECs present.
The weight percent ratio can range from about 1:8 to about 1:10 PVMMA:polyquat-
28.
Thus, the cationic polymer and anionic polymer in the compositions of the
present invention,
and used in the methods of the present invention, can be in the weight ratio
of actives from
about 1:8 to about 1:10.
100581 In addition to weight percent ratios, the formation of PECs may be
determined
based on the charge-charge ratio of polymers. PECs are usually formed when the
charge-
charge ratio of the polymers is 1:1. Therefore, PECs are likely to form when,
e.g., each
negative charge of a polymer is balanced by a positive charge of another
polymer. However,
PECs may exist at other charge-charge ratios. For example, PECs can be formed
around the
1:1 charge-charge ratio, such that a ratio slightly higher or lower than 1:1
will have at least
some amount of PECs present, for example at ratios such as 0.82 to 1.8
cationic to anionic
charge. A phase diagram can be produced to determine the presence of PECs at
varying
charge-charge ratios.
[0059] Contemplated herein are PECs formed between polymers comprising
cationic
charges and polymers comprising anionic charges. However, phase diagrams may
be
constructed to determine the suitability of PEC formation for any polymer-
polymer system,
CA 2812991 2017-11-27
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
21
so long as the polymers interact through ionic bonds. The compositions and
methods of the
present invention may include a polyelectrolyte complex wherein a cationic
polymer
comprises one or more monomeric units with one or more quaternary ammonium
nitrogen
moieties, for example, vinylpyrrolidone/methacrylamidopropyl trimethylammonium
chloride
copolymer (polyquaternium-28). Non-limiting examples of other cationic
polymers that may
be used in forming PECs include other polyquat polymers such as polyquaternium-
7,
polyquaternium-10, or polyquaternium-11. The compositions and methods of the
present
invention may include a polyelectrolyte complex wherein an anionic polymer
comprises
monomeric units having ionizable carboxylic acid moieties, for example, a
methylvinylethcr/maleic acid copolymer. Another example of an anionic polymer
that may
be used in forming PECs is vinylpyrrolidonc/acrylatcs/lauryl methacrylate
copolymer.
[0060] Polymers with ionizable groups, such as carboxylic acid groups or
tertiary amine
groups, may require the adjustment of the pH in order for a polyelcctrolytc
complex to form.
Adjustment of the pH alters the percent of ionizable groups that arc ionized
and thus adjusts
the number of groups that may interact through ionic bonds. Production of
phase diagrams at
varying pHs can be used to determine the proper pH for PEC formation. For
PVMMA/polyquat-28 PECs, a pH range of from about 6.5 to about 7.5 may be used
for PEC
foimation. The suitable pH can range, e.g., as listed in the table below. In
the table, an
represents the range "from [corresponding value in first row] to
[corresponding value in first
column]." For example, the first "X" is the range "from about pH 6.5 to about
pH 6.6."
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
22
[0061] Table 4
about about about about about about about about
about about
pH 6.5 pH 6.6 pH 6.7 pH 6.8 pH 6.9 pH 7.0 pH 7.1 pH 7.2 pH 7.3 pH 7.4
about
X
6.6
about X X
pH 6.7
about X X X
pH 6.8
about
X X X X
pH 6.9
about X X X X X
pH 7.0
about X X X X X X
pH 7.1
about
X X X X X X X
pH 7.2
about
X X X X X X X X
pH 7.3
about X X X X X X X X X
pH 7.4
about
X X X X X X X X X X
pH 7.5
Thus, the pH can have a range bounded by any two of the aforementioned
endpoints.
[0062] The pH of a composition may be adjusted using neutralizing/buffering
agents.
For acidic groups such as carboxylic acid, a basic neutralizer can be used,
such as a
hydroxide compound. Suitable hydroxide compounds include strong bases such as
sodium
hydroxide. For basic groups, an acidic neutralizer can be used, such as citric
acid. Any
suitable concentration of neutralizer can be used, including, e.g., those
listed in the table
below. In the table, an "X" represents the range "from [corresponding value in
first row] to
[corresponding value in first column]." For example, the first "X" is the
range "from about
0.1 wt.% to about 1 wt.%."
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
23
100631 Table 5
about about about about about about about about
0.1 wt.% 1 wt.% 2 wt.% 3 wt.% 4 wt.% 5 wt % 10 wt.%
20 wt.%
about X
1 wt.%
about X X
2 wt.%
about
X X X
about
X X X X
about X X X X X
about
X X X X X X
wt.%
about X X X X X X X
wt.%
about X X X X X X X X
wt.%
Thus, the concentration of neutralizer can have a range bounded by any two of
the
aforementioned endpoints. So long as the PECs have formed under desired pH
conditions,
the final pH of any resulting composition comprising the PECs may be the same
or different
from the pH at which the PECs were fowled, so long as the PECs remain intact.
[0064] The PVMMA/polyquat-28 PECs have the ability to mend split-ends of
hair fibers.
Hair has a net negative charge. Without being bound to any particular theory,
PECs are
believed to be substantive to the hair fiber and adhere the ends of a split-
end together through
adhesive properties. The positive charges of the polyquat-28 polymer are
attracted to the
negatively charged hair fibers and are substantive to the hair. Since the
negatively charged
PVMMA polymer is complexed to the polyquat-28, the PVMMA also is drawn to the
hair.
The ends of the split-end are then adhered together through the adhesive
action of multiple
PECs interacting with the ends of the split-end and/or each other (e.g., in
film-formation
where the film contracts while drying). Additionally, the surface tension
experienced by the
ends of the split-end due to the interaction of water during film-formation
assists in adhering
the ends together.
[0065] To the extent that the PECs exist in the foul' of suspended or
emulsified particles,
the particle size of PECs should allow the PECs access to the ends of a spilt-
end in order for
the PECs to mend damaged hair fibers. As long as the PECs have access to the
ends of a
split-end, the particle size distribution can have any suitable average PEC
particle size.
Suitable average PEC particle sizes can include, e.g., those listed in the
table below. In the
table, an "X" represents the range "from [corresponding value in first row] to
[corresponding
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
24
value in first column]." For example, the first "X" is the range "from about
0.5 pm to about
1 pm."
[0066] Table 6
about about about about about about about about
0.5 pm 1 pm 2 i_tm 3 p.m 5 m 10 pm 20 pm 30
pm
about
X
1 pm
about
X X
2 pm
about
X X X
3 p.m
about
X X X X
pm
about
X X X X X
pm
about
X X X X X X
p.m
about
X X X X X X X
p.m
about
X X X X X X X X
40_ptu
Thus, the average PEC particle size distribution can have a range bounded by
any two of the
aforementioned endpoints. In some embodiments, the compositions and methods of
the
present invention includea PEC particle distribution with an average PEC
particle size of
about 5 micrometers, e.g., of about 5 3 micrometers or about 5 2
micrometers. The
compositions and methods of the present invention also can include PEC
particles that exist
within a microgel, e.g., an interlocking microgel structure.
[0067] The compositions and methods of the present invention can
incorporate PECs at
higher concentrations than previously recognized as achievable in the art. For
instance, the
compositions of the present invention can include PECs of PVMMA/polyquat-28 at
a
concentration of 8 wt. %. The concentration of PECs in a hair care composition
may be
varied. The compositions and methods of the present invention may contain the
polyelectrolyte complex in a concentration of from about 1% to about 8% based
on the total
weight of the composition. The compositions of the present invention may
contain the
polyelectrolyte complex in a concentration of from about 1% to about 3% or
from about 2%
to about 4% based on the total weight of the composition. The concentration of
PECs may
be, e.g., as listed in the table below. In the table, an "X" represents the
range "from
[corresponding value in first row] to [corresponding value in first column]."
For example,
the first "X" is the range "from about 0.1% to about 0.5%."
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
100681 Table 7
about about about about about about about about
about
0.1% 0.5% 1% 2% 3% 4% 5% 6% 7%
about
X
0.5%
about
X X
1%
about
X X X
24)/0
about
X X X X
3%
about X X X X X
4%
about X X X X X X
about
X X X X X X X
6%
about
X X X X X X X X
7%
about X X X X X X X X X
8%
Thus, the concentration of PECs can have a range bounded by any two of the
aforementioned
endpoints.
100691 PEC formation may be confirmed using any suitable method. An example
of a
suitable method includes microscopy. Under a light microscope, the structure
of a polymer-
polymer system can be investigated, and the sizes of any particles present can
be determined
using sizing software. Such a method can yield the particle size distribution
of PECs,
provided the presence of other ingredients does not obscure the PEC structure.
Another
method includes determining the particle size distribution using a Malvern
particle size
analyzer. Also, the physical properties of a composition of only PECs in a
carrier solvent can
indicate the presence of the PECs. For example, as the presence of PECs
increases, such a
composition increases in haziness and opacity. Also, the viscosity of such a
composition
decreases to a minimum that corresponds to the presence of the greatest amount
of PECs for a
given polymer-polymer system, where the PECs are the most compact.
[0070] The compositions of the present invention may be in the form of, and
the methods
of the present invention can produce or use compositions in the form of, e.g.,
shampoos,
conditioners, gels, rinses, emulsions (oil-in-water, water-in-oil or
multiphase), lotions,
creams, crèmes, ointments, pomades, sprays (pressurized or non-pressurized),
spritzes,
mousses, foams, shampoos, solutions, and solids (e.g., as sticks, semisolids
and the like).
Thus, the compositions of the present invention may be in the form of, and the
methods of the
present invention can produce or use compositions in the foitii of, e.g., a
cream, a lotion, a
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
26
solution, an ointment, or a gel. Thus, the hair care compositions and methods
of the present
invention can include other components that may be suitable for use in these
types of
compositions. Preferably such components are compatible with PECs, in that the
components do not disrupt PEC structure.
[0071] Compositions can be meant for rinse-out, leave-in, and/or overnight
treatments.
The methods and hair care compositions of the present invention may include
mixing a
polyelectrolyte complex with one or more components selected from aqueous
carriers,
surfactants, neutralizers, fragrances, conditioning agents, emulsifiers,
thickening agents,
preservatives, gelling agents, silicones, hair fixatives, humectants and
moisturizers to form a
hair care composition. Thus, the compositions and methods of the present
invention can
include, e.g., a preservative, a neutralizer, a fragrance, a silicone, or a
combination thereof
One of ordinary skill in the art would recognize that the ingredients
identified herein may
have multiple properties and thus may fit within multiple ingredient
categories, especially if it
is a commercially available product with multiple components.
[0072] The aqueous carrier can include any suitable quantity of water,
e.g., from about 25
wt% to about 97 wt% water (e.g., from about 30% to about 95% water). The
composition of
the present invention can include from about 30 wt. % to about 97 wt. % water,
from about
50 wt. % to about 80 wt. % water, or from about 60 wt. % to about 70 wt. %
water. The
water used in the composition of the present invention can be deionized water.
[0073] Suitable emulsifiers can include, for example, PPG-3 benzyl ether
myristate (e.g.,
Crodamol STS; Croda, Inc., Edison, NJ, USA), arachidyl alcohol and behenyl
alcohol and
arachidyl glucoside (e.g., Montanov 202; SEPPIC, Paris, France),
polyacrylamide and C13-
14 isoparaffin and laureth-7 (e.g., SepigelTM 305; SEPPIC), glyceryl stearate,
isoceteth-20,
oleth-2, methoxy PEG/PPG-7/3 aminopropyl dimethicone, PEG/PPG-18/18
Dimethicone
(e.g., DC-190; Dow Corning), PEG-12 dimethicone, PEG-40 hydrogenated castor
oil, PEG-6
caprylic/capric triglyceride, aminomethyl propanol (AMP-95), and polyglycery1-
3 distearate.
[0074] Suitable surfactants, e.g., detersive and/or cleansing surfactants,
may be used,
including, for example, disodium laureth sulfosuccinate, sodium laureth
sulfate, polysorbate
20, polysorbatc 60, cocamidopropyl betaine, and stearalkonium chloride. Such
surfactants
may be present in a shampoo composition. A conditioner preferably is
substantially free of
detersive surfactants, unless the conditioner is a two-in-one combination of a
shampoo and
conditioner. As used herein, "substantially free of detersive surfactants"
means that the
composition of the present invention contains less than about 2 wt. %
detersive surfactants
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
27
and more preferably less than about 1 wt. %, e.g., 0 wt. % or no detersive
surfactants.
[0075] Suitable conditioning agents can include, for example, tertiary or
quaternary
amines such as stearamidopropyl dimethylamine, polyquaternium-47 (e.g.,
Merquat 2001;
Nalco, Naperville, IL, USA), silicone quaternium-22 (e.g., Abil T Quat 60;
Evonik, Essen,
Germany), cocamidopropyl betaine, polyquatemium-11, polyquaternium-39,
polyquaternium-4 (Celquat H-100; Akzo Nobel, Amsterdam, Netherlands),
polyquaternium-
4 (Celquat L-200; Akzo Nobel) to 0.5 wt. %, polyquaternium-7, polyquaternium
10, and
quatemium-80. Other suitable conditioning agents include, e.g., Aqu D 4272 N-
Hance
SP100 (Acrylamidopropyltrimonium Chloride/Acrylamide Copolymer),
Distearoylethyl
Dimonium Chloride; Cetearyl Alcohol (Varisoft EQ 65), Rhodia Guar S.
Behenyltrimethyl
Ammonium Chloride, and Behentimonium Chloride/Cetearyl Alcohol. The N-Hance
SP100
copolymer has been found to be especially beneficial. Thus, the compositions
and methods
of the present invention can include, e.g., aerylamidopropyltrimonium
chloride/acrylamide
copolymer. As is shown in Example 16 below, this copolymer provides additional
split-end
mending in a composition that contains PECs.
[0076] Although not essential, an effective amount of at least one
preservative may be
incorporated in the composition. For example, the preservative can be selected
to kill
bacteria that might otherwise be sustained or multiply in the composition.
Suitable
preservatives can include, for example, DMDM hydantoin, disodium EDTA,
KathonTM CG
(actives: 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-
one) and the
like, and combinations thereof.
[0077] Suitable gelling agents can be used. Suitable gelling agents can
include, for
example, acrylic acid/VP crosspolymer (e.g., UltrathixTM P-100; ISP).
[0078] Suitable silicones can be added, e.g., to improve conditioning of
hair. Suitable
silicones can include, for example, polysiloxanes, including dimethicone,
dimethiconol,
cyclopentasiloxane, and cyclohexasiloxane. These include, e.g., phenyl
trimethicone, Abil
OSW 5 (84% Cyclopentasiloxane, 15% Dimethiconol, 1% Dimethicone; Evonik,
Essen,
Germany), DC-200 (dimethicone; Dow Corning, Midland, MI, USA), Fluid Blend
(80%
cyclornethicone, 20% dimethicone), and DC-1501 (D5/Dimethiconol; Dow Corning).
Other
suitable silicones include, for example, DC-556 (phenyl trimethicone; Dow
Corning), and
aminofunctional silicones, for example, DC-949 (31% amodimethicone, 1.9%
trideceth-12,
2.2% eetrimonium chloride, 55-60% water, 2.2% cyclotetrasiloxanc, 1.6%
cyclopentasiloxane, and <0.5% sodium benzoate; Dow Corning), DC-8500 (82%
Bis(C13-15
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
28 =
Alkoxy) PG-Amodimethicone, 18% C14-15 Alcohols; Dow Corning), aminopropyl
dimethicone, DC 5-7113 Silicone Quat Microemulsion (66% Water, 25% Silicone
Quaternium-16, 7.4% Undeceth-11, 4.5% Butyloctanol, 3.5% Undeceth-5; Dow
Corning),
DC 2-8566 (amodimethicone; Dow Corning), and amodimethicone (ADM 1100;
Wacker).
[0079] Suitable hair fixative may be used. Suitable examples include, for
example
VP/methacrylamide/vinyl imidazole Copolymer (e.g., LUVISET Clear; BASF),
acrylic
acid/vinylpyrrolidone crosspolymer (e.g., UltrathixTM P-100; ISP), vinyl
caprolactum/VP/dimethylaminoethyl mcthacrylate copolymer (Advantage S; ISP),
and
VP/VA Copolymer.
[0080] Additional ingredients may be added, including, for example, Cocos
nucifera
(coconut) oil, mineral oil (paraffinum liquidum), sodium chloride, hydrolyzed
silk, keratin
amino acids, ascorbic acid, panthenol, tocopherol acetate, biotin,
niacinamide,
triethanolamine, triticum vulgare (wheat) flour lipids, ceramide 3, persea
gratissima
(avocado) oil, tetrahexyldecyl ascorbate, glycine soja (soybean) sterols,
alpha-gluean
oligosaecharide, ethylhexyl methoxycimaamate, butyl methoxydibenzoylmethane,
and
tocopheryl acetate. A propellant may be used, such as in a spray composition,
including
isobutane and propane and 152A (78.5% A46; 28.5% HFC 152A). Fatty acids can be
used,
such as myristie acid, palmitic acid, and stearic acid.
[0081] Additional components and/or ingredients can be provided to impart
beneficial
properties to the hair, e.g., components and/or ingredients for imparting
softness to the hair
after drying, providing moisturization to the hair, providing pleasing
consistency/viscosity of
the composition, and providing volume/fullness to the hair.
[0082] Fragrances can be provided in the compositions of the present
invention. A non-
limiting example of a fragrance is flower extract. Any particular fragrance
can be used, and
one of ordinary skill in the art would recognize that the particular identity
of fragrance is not
important. Indeed, the compositions of the present invention can be provided
without
fragrance.
[0083] An embodiment of a composition of the present invention can include,
for
example, 1-2 wt. % PEC of PVMMA copolymer and polyquaternium-28 in a 1:9
ratio. Such
a complex can be manufactured in a side tank and added to the main batch tank
after an
emulsion phase is prepared and when the emulsion phase has cooled to 45-65 C.
A tertiary
or quaternary amine at approximately 1-2 wt. % can be included in the emulsion
phase and
neutralized to a pH of about 4.0-6Ø Fatty alcohol (e.g., cetyl and/or
stearyl) can be included
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
29
at approximately 3-7 wt. % in conjunction with a low-HLB co-emulsifier such as
glyceryl
monostcarate, distearate, or the like, in a 5:1 ratio and can be included in
the emulsion phase.
Silicones at, e.g., 0.1-10 wt. %, or a blend of dimethicones, cylcomethicones,
phenyl and/or
amino functional silicones also can be included. An emollient ester, such as
PPG-3 benzyl
ether myristate (e.g., Crodamol STS), at, e.g., 1-4 wt. % can be added to
enhance product
spreadability in addition to enhancing shine and hair feel. Propylene glycol
at 10% can be
included to improve freeze/thaw stability. Salcare SC-96 can also be
included, which can be
after the emulsion phase and when the batch has cooled to 45-65 C, at, e.g.,
0.1-5 wt. % to
increase viscosity, improve conditioned feel in hair, and improve long term
stability and
viscosity control. Another embodiment of a composition of the present
invention can
include, for example, the same composition except with approximately 1% fatty
alcohol, no
emollient ester, and Salcare SC 96 at, e.g., 1-7 wt. %. An embodiment of a
composition
with approximately 3-7 wt. % fatty alcohol can include PEC complex that has
been made first
in a main tank, with the rest of the composition then made in the same tank,
where Salcare
SC-96 has been increased to, e.g., 1-7 wt. %. An embodiment of a composition
with
approximately 1 wt. % fatty alcohol can include PEC complex that has been made
first in a
main tank, with the rest of the composition then made in the same tank, where
Salcare SC
96 has been increased to, e.g., 3-10 wt. %.
100841 The present invention includes hair care compositions formed from
any of the
suitable ingredients described herein. In an embodiment, the present invention
includes hair
care compositions formed from polyquatemium-28 and methylvinylether/maleic
acid
copolymer; from about 1% to about 5% of a thickening agent; about 10% or
greater of
propylene glycol; and about 5% or greater of an emollient; wherein the
percentages are based
on the total weight of the composition. In an embodiment, the present
invention includes hair
care compositions formed from polyquatemium-28 and methylvinylether/maleic
acid
copolymer; from about 3% to about 5% of a thickening agent; and about 2% or
less of an
emollient; wherein the percentages are based on the total weight of the
composition. In an
embodiment, the present invention includes hair care compositions formed from
polyquatemium-28 and methylvinylether/maleic acid copolymer, wherein the
viscosity of the
composition is greater than 3000 cps. In an embodiment, the present invention
includes hair
care compositions formed from polyquatemium-28 and methylvinylether/maleic
acid
copolymer in the form of an emulsion with improved freeze-thaw stability
relative to
comparative compositions containing such polyelectrolytc complexes. In an
embodiment, the
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
present invention includes hair care compositions fot med from
polyquatemium-28,
methylvinylether/maleic acid copolymer, and polyvinylpyrrolidone.
[0085] The present invention also provides embodiments of hair care
formulations and
their method of use that do not: increase the force required to comb hair, as
compared to
untreated hair; increase the force required to separate the adhesion of two
hair fibers, as
compared to untreated hair; increase the "three point bending" force, as
compared to
untreated hair; increase Young's Modulus, as compared to untreated hair;
reduce the
luster/shine of hair, as compared to untreated hair; or impart other
quantifiable "negative"
attributes.
[0086] The compositions of the present invention may be used in any
suitable method for
treating hair. For example, compositions described herein may be used for
conditioning a
hair fiber by applying a composition to the hair fiber and rinsing the hair
fiber with water.
After rinsing, the hair fiber may be dried with a blow dryer, combed, and/or
styled using
styling products or compositions. Additionally, compositions described herein
may be used
to repair a split-end of a hair fiber by applying a composition to the split-
end and rinsing the
split-end with water. This method also may be followed by blow drying,
combing, and/or
styling. The compositions described herein further may be used in a method of
thickening a
hair fiber by applying to the hair fiber a composition of the present
invention and rinsing the
hair with water. In other embodiments, the compositions of the present
invention can be used
for hair styling, for example, when the compositions comprise a styling hair
benefit agent.
For example, the composition can be a styling spray (aerosol and non-aerosol).
In other
embodiments, the compositions of the present invention can be used for
shampooing hair
when fomiulated as a shampoo. Other styling products can include leave-in
conditioners,
overnight conditioning treatments, styling lotions/cremes/balms, styling gels,
styling
mousses, serums, oil treatments, glazes, and conditioning sprays (aerosol and
non-aerosol).
[0087] The freeze-thaw stability of a hair care composition comprising a
polyelectrolyte
complex of a cationic polymer and an anionic polymer may be improved by adding
to the
hair care composition from about 1% to about 5% of a thickening agent, wherein
the
percentage is based on the total weight of the composition. The thickening
agent can
comprise a quaternary ammonium nitrogen compound or polymer. The quaternary
ammonium nitrogen compound or polymer can be, e.g., polyquatemium-37. The
polyquatemium-37 can be in a mixture with propylene glycol
dicaprylate/dicaprate and
polypropylene glycol-1 trideceth-6. Alternatively, the freeze-thaw stability
of a hair care
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
31
composition comprising a polyeleetrolyte complex of a cationic polymer and an
anionic
polymer may be improved by adding to the hair care composition from about 10%
or greater
of propylene glycol, wherein the percentage is based on the total weight of
the composition.
[0088] The present invention provides for the thermal protection of hair.
When a leave-
on composition with PECs as described herein is applied to hair, the PECs
protect the hair
shaft from damage (e.g., fiber fragmentation) due to heat. The heat can be
from any source,
including, for example, a hair dryer, a flat iron, or a hot styling tool.
[0089] The methods of the present invention allow for the production of
PECs in one
container. Accordingly, one aspect of the present invention provides a method
of producing a
polyelectrolyte complex, the method comprising hydrating a
methylvinylether/maleic acid
copolymer having repeating units of the formula (Formula I)
OCRoç
_________________________ cH2¨cH¨yii¨cH
OH OH
in a container; reacting the methylvinylether/maleic acid copolymer with a
base, such as, e.g.,
sodium hydroxide, in the container in an amount sufficient to at least
partially neutralize the
acidic groups thereof, to form an intemiediate mixture; heating the
intermediate mixture in
the container; adding to the intei mediate mixture in the container a
cationic copolymer of a
vinylpyrrolidone of the formula (Formula II)
õAy
õ /
and a methacrylamidopropyl trimethylammonium chloride of the formula (Fommla
III)
co
-c __________________________________
(G.Haki
C140-14.--CH3
C4"
01-6
; and
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
32
mixing the polymers in the container at high shear force and at a temperature
of at least about
50-60 C to produce the polyelectrolyte complex.
[0090] Additionally, another aspect of the present invention allows for
production of a
hair care composition by combining the PECs produced in accordance with the
present
invention with other hair benefit agents. In accordance with the process of
the present
invention, such hair care compositions can be prepared by combining the PECs
produced in
accordance with the present invention with other hair benefit agents in a
single container.
Accordingly, the present invention also provides a method of producing a hair
care
composition comprising producing a polyelectrolyte complex, comprising the
steps of
hydrating a methylvinylether/maleic acid copolymer having repeating units of
the formula I
in a container; reacting the methylvinylether/maleic acid copolymer with a
base, such as, e.g.,
sodium hydroxide (e.g., a 20% sodium hydroxide solution, e.g., in water), in
the container in
an amount sufficient to at least partially neutralize the acidic groups
thereof (e.g., by adding
sufficient base to achieve a pH of from about 6.5 to about 7.5 or from about
6.9 to about 7.0),
to form an intermediate mixture; heating the intermediate mixture in the
container, e.g., to a
temperature of from about 50 C to about 60 C; adding to the intermediate
mixture in the
container a cationic copolymer of a vinylpyrrolidone of the formula II and a
methacrylamidopropyl trimethylammonium chloride of the formula III; mixing the
polymers
in the container at high shear force, e.g., at a temperature of about 50-60 C
to produce the
polyelectrolyte complex. The process of the present invention optionally
includes further
adding to the polyelectrolyte complex in the container one or more additional
components
selected from aqueous carriers, surfactants, fragrances, conditioning agents,
emollients,
emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair
fixatives,
humectants and moisturizers; and mixing the resulting composition in the
container.
[0091] The present invention also allows for producing a hair care
composition in two
containers, the PECs being produced in one container and the rest of the
composition being
produced in a second container, where the PECs and other ingredients are then
combined. In
this aspect, the present invention also provides a method of producing a hair
care composition
comprising producing a polyelectrolyte complex between a
methylvinylether/maleic acid
copolymer and a cationic copolymer of a vinylpyn-olidone and a
methacrylamidopropyl
trimethylammonium chloride, comprising the steps of hydrating a
methylvinylether/maleic
acid copolymer having repeating units of the formula I in a first container;
reacting the
methylvinylether/maleic acid copolymer with a base, such as, e.g., sodium
hydroxide, in the
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
33
first container in an amount sufficient to at least partially neutralize the
acidic groups thereof,
to form an intermediate mixture; heating the intermediate mixture in the first
container;
adding to the intermediate mixture in the first container a cationic copolymer
of a
vinylpyrrolidone of the formula 11 and a methacrylamidopropyl
trimethylammonium chloride
of the formula III; mixing the polymers in the first container at high shear
force and at a
temperature of at least about 50-60 C to produce the polyelectrolyte complex;
mixing in a
second container one or more components selected from aqueous carriers,
surfactants,
fragrances, conditioning agents, emollients, emulsifiers, thickening agents,
preservatives,
gelling agents, silicones, hair fixatives, humectants and moisturizers; and
mixing together in
the first or second container the polyelectrolyte complex of the first
container and the mixed
components of the second container.
[0092] Phase diagrams, as indicated above, can be produced to determine the
conditions
under which PECs form, including within which polymer:polymer weight ratios
and charge-
charge ratios. Additional conditions may be varied as well, including
temperature, solvent
system, etc. Each of these conditions may be varied to determine their effects
on PEC
formation. Thus, due to the various conditions required to produce PECs and
the vast
number of variables involved, the production of PECs can be complicated and
difficult. This
is especially the case when a particular particle size is desired, as in
producing
PVMMA/polyquat-28 PECs that can mend split-end damaged hair. In addition to
the
polymer:polymer weight ratios and/or charge-charge ratios, etc., the
particular production
method used also may impact the average particle size distribution of PECs.
For example,
the mixing speed and/or mixing time during the addition of one polymer to
another, and the
mixing speed and/or mixing time after this addition, can affect the PEC
particle size
distribution. Other process variables such as temperature, pH, and the
presence of other
charged compounds during the formation of PECs can also have an affect. The
compositions
of the present invention can be produced by methods that allow for production
of PECs on a
large scale where the proper particle size distribution for mending split-ends
is achieved.
[0093] The formation of PECs may be facilitated by application of heat at a
certain stage,
e.g., when the anionic polymer is neutralized with a base and/or when the
cationic polymer is
added to the anionic polymer to produce the complex. A composition may be
preheated prior
to combining polymers, may be heated with one or a subset of polymers, or may
be heated
during or after combining all polymers for PEC formation. For PVMMA/polyquat-
28 PECs,
it has been found that heating neutralized PVMMA prior to addition of the
polyquat-28 is
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
34
advantageous, e.g., with the temperature ranging from at least 50 C to 60 C
or greater. The
temperature may range, e.g., as listed in the table below. In the table, an
"X" represents the
range "from [corresponding value in first row] to [corresponding value in
first column]." For
example, the first "X" is the range "from about 50 C to about 51 C."
[0094] Table 8
about about about about about about about about about about
50 C 51 C 52 C 53 C 54 C 55 C 56 C 57
C 58 C 59 C
about
X
51 C
about
X
52 C X
about
X X X
53 C
about
X X X X
54 C
abo ut
X X X X X
55 C
about
X X X X X X
56 C
about
X X X X X X X
57 C
about
X X X X X X X X
58 C
about
X X X X X X X X X
59 C
abo ut
X X X X X X X X X X
60 C
Thus, the temperature can have a range bounded by any two of the
aforementioned endpoints.
[0095] The compositions of the present invention may be prepared in a
single container
or may be prepared in separate containers, e.g., by preparing the PECs
separately from other
components prior to combining the PECs with the other components. The methods
described
herein produce PECs of the same size, morphology, and stability as
conventional methods,
yet do so with reduced numbers of containers.
[0096] The step of adding a cationic polymer to the intermediate mixture
can include
adding a solution, e.g., an aqueous solution, of the cationic polymer to the
intermediate
mixture. The cationic polymer can be added to the intermediate mixture at any
suitable rate,
which can include, e.g., from about 0.3 kg/min per minute to about 1.0 kg/min
per minute
(e.g., if the period of addition is 10 minutes, the rates would be from about
3 kg/min to about
kg/min) and can include, e.g., those listed in the table below. In the table,
an
represents the range "from [corresponding value in first row] to
[corresponding value in first
column]." For example, the first "X" is the range "from about 0.3 kg/min per
min to about
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
0.4 kg/min per min."
[0097] Table 9
about about about about about about about
0.3 kg/min 0.4 kg/min 0.5 kg/min 0.6 kg/min 0.7 kg/min 0.8 kg/min 0.9 kg/min
per min per min per min per min per min per min per
min
about
0.4 kg/min X
per min
about
0.5 kg/min X X
per min
about
0.6 kg/min X X X
per min
about
0.7 kg/min X X X X
per min
about
0.8 kg/min X X X X X
per min
about
0.9 kg/min X X X X X X
per min
about
1.0 kg/min X X X X X X X
per min
Thus, the addition can have a range bounded by any two of the aforementioned
endpoints.
[0098] The foHnation of PECs depends on the mixing speed and mixing
duration when
one polymer is added to another. A high shear force can be used for complete
mixing.
However, depending on the polymer-polymer systems, the mixing speed may have
to be
adjusted for proper PEC foimation. For PVMMA/polyquat-28 PECs, the polyquat-28
can be
first mixed prior to addition of the PVMMA for, e.g., 5 minutes, 10 minutes,
20 minutes, 25
minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes. The polyquat-28
can be added
to the PVMMA over a period of, e.g., 5 minutes, 10 minutes, 20 minutes, 25
minutes, 30
minutes, 40 minutes, 50 minutes, or 60 minutes. The polyquat-28 can be added
to the
PVMMA over a period of 30 minutes. The rate of addition can be any suitable
rate in which
PECs are formed. The rate can be determined based on the time needed for the
period of
addition. For example, the rate can be based on the amount added per minute
per minute of
the period of addition. For PVMMA/polyquat-28 PECs, this can be from about 0.4
kg/min
per minute to 1.0 kg/min per minute. Thus, if the period of addition is 10
minutes, the rates
would be from about 4 kg/min to about 10 kg/min. After the addition of the
polymer, mixing
can occur for over a period of, e.g., 5 minutes, 10 minutes, 20 minutes, 25
minutes, 30
minutes, 40 minutes, 50 minutes, or 60 minutes. The mixing can include a
combination of
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
36
mixing before, during, and/or after addition of the polyquat-28. Thus, the
intermediate
mixture of PVMMA can be mixed for at least about 10 minutes prior to addition
of the
cationic polymer, at least about 10 minutes after addition of the cationic
polymer, or a
combination thereof.
[0099] Some embodiments of the compositions of the present invention
include
compositions with the formulations of PVMMA and polyquat-28 as in Table 10.
[0100] Table 10
wt. % active PECs: 1% 2% 4% 6% 8%
Water 7.775 15.55 31.1 46.65 62.2
PVM/MA Copolymer 0.1 0.2 0.4 0.6 0.8
Sodium Hydroxide, Water (20%
active) 0.125 0.25 0.5 0.75 1
Polyquatemium-28, Water (20%
active) 4.5 9 18 27 36
*Remainder of composition* 87.5 75 50 25 0
Total 100 100 100 100 100
[0101] The present invention provides for mixing in additional ingredients
after PEC
formation, wherein the mixing is sufficient to allow adequate incorporation of
the one or
more components.
[0102] The present invention provides a one-container process for producing
a PEC,
which is highly efficient, cost effective, and eliminates the additional time
and labor required
to transfer materials from one tank to another as is done in conventional PEC
production
processes. Accordingly the process of the present invention is particularly
suitable for
manufacturing PECs and hair care compositions containing PECs on a commercial
scale, e.g.,
about 500 to about 10,000 gallons.
[0103] The
process of the present invention further provides for the production of PEC
compositions (e.g., at 8 wt. %) at concentrations that substantially exceed
the concentration
of PEC compositions which have been produced conventionally. Increasing the
concentration at which PECs are produced has several advantages. The higher
concentration
allows for a smaller pre-mix tank to be used in connection with combining the
PECs with
other ingredients to produce hair care products, e.g., conditioners. Also,
PECs can be
prepared and stored for future use, and less storage space is needed for a
more concentrated
stock. Furthermore, fewer quality control steps would be required in that one
batch of PECs
could be prepared and tested at a higher concentration instead of preparing
multiple batches
at lower concentrations, requiring additional testing. Additionally, if a PEC
stock is used for
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
37
preparing a hair care composition, the PEC stock will not require as much
volume in a
processing container, allowing for the addition of a greater volume of other
ingredients and
allowing for higher concentrations to be achieved for additional ingredients.
For example,
the Applicants have found for preparing PVMMA/polyquat-28 PECs, it is not
necessary to
dilute the polyquat-28 (e.g., Conditioneze NT-20 which is commercially
available at a
concentration of 20% actives). Rather, in accordance with the present
invention,
PVMMA/polyquat-28 PECs can be prepared in a single container by directly
adding
Conditioneze NT-20 at full strength to the PVMMA copolymer, which surprisingly
produces
a stable PEC at high concentration. Further, Applicants have found that the
higher PEC
concentration in the compositions produced in accordance with the present
invention are
substantially more likely than conventional PEC compositions of lower
concentration to form
stable emulsions with other ingredients used to produce hair care products
such as, e.g.,
conditioners.
[01041 The present invention provides a method of graphically
reconstructing the repair
process in the mending of a split-end of a hair fiber. In one embodiment the
method includes
securing a hair fiber to a surface, wherein the hair fiber secured to the
surface has a split-end
or is damaged while on the surface to produce a split-end; associating the
surface with a
magnifying device, wherein the split-end is positioned within the field of
view of the
magnifying device; associating an image capture device with the magnifying
device so as to
capture an enlarged image of the field of view of the magnifying device;
treating the spilt-end
with a composition, wherein the composition repairs the split-end and wherein
the split-end
fuses together; and via the image capture device associated with the
magnifying device,
capturing an image of the repair of the split-end during treatment with the
composition, and
storing a representation of the captured image of the repair for subsequent
retrieval. The
method of graphically reconstructing hair mending in accordance with the
present invention
includes using video to record the hair mending process in real-time.
Desirably the hair
mending process is recorded using a video device adapted to record the
reparation process, in
real-time, at a magnification sufficient to visualize the reparation process
with the naked eye,
e.g., at 20-50X magnification. The video can be stored on a recording media,
using methods
that are well known to those of ordinary skill in the art, for subsequent
retrieval.
[0105] Additionally, the methods of the present invention may include
securing a hair
fiber to a surface, wherein the hair fiber secured to the surface has a split-
end or is damaged
while on the surface to produce a split-end. The hair fiber, thus, may have a
split-end prior to
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
38
securing it to the surface, or a split-end can be induced (for example, by
mechanical means)
after the hair fiber is secured to the surface. The surface may be any surface
that can be
associated with a magnifying device. Such a surface can include, for example,
a table top or
a microscope slide. The properties of the surface can be determined by the
type of
magnifying device used. For example, if a light microscope is used wherein
light is
transmitted through a sample, a transparent surface, e.g., a microscope slide,
may be used.
As another example, the surface may be a stage on which the hair fiber rests.
As yet another
example, if the magnifying device is a simple lens, such as a magnifying
glass, the surface
can be a table top. Nothing should interfere with the mending of the split-
end. For example,
cover slips for microscope slides should not be used if the slip would prevent
the ends of the
split-end from coming together.
[0106] The hair fiber can be secured by any suitable means, including, for
example, using
one or more clamps. The hair fiber can also be secured using tape, for
example, when using a
table top or a microscope slide. As long as the split of the hair fiber can be
observed with the
magnifying device, any suitable means may be used for securing (e.g.,
fastening) the hair
fiber to the surface.
[0107] The methods of the present invention can include associating the
surface with a
magnifying device, wherein the split-end is positioned within the field of
view of the
magnifying device. The magnifying device may be, for example, a magnifying
glass, a
microscope (e.g., a light microscope). Each magnifying device has a field of
view. "Field of
view" means the image area that the magnifying devices magnifies for
observation. The
split-end is positioned within the field of view such that the split-end is
magnified for
observation.
[0108] The methods of the present invention can include associating an
image capture
device with the magnifying device so as to capture an enlarged image of the
field of view of
the magnifying device. The image capture device can be, for example, a digital
recorder.
The image capture device also can be analog. Non-limiting examples of image
capture
devices include still cameras, video cameras, charge-coupled device (CCD)
cameras, digital
cameras and/or camcorders, or any other similar recording device.
[0109] The methods of the present invention can include treating the spilt-
end with a
composition, wherein the composition repairs the split-end and wherein the
split-end fuses
together. Treatment may include, for example, massaging the composition into
the hair.
Treatment also may include, for example, rinsing the hair to remove the
composition, such as
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
39
with a rinse-off composition. The composition may be allowed to remain on the
hair, for
example, when using a leave-in composition. The method of treatment may be any
suitable
method, including methods described herein. The composition may be any
suitable
compositions, including compositions described herein.
101101 The methods of the present invention can include a step where, via
the image
capture device associated with a magnifying device, capturing an image of the
repair of the
split-end during treatment with the composition, and storing a representation
of the captured
image of the repair for subsequent retrieval. The image capture device can
capture the repair
of the split-end using any suitable means. For example, if the image capture
device is a
digital recorder, the digital recorder may generate an electronic file. As
another example, if
the image capture device is a camera, the camera may capture the repair using
photographic
film.
10111] Storage of a representation of a captured image of repair for
subsequent retrieval
may be through any suitable means. For example, this may include storing an
electronic
representation of the image, for example, using an electronic file accessible
on a digital
camera and/or computer. This may also be through the use of photographic film.
101121 Furthermore, the present invention can be used for any method of
communicating
to consumers. These may include, for example, the use of still photographs
(e.g., before and
after photographs); diagrams, depictions, and/or drawings; computer animation;
and/or in-
vivo/in-vitro/in-situ video using actual human hair fiber or analogues (e.g.,
sheep wool).
Additionally, the methods of communication can be in print, on television, on
the Internet, in-
store, in-person (e.g., live demonstrations), and/or on social media. The
methods of the
present invention also can be used for the explanation of a binding mechanism
(e.g., PECs
shrinking to draw together two ends of a split-end).
[0113] The present invention also provides a method of quantitatively
assessing the
degree of split-end hair fiber repair, the method comprising obtaining a tress
of hair,
preferably twice-bleached hair; producing at least one spilt-end of a hair
fiber in the tress
(e.g., by combing and/or blow drying the tress sufficiently to produce split-
ends); removing at
least one hair fiber having a split-end from the tress; optionally marking the
at least one
removed hair fiber; capturing a first image of the split-end of the at least
one removed hair
fiber; associating the hair fiber with the tress from which the hair fiber was
removed; treating
the tress and the hair fiber with a composition; removing the hair fiber from
the tress;
capturing a second image of the end of the hair fiber, wherein the end is the
same end
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
captured for the first image of the split-end of the at least one removed hair
fiber; assigning a
value of 0 for no repair of the split-end, 'A for partial repair, or 1 for
complete repair; and
summing the assigned numbers for all marked hair fibers and dividing the sum
by the total
number of marked hair fibers. Exemplary compositions of the present invention,
when
assessed according to this method can achieve an average value of, e.g., 0.85
or greater, e.g.,
0.925, 0.95, and even 0.975 based on an assessment of 20 fibers.
[0114] The methods of the present invention can include producing split-
ends. This may
include combing and blow drying the tress of hair to produce at least one hair
fiber of the
tress having a spilt-end. Other methods include selecting split-ends
naturally. For example,
hair samples may be attained from live specimens wherein the hairs are already
split. Due to
variety, however, this method may cause data to have poor reproducibility.
[0115] The methods of the present invention can include marking at least
one removed
hair fiber of the tress of hair. The split-end can be marked right at the
beginning of the split.
If the mark is gone after treatment with the composition, this can indicate
that the split-end
broke off the hair fiber. When assigning a value to the fibers, then, this
fiber can be excluded
since the split-end neither remained as a split-end nor was repaired. Thus,
e.g., false positives
can be avoided when assessing the mending ability of a composition.
[0116] The methods of the present invention can include the capturing an
image of the
split-end of at least one removed hair fiber. Examples of such capturing
methods are
described herein. This step may include storing an electronic representation
of the image, for
example, using an electronic file accessible on a digital camera and/or
computer.
[0117] The methods of the present invention can include associating the at
least one
marked hair fiber with the tress from which the hair fiber was removed.
Replacing the
removed hair fiber back with the tress provides a more natural environment for
testing the
mending ability of a composition. The hair fibers with split-ends remain with
other hair
fibers that may not have split-ends and remain within a larger grouping of
hair fibers. This
situation better simulates the environment of a normal lock of hair, e.g., on
a human head.
Simply removing the hair fibers with split-ends and testing compositions on
these removed
fibers would only provide results based on an artificial environment. Thus,
when using the
method to test compositions for use by consumers, the present invention allows
for reporting
results that are meaningful to those consumers, e.g., results that report on
the mending of hair
fibers that are in an environment important to the consumers.
[0118] The methods of the present invention can include treating the tress
and the at least
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
41
one marked hair fiber with a composition. Treatments may include, for example,
massaging
the composition into the hair. Treatment also may include, for example,
rinsing the hair to
remove the composition, such as with a rinse-off composition. The composition
may be
allowed to remain on the hair, for example, when using a leave-in composition.
The method
of treatment may be any suitable method, including methods described herein.
The
composition may be any suitable compositions, including compositions described
herein.
[0119] The methods of the present invention can include determining
parameters of hair
mending. For example, the rate at which a split-end is mended can be
determined under
defined conditions, e.g., those described herein. Compositions can then be
compared to
determine which provide for faster mending of split-ends. The split-end
mending efficacy of
the compositions used and/or tested also can be determined, e.g., using the
video methods
described herein. Mending of a split-end is preferable within one hour, less
than 50 minutes,
less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10
minutes, less
than 5 minutes, or less than 1 minute. The completion or amount of mending may
be 10% or
greater, 20% or greater, 30% or greater, 40% or greater, 50% or greater, 60%
or greater, 70%
or greater, 80% or greater, 90% or greater, or complete (e.g., about100%). The
mending can
be measured against a negative control or no treatment, wherein the treated
split-end can
show a statistically significant improvement in split-end mending (e.g.,
faster mending and/or
greater amount or completion of mending).
[0120] The methods of the present invention can include assigning a value
of 0 for no
repair of the split-end, 'A for partial repair, or I for complete repair and
summing the assigned
numbers for all marked hair fibers and dividing the sum by the total number of
marked hair
fibers. Thus, e.g., when there is an accounting for all of the split-ends of a
tress, the resulting
value will report on the ability of the composition to mend split-ends. A
composition with
poor mending ability will have a value that is low and/or approaches zero,
whereas a
composition with better mending ability will have a value that is higher
and/or approaches
one. Compositions thus may be compared using the method of the present
invention where a
composition that results in a higher value provides better mending than a
composition that
results in a lower value.
[0121] Any type of split-end can be mended by the methods of the present
invention.
One type of split-end includes, for example, the primary split-end. With this
type of split-
end, the hair fiber contains a single split along the longitudinal axis of the
hair fiber,
producing two ends of the hair fiber. Another example of a split-end includes
the double Y
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
42
split-end, which is created by an additional split along the longitudinal axis
of an end of a
primary split. The tree split-end is an example of a split-end where there are
several double
Y splits within one hair fiber. Another example of a split-end is where the
end of a hair fiber
has many short splits that feather out, often resulting in fiber shafts of
varying thickness.
Another example of a split-end is the long split-end where one side of a
primary split end is
significantly longer than the other (e.g., one side broke off). The taper
split-end is another
example of a split-end where only a portion of the hair fiber remains at the
end. Split-ends
also may, for example, be characterized by the number of ends, such as with
the triple split-
end with two splits of the hair fiber. A deep split-end is an example of a
split that occurs at
the mid-point of a hair shaft (not necessarily the end). A baby split-end is
an example of a
split-end that only has a small split in the hair fiber. The term "split-ends"
as used herein also
can include splits that do not extend to the end of the hair fiber. An example
of such a split is
an incomplete split. Figures 4A-4D show some types of split-ends.
[0122] The hair fibers used in the methods of the present invention may be
of any
mammalian hair. In one embodiment, the hair is human hair. Human hair of any
nationality,
region, or ethnicity may be used, e.g., European, Asian, African, or
Caucasian. In an
embodiment, the hair is European hair. The hair may have any type of damage
due to, e.g.,
bleaching once, bleaching twice, bleaching more than twice, dyeing, or
mechanical damage.
The hair fibers may have no damage, for example, as with virgin hair.
Additionally, the type
of hair used in the methods of the present invention can be varied from one
run of the method
to another. This varying of the hair can correspond to the use and testing of
various
compositions, which can, e.g., depend on what type of results are desired to
be communicated
to consumers. Varying the hair type and/or composition will allow for the
communication of
results for any hair type and any hair care composition.
[0123] An aspect of the present invention includes selecting a hair fiber
with a split end
and cutting to, e.g., about 1-1.5 inch in length (measuring from the split end
side). A small
piece of clear tape can be used to secure the fiber on, for example, a glass
slide. The glass
slide can be placed under a microscope with, e.g., 50X magnification and that
has an
interface with a camera and computer. Lighting and focus can be adjusted
accordingly.
Depending on set-up, a recording can take place within the computer interface
or a video
camera can be set-up on, e.g., a tripod pointing at the computer screen. With
the camera
recording, one drop of a composition, e.g., containing 2% active complex can
be applied over
the split-end using a micropipette. Lighting and focus can be further adjusted
accordingly. A
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
43
blow drier can be turned on, e.g., medium heat and aimed toward the split end.
Recording
can take place during and until the split end has fully or partially mended.
[0124] An aspect of the invention includes taking human hair, preferably
damaged, most
preferably twice-bleached European hair, and assembling into, e.g., wax bound
strips that
may be, for example, 1-1.5 inches wide. These tresses are then combed many
thousands of
times while a blow dryer is pointed perpendicularly to brushing to form an
appropriate
number of split- ends. A select number (for example, 10-20) of fibers with
split-ends are
selected and pulled out of the fiber assembly. Pictures of each split-end are
taken with the
use of a microscope at 20-50X magnification. Brass ferrule tabs are clamped on
the end
opposite of the split-end of each fiber. These brass tabs are then labeled and
placed between
two pieces of masking tape. The assembly is then inserted into the middle of
the hair tress
and a paper clamp is affixed to keep the assembly in place. The tress is then
treated with a
rinse-out split-end mending composition for a series of, e.g., three cycles.
After the final
cycle, the clamp is removed and new pictures of the split-ends are taken. By
comparing the
before and after pictures, an evaluator can give a value of "0" for no
mending, "1/2" for
partial mending, and "1" for complete mending. Summing these numbers and
dividing by the
total number of fibers allows for the expression of the degree of split-end
repair.
[0125] As noted above, an image capture system is used in an embodiment of
the
invention to produce a representation of the appearance of the split end both
before and after
repair or attempted repair. While various such image capture systems are
possible within the
scope of the teachings herein, an exemplary such system is shown in FIG. 6. In
particular,
FIG. 6 is a schematic diagram showing an image data capture system in which
the described
image capture and processing steps may be executed.
[0126] The illustrated system 600 comprises a number of interacting
components,
including a sample support device 601, such as a platform or surface suitable
for supporting a
sample 602. The sample support device 601 may be transparent to allow under-
lighting, via a
light source 603. The light source 603 may also be situated above the support
device 601 to
provide illumination via reflectance.
[0127] An electrical image capture device 604 is provided for capturing an
enlarged
image or video sequence of the sample 602 under treatment. In this regard, a
magnification
device 605 is provided adjacent the sample support device 601, between the
sample support
device 601 and the image capture device 604. The image capture device 604 may
be a still
camera or video camera adapted to capture a sequence of images. The
magnification device
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
44
605 may be an optical magnifying lens or lens arrangement such as an optical
microscope, or
may be an electronic magnification device such as an electron microscope or
the like. In an
embodiment of the invention, the image capture device 604 and/or the
magnification device
605 may be scannable to capture images of different regions or segments of the
sample 602.
[0128] An auxiliary computing and data capture device 606 is provided from
controlling
and receiving data from the image capture device 604. The auxiliary computing
and data
capture device 606 is a com-putting a processing device able to receive
electronic image data
from the image capture device 604 and send control signals to the image
capture device 604
to cause image capture. The auxiliary computing and data capture device 606
may also
control the illumination device 603.
[0129] In an embodiment of the invention, the auxiliary computing and data
capture
device 606 is communicably linked to an electronic database 607, either
locally or remotely
via a wired or wireless link. In this manner, the auxiliary computing and data
capture device
606 is able to gather data from the image capture device 604 and to store the
gathered data in
the electronic database 607 for later analysis, manipulation, and/or
retransmission, e.g., to a
printing or publishing facility (not shown).
[0130] The auxiliary computing and data capture device 606 may be a
computer such as a
person computer, laptop computer, workstation or the like, and operates by the
computer-
execution of computer readable instructions stored on a computer-readable
medium. The
computer-readable medium is a tangible medium such as a magnetic or optical
disc system,
flash drive, PRO, etc. Thus, the steps discussed herein that involve the
capture, manipulation,
and/or transmission of data are executed in this manner. A user interface 608
allows a user to
receive information from the auxiliary computing and data capture device 606
in human
understandable form and to provide input to the device in computer
understandable form. In
an embodiment of the invention, the user interface 608 includes a graphical
user interface on
a screen and a keyboard, keypad, stylus pad, mouse, and/or other user input
mechanism.
[0131] In one embodiment of the present invention, the image capture device
is a video
camera adapted to record reparation of one or more hair shafts, e.g., a hair
shaft containing
one or more split-ends, in real-time. Desirably, the video is recorded at
magnification
sufficient to visualize with the naked eye the hair reparation process in real-
time. Suitable
magnification can include, e.g., 20-50X magnification.
[0132] The following examples further illustrate the invention but, of
course, should not
be construed as in any way limiting its scope.
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
EXAMPLE 1
[0133] This example demonstrates production of hair care compositions
comprising a
polyelectrolyte complex using a two-tank process.
[0134] Compositions 1A-1C
Ingredient Composition 1A Composition 1B
Composition 1C
(Conditioner) (Overnight (Leave-in
(wt. %) Crème) Crème)
(wt. %) (wt. %)
Water 15.55 15.55 15.55
PVMMA Copolymer 0.2_ 0.2 0.2
Sodium Hydroxide (20%),Water 0.25 0.25 0.25
Polyquaternium-28 (20%), Water 9 9 9
Water 43.3997 48.7997 52.7997
Disodium EDTA (99.3% 0.05 0.05 0.05
EDTANa2*2H20 in water)
Aspartic Acid 0.75 0.75 0.75
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 4 1 1
Stearyl Alcohol 1 0 0
Glyceryl Stearate 1 0.2 0.2
Aminopropyl Dimethicone, Water 0 0.5 0
PPG-3 Benzyl Ether Myristate 2 0 0
(Crodamol STS)
Propylene Glycol 10 10 0.5
Water 4 4 8
Fluid Blend 5 0 0
Abe OSW 5 0 2 0
Dimethicone 0 1 2
DC-8500 0 1 0
Parfum (Fragrance) 0.6 0.5 0.5
DMDM hydantoin, water 0.2 0.2 0.2
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
Keratin Amino Acids, Water 0.0001 0.0001 0.0001
Flower/Leaf extract 0.0001 0.0001 0.0001
Salcare SC 96 1 3 3
Glycerin, USP VEG 0 0 1
Cyclopentasiloxane, Dimethiconol 0 0 1
Phenyl Trimethicone 0 0 2
[0135] One of ordinary skill in the art would be able to detemine the
proper RPM
settings for the mixers as listed in this Example and other Examples based on
the identity of
the particular tanks to be used in following the listed protocols.
[0136] In a suitable, stainless steel premix tank, charge water set at 113-
131 F (45-55
C). Begin vigorous turbine mixing (turbine mixer at vigorous clockwise
direction; side
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
46
sweep mixer off). Once the batch temperature is 86 F (30 C) or above, and
with vigorous
mixing, slowly add PVMMA Copolymer (Gantrez S-97 BF; ISP, Wayne, NJ, USA) to
the
premix tank. Adjust mixing accordingly in order to achieve vigorous agitation
without
creating excessive foam on the liquid surface. Once all of the powder has been
added, use
water set at 113-131 F (45-55 C) to rinse the mixing blades and side walls.
Once the rinse
is completed, turn on the side sweep agitator and begin heating to 122-131 F
(50-55 C).
(The powder lumps will disperse more quickly when the premix is 113-131 F (45-
55 C)).
Continue heating and maintain the temperature throughout the mix time. Set the
mixer
(turbine mixer at vigorous counterclockwise direction; side sweep mixer at
moderate
clockwise direction).
101371 Mix the batch for a minimum of 20 minutes or until no particles or
lumps are
present.
101381 Once the premix is uniform and free of lumps, reduce turbine mixing
to moderate.
Add the sodium hydroxide to the premix tank and mix for 10 minutes. The
solution will have
a low viscosity and will appear slightly hazy. (Mixer settings: turbine mixer
at moderate
counterclockwise direction; side sweep mixer at moderate clockwise direction.)
Mix the
batch for a minimum of 10 minutes or until completely uniform.
[0139] Once the batch is uniform, submit a sample for an in-process pH
test. Continue to
retest the sample until a stable pH reading of 6.9-7.0 is achieved. If pH is
low, add additional
sodium hydroxide 20% to meet the specification range. Remix and resample. If
pH is high,
add additional aspartic acid to meet specification range. Remix and resample.
101401 Once the Gantrez has been completely hydrated and the pH is within
specification, check that the premix temperature is 122-131 F (50-55 C).
Heat if necessary.
Once the premix is 122-131 F (50-55 C), turn off the side sweep agitator,
reverse turbine
direction and increase turbine mixing speed to create a vortex (turbine mixer
at vigorous
clockwise direction; side sweep mixer off).
10141] Slowly add the polyquatemium 28 (Conditioneze NT-20 (20% active);
ISP,
Wayne, NJ, USA) to the premix vessel. Add slowly to the premix vessel for the
proper
polyelectrolyte complex particle size. Use a drum spout to regulate addition
flow rate. Do
not dump the entire open container into the premix vessel at once. During this
material
addition, the premix will become very viscous and begin to turn white. Once
all of the
material has been added, the solution will again thin out and appear milky in
appearance.
101421 Reverse turbine direction and turn on side sweep agitator. Mix
vigorously for 20
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
47
minutes or until the premix is completely uniform (turbine mixer at vigorous
counterclockwise direction; side sweep mixer at moderate clockwise direction).
Mix the
batch for a minimum of 20 minutes or until no visible particles or lumps are
present.
[0143] Once the mix is complete, take a sample and visually inspect the
premix. Check
that it is completely white and not hazy or gray. Also check that the premix
viscosity is thin
and milk-like and not too viscous. If the premix is not thin and milky white,
continue mixing
vigorously for an additional 20 minutes and resample.
[0144] Once the premix is completely unifomi, reduce agitation and begin
cooling to 86-
113 F (30-45 C). Maintain mixing and temperature until the premix is ready
to be added to
the main compounding tank (turbine mixer at moderate counterclockwise
direction; side
sweep mixer at moderate clockwise direction).
[0145] Into a main stainless steel compounding tank, charge water set at
180-185 F (82-
85 C) with moderate mixing (turbine mixer at moderate counterclockwise
direction; side
sweep mixer at moderate clockwise direction). Slowly add the disodium EDTA and
aspartic
acid to the main compounding tank. After the items have been added, begin
heating the batch
to 180-185 F (82-85 C), as necessary (turbine mixer at moderate
counterclockwise
direction). Continue heating the batch to 180-185 F (82-85 C). Mix the batch
for a
minimum of 5 minutes or until the solids are completely dissolved.
[0146] Once the batch temperature is 176 F (80 C) or above, add the
stearamidopropyl
dimethylamine to the main compounding tank and mix until it is completely
incited (turbine
mixer at moderate counterclockwise direction; side sweep mixer at moderate
clockwise
direction). Continue heating the batch to 180-185 F (82-85 C). Mix the batch
for a
minimum of 5 minutes or until the solids are completely melted.
[0147] Once the batch temperature is 180-185 F (82-85 C), add the
following items to
the main compounding tank: cetyl alcohol, stearyl alcohol, glyceryl stearate,
and PPG-3
benzyl ether myristate for Composition IA (conditioner); cetyl alcohol,
glyceryl stearate, and
aminopropyl dimethicone for Composition 1B (overnight crème); cetyl alcohol
and glyceryl
stearate for Composition 1C (leave-in crème). Once the batch temperature is
again 180-185
F (82-85 C), maintain this temperature and mix for a minimum of 30 minutes
(turbine
mixer at moderate counterclockwise direction; side sweep mixer at moderate
clockwise
direction). Mix the batch while holding it between 180-185 F (82-85 C).
[0148] Take a sample from the main compounding tank and visually verify
that all of the
solids have been melted and that the batch is smooth and uniform. If there
remains any non-
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
48
dissolved materials or particles, continue vigorous mixing and resample.
101491 Begin cooling the batch to 104-113 F (40-45 C) and reduce the
turbine and side
sweep agitator speeds to moderate/slow to help de-aerate the batch (turbine
mixer at
moderate counterclockwise direction; side sweep mixer at slow clockwise
direction). While
cooling and once the batch temperature is 167 F (75 C) or below, add the
propylene glycol
to the main compounding tank (turbine mixer at moderate counterclockwise
direction; side
sweep mixer at moderate clockwise direction). For Composition 1C (leave-in
creme), also
add glycerin at this mixing speed.
[0150] Once the main batch temperature is 150 F (65 C) or below for
Composition IA
(conditioner) or 131 F (55 C) or below for the crèmes turn off the side
sweep agitator,
reverse the direction of the turbine agitator, and increase mixing to create a
slight vortex
(turbine mixer at moderate clockwise direction; side sweep mixer off). Add the
Salcare SC-
96 (65% polyquaternium-37, 25% propylene glycol dicaprylate/dicaprate, 10% PPG-
1
trideceth-6; Ciba/BASF, Basel, Switzerland) to the main compounding tank and
continue
cooling to 104-113 F (40-45 C). (Mix Salcare SC-96 well in its container
prior to addition
to the batch.)
[0151] Once all of the material has been incorporated into the batch and is
no longer
sitting on the surface, reverse turbine agitator and turn on side sweep
agitator (turbine mixer
at moderate counterclockwise direction; side sweep mixer at moderate clockwise
direction).
[0152] Once the main batch temperature is 150 F (65 C) or below for
Composition lA
(conditioner) or 131 F (55 C) or below for Composition 1B (overnight crème),
and the
premix is ready, add the premix to the main compounding tank. While the premix
is being
added, turn off the turbine mixer or reduce it to slow as the liquid level
passes the top set of
turbine blades to minimize aeration. Once the premix has been added, rinse the
premix tank
with water set at 77-95 F (25-35 C) and add it to the main compounding tank.
The batch
viscosity will decrease as the premix is mixed into the batch. Adjust mixer
speeds
accordingly to avoid splashing (turbine mixer at moderate counterclockwise
direction; side
sweep mixer at moderate clockwise direction).
[0153] For Composition lA (conditioner), mix the batch for a minimum of 15
minutes or
until the batch is uniform. Once the main batch temperature is 122 F (50 C)
or below, add
the Fluid Blend directly to the main compounding tank. Mix well during
addition. Increase
mixing as necessary to mix in the silicone turbine mixer at vigorous
counterclockwise
direction; side sweep mixer at moderate clockwise direction).
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
49
[0154] For the crèmes, once all of the premix has been added, charge with
water set at
77-95 F (25-35 C) below the surface of the batch, to minimize aeration, if
possible. Mix
the batch for a minimum of 15 minutes or until the batch is uniform. Continue
cooling to
104-113 F (40-45 C). In a suitable stainless steel phase vessel or
container, premix the
following silicone itcms with vigorous agitation: Abil OSW 5 (84%
cyclopentasiloxane,
15% dimethiconol, 1% dimethicone), and dimethicone (60,000 est) for
Composition 1B
(overnight crème); dimethiconc (60,000 cst), phenyl trimethicone (DC-556; Dow
Corning),
and D5 dimethiconol (DC- 1501) for Composition 1C (leave-in crème). Once the
silicone
premix is uniform, add it to the main compounding tank and allow the silicone
premix
container to drain out as much as possible into the main batch tank. Increase
mixing as
necessary to mix in the silicones (turbine mixer at vigorous counterclockwise
direction; side
sweep mixer at moderate clockwise direction).
101551 When the batch temperature is 113 F (45 C) or below, add the
following
ingredients to the main compounding tank: fragrance (parfum), DMDM hydantoin,
cocos
nucifera oil, keratin amino acids, flower/leaf extract. For the Composition 1B
(overnight
crème), also add DC-8500 (82% Bis(C13-15 alkoxy) PG-Amodimethicone, 18% C14-15
alcohols; Dow Corning, Midland, MI, USA). Continue mixing and cooling to 95-
104 F (35-
40 C).
[0156] Mix vigorously for a minimum of 45 minutes or until all of the lumps
have been
removed and the batch is smooth and uniform. The batch may be recirculated
through an 80
Mesh Filter throughout this Final Mix to help break down the lumps. Although
shear
(increased mixing and/or recirculating) is needed to break down the lumps,
minimize aeration
as much as possible (turbine mixer at vigorous counterclockwise direction;
side sweep mixer
at moderate clockwise). Mix for a minimum of 45 minutes.
[0157] When the batch temperature is 95-104 F (35-40 C), analyze
sample(s).
Discontinue mixing and cooling.
[0158] Adjustments that may be made are the following. If the pH is low,
add sodium
hydroxide (20%) at a maximum of 5% of the total batch requirement. Remix and
resample.
If the pH is high, add aspartic acid at a maximum of 7.5% of the total batch
requirement.
Remix and resample. If the viscosity is low, mix additional 60 minutes and
resample. Batch
may also be recirculated through an 80 Mesh Filter.
[0159] Pumps that should be used for pumping material into the tanks
include air
diaphragm and positive displacement. Filters that should be used include 80
mesh for all
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
transfer operations. The fill temperature should be 90-99 F (32-37 C). Do
not reheat batch
if product temperature falls below 90 F (32 C).
[0160] Composition 1D
Composition
Ingredient 1D
(Spray)
(wt. %)
Water 93.33163
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.001
NaOH, 20% in water 0.00125
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20%
0.045
active), water
PVP 0.45
Disodium EDTA, Water 0.02
Stearalkonium Chloride, Water 1
[DC-949 Cationic Emulsion]
Amodimethicone, Trideceth-12, Cetrimonium 2
Chloride, Water
Glycerin 1
PEG-12 Dimethicone 0.5
Propylene Glycol 0.5
Triethanolamine 0.00001
Citric Acid 0.00001
DMDM Hydantoin, Water 0.3
Hydrolyzed Silk, Water 0.05
Water, Polysorbate 20, Ascorbic Acid, Panthenol,
0.001
Tocopherol Acetate, Biotin, Niacinamide
Water, Polyglycery1-3 Distearate, Polysorbate 60,
Myristic Acid, Palmitic Acid, Stearic Acid, Guar
Hydroxypropyltrimonium Chloride, Triticum Vulgare
(Wheat) Flour Lipids, Ceramide 3, Persea Gratissima
0.0001
(Avocado) Oil, Tetrahexyldecyl Ascorbate, Glycine
Soja (Soybean) Sterols, Alpha-Glucan
Oligosaccharide, Ethylhexyl Methoxycinnamate,
Butyl Methoxydibenzoylmethane, Tocopheryl Acetate
Polysorbate 20 0.4
Fragrance 0.4
[0161] Into a main stainless steel compounding tank, charge water, set at
95 - 104 F (30
- 35 C), and begin vigorous agitation (turbine mixer at vigorous
counterclockwise direction;
side sweep mixer at moderate clockwise direction, if available). Do not heat
the water to
maintain temperature. Slowly add the following items, in order, to the main
compounding
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
51
tank and mix vigorously (turbine mixer at vigorous counterclockwise direction;
side sweep
mixer at moderate clockwise direction, if available) for 10 minutes or until
the batch is
completely uniform and no lumps are present: PVM/MA copolymer (Gantrez S97BF),
NaOH, Polyquaternium 28 (Conditioneze). Mix the batch for a minimum of 10
minutes or
until the batch is completely uniform and no lumps are present.
[0162] With vigorous mixing (turbine mixer at vigorous counterclockwise
direction; side
sweep mixer at moderate clockwise direction, if available) add the following
ingredients to
the main compounding tank: PVP, disodium EDTA. Mix the batch for a minimum of
15
minutes or until the solids are completely dissolved and the batch is uniform.
[0163] After mixing, take a sample from the main compounding tank and
verify
that there are no lumps or particulates, and that the batch is smooth and
uniform. If there are
lumps or particulates, continue to mix and resample until the batch is smooth
and uniform.
[0164] Begin heating the batch to 170 ¨ 175 F (76 ¨ 79 C) with vigorous
agitation
(turbine mixer at vigorous counterclockwise direction; side sweep mixer at
moderate
clockwise direction, if available). Once the batch temperature is 150 F (65 C)
or above, add
the following ingredient to the main compounding tank: stearalkonium chloride.
Mix the
batch while holding it between 170 - 175 F (76 - 79 C). Mix the batch for a
minimum of 60
minutes.
[0165] Take a sample from the main compounding tank and visually verify
that there are
no lumps or particulates, and the batch is uniform. If lumps or particulates
are present,
continue to mix vigorously and resample until the batch is uniform.
[0166] Reduce agitation to moderate (turbine mixer at moderate
counterclockwise
direction; side sweep mixer at moderate clockwise direction, if available) and
begin cooling
the batch to 90 - 95 F (32 - 35 C).
[0167] While cooling, add the following ingredients, in order, to the main
compounding tank. Mix well after each addition: DC 949 cationic emulsion;
glycerin USP
VEG; PEG-12 dimethicone; propylene glycol; triethanolamine; citric acid.
[0168] Once the batch temperature is 113 F (45 C) or below, add the
following
ingredients, in order, to the main compounding tank: DMDM hydantoin;
hydrolyzed silk;
vitamin blend; polyglycery1-3-distearate mixture.
[0169] Into a separate stainless steel vessel or container equipped with an
electric or air
mixer, premix the following ingredients: polysorbate 20; fragrance. Blend this
premix
vigorously until all of the fragrance is solubilized and the premix is uniform
and clear.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
52
Charge this premix to the main compounding tank with moderate agitation. Rinse
the premix
vessel/container with cold water, set at 60 - 80 F (15 - 27 C), and add to the
main
compounding tank. Mix (turbine mixer at moderate counterclockwise direction;
side sweep
mixer at moderate clockwise direction, if available) for a minimum of 20
minutes or until the
batch is completely uniform.
[0170] Adjustments that may be made are the following. If the pH is low,
add
triethanolamine in 0.20% solution increments. If the pH is high, add citric
acid in 0.20%
solution increments.
[0171] Pumps that should be used for pumping material into the tanks
include air
diaphragm and positive displacement. Filters that should be used include 80
mesh for all
transfer operations. The fill temperature should be ambient. Batch may be
cooled as
necessary to facilitate filling.
[0172] Composition 1E
Ingredients Composition lE
(Shampoo)
(wt. %)
Water 31.5
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.001
Sodium hydroxide (20%), water 0.00125
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active), water 0.045
Polyquatemium-10, water 0.8
Water 0.025
Cocamidopropyl betaine 8.2
Disodium EDTA, water 0.1
Citric acid, USP 0.1
Sodium Laureth Sulfate, water 32
Disodium laureth sulfosuccinate, water 12.8
Glycol distearate, cocamidopropyl betaine, cocamide MEA, water 6
PEG-6 caprylic/capric glycerides 0.6
Fragrance 0.7
Methylchloroisothiazolinone, methylisothiazolinone, water 0.07
Cocos nucifera (coconut) oil 0.0001
Keratin amino acids, water 0.0001
Flower/leaf extract, propylene glycol, water 0.0001
Water 4.65745
Sodium chloride 1.5
Water 0.9
[0173] Into a
main stainless steel compounding tank, charge water, set at 68 - 86 F (20 -
30 C), where available, and begin vigorous agitation (turbine mixer at
vigorous
counterclockwise direction; side sweep mixer at moderate clockwise direction).
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
53
[0174] Slowly add the following items, in order, to the main compounding
tank
and mix vigorously (turbine mixer at vigorous counterclockwise direction; side
sweep mixer
at moderate clockwise direction) for 5 minutes or until the batch is
completely uniform and
no lumps are present: PVM/MA copolymer (Gantrez S97BF), sodium hydroxide
(20%),
Polyquaternium 28 (Conditioneze). Mix the batch for a minimum of 5 minutes or
until the
batch is completely uniform and no lumps are present.
[0175] Once the batch is uniform, slowly sprinkle the following item into
the main
compounding tank: Polyquaternium-TO. Use vigorous mixing to achieve a vortex,
where
possible. Rinse the inside of the tank and mixer blades with water (turbine
mixer at vigorous
counterclockwise direction; side sweep mixer at moderate clockwise direction).
[0176] Begin heating the batch to 113 - 122 F (45 - 50 C). While heating,
mix
for a minimum of 20 minutes, or until the polymer is completely hydrated and
the solution is
clear and uniform.
[0177] After mixing, take a sample from the main compounding tank and
verify that there
are no lumps or particles, and that the batch is smooth and homogeneous. If
there are lumps
or particles, continue to mix and resample until the batch is smooth and
uniform. While
continuing to heat, reduce turbine agitation (turbine mixer at moderate
counterclockwise
direction; side sweep mixer at moderate clockwise direction) and add the
following items, in
order, to the main compounding tank: cocamidopropyl betaine, disodium EDTA,
citric acid,
USP. Mix for a minimum of 10 minutes, or until the batch is unifolin and all
items are fully
dissolved.
[0178] Check that the batch temperature is 113 - 122 F (45 - 50 C). Then,
add the
following items to the main compounding tank, in order, with moderate
agitation (turbine
mixer at moderate counterclockwise direction; side sweep mixer at moderate
clockwise
direction). Use caution to avoid aeration, and slow the mixing during addition
if necessary:
sodium laureth sulfate; disodium laureth sulfosuccinate; glycol distearate,
cocamidopropyl
betaine, cocamidc MBA, water mixture; PEG-6 caprylic/capric glycerides. As the
level in the
tank increases, reduce the turbine mixer speed to SLOW when the level
approaches the
blades. Once the blades arc completely covered by the batch, increase the
turbine mixer
speed back to moderate. This will help to reduce aeration of the batch. Mix
the batch while
holding it between 113 - 122 F (45 - 50 C). Mix for a minimum of 20 minutes or
until the
batch is smooth and completely uniform.
[0179] De-aerate the batch by reducing both turbine and sweep agitation to
slow (turbine
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
54
mixer at slow counterclockwise direction; side sweep mixer at slow clockwise
direction) and
begin cooling the batch to 95 - 104 F (35 - 40 C).
[01801 Once the batch temperature is 113 F (45 C) or below, increase
turbine and sweep
agitation to moderate (turbine mixer at moderate counterclockwise direction;
side sweep
mixer at moderate clockwise direction) and add the following items, in order,
to the main
compounding tank: fragrance; methylchloroisothiazolinone,
methylisothiazolinone, water
mixture; coconut oil; keratin amino acids, flower extract.
[01811 In a separate stainless steel vessel or container, mix the sodium
chloride and
water, set at 95 - 104 F (35 - 40 C), until the salt is completely dispersed.
The salt may not
completely dissolve as there may not be enough Water available. Mix until the
salt is
completely dispersed and then continue.
10182] Once the salt premix is ready, add it to the main compounding tank
and mix until
the batch is completely unifolin (turbine mixer at moderate counterclockwise
direction; side
sweep mixer at moderate clockwise direction). With cold water, rinse the
premix vessel or
container and flush the transfer line. Add this rinse/flush water to the main
compounding
tank. Mix for a minimum of 30 minutes or until the batch is completely
uniform. Sample the composition. Discontinue mixing and cooling (if
applicable).
[0183] Adjustments that may be made are the following. If the viscosity is
low, add
sodium chloride. Do not exceed a total sodium chloride level of 2.00% in this
formula. If the
viscosity is high, add propylene glycol. If the pH is low, add sodium
hydroxide (20%). If the
pH is high, add citric acid.
[0184] Aerated batch: Reheat the batch to 120 - 125 F (48 - 52 C) and mix
slowly for 20 minutes. Cool back down to 95 - 100 F (35 - 38 C), add
back 10% preservative and add back fragrance if necessary.
[0185] Pumps that should be used for pumping material into the tanks
include air
diaphragm and positive displacement. Filters that should be used include 80
mesh for all
transfer operations. The fill temperature should be 90-100 F (32-38 C). Batch
may be
warmed to this temperature range to help facilitate filling.
[0186] Composition 1F
Ingredients Composition 1F
(Overnight Treatment
Crème)
(wt. %)
Water 15.45
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
Water 0.1
Sodium Hydroxide (20%), water 0.25
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20%), 9
water
Water 38.8497
Disodium EDTA, water (2 mol water per 1 mol 0.05
disodium EDTA)
Aspartic Acid 0.7
Stearamidopropyl Dimethylamine 2
Cetyl Alcohol 1
Glyceryl Stcarate 0.2
Aminopropyl dimethicone, water (2% max. water) 0.5
Propylene Glycol 10
Polyquatemium-37, propylene glycol 3
dicaprylate/dicaprate, PPG-1 trdeceth-6 (Salcare SC-
96)
Water 2
Water 12
Cyclopentasiloxane, dimethiconol, dimethicone (Abil 2
OSW 5)
Dimethicone 1
DC-8500 1
Fragrance 0.5
DMDM Hydantoin 0.2
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids, water 0.0001
Flower/Leaf Extract, propylene glycol, water 0.0001
[0187] Mix the Salcare SC-96 well in its container prior to being weighed
and prior to
addition to the batch.
[0188] In a suitable, stainless steel premix tank, charge water set at 113 -
131 F (45 -
55 C). Begin vigorous turbine mixing (turbine mixer at vigorous clockwise
direction; side
sweep mixer off).
[0189] Once the batch temperature is 86 F (30 C) or above, and with
vigorous mixing,
slowly add PVM/MA Copolymer (Gantrez S-97 BF) to the premix tank. Adjust
mixing
accordingly in order to achieve vigorous agitation without creating excessive
foam on the
liquid surface. Once all of the powder has been added, use water set at 113 -
131 F (45 -
55 C) to rinse the mixing blades and side walls. Once the rinse is completed,
turn on the side
sweep agitator (turbine mixer at vigorous counterclockwise direction; side
sweep mixer at
moderate clockwise direction) and begin heating to 122 - 131 F (50 - 55 C).
The powder
lumps will disperse more quickly when the premix is 113 - 131 F (45 - 55 C).
Continue
heating and maintain the temperature throughout the mix time. Mix the batch
for a minimum
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
56
of 20 minutes or until no particles or lumps are present.
[0190] Once the premix is uniform and free of lumps, reduce turbine mixing
to moderate
(turbine mixer at moderate counterclockwise direction; side sweep mixer at
moderate
clockwise direction). Add the sodium hydroxide to the premix tank and mix for
10 minutes.
The solution will have a low viscosity and will appear slightly hazy. Mix the
batch for a
minimum of 10 minutes or until completely uniform.
[0191] Once the batch is uniform, submit a sample for an in-process pH
test. Continue to
retest the sample until a stable pH reading is achieved. If pH is low, add
additional sodium
hydroxide (20%) to meet specification range. Remix and resample. If pH is
high, add
additional aspartic acid to meet specification range. Remix and resample.
[0192] Once the Gantrez has been completely hydrated and the pH is within
specification, check that the premix temperature is 122 - 131 F (50 - 55 C).
Heat if
necessary.
[0193] Once the premix is 122 - 131 F (50 - 55 C), turn off the side sweep
agitator,
reverse turbine direction and increase turbine mixing speed to create a vortex
(turbine mixer
at vigorous clockwise direction; side sweep mixer off). Slowly add the
Polyquaternium 28
(Conditioneze NT-20) to the premix vessel. Add slowly to the premix vessel for
the proper
complex particle size. This addition should take 10 - 15 minutes to be
completed. Use a
drum spout to regulate addition flow rate. Do not dump the entire open
container into
the premix vessel at once.
[0194] During this material addition, the premix will become very viscous
and begin to
turn white. Once all of the material has been added, the solution will again
thin out and
appear milky in appearance.
[0195] Reverse turbine direction and turn on side sweep agitator (turbine
mixer at
vigorous counterclockwise direction; side sweep mixer at moderate clockwise
direction).
Mix vigorously for 20 minutes or until the premix is completely uniform. Mix
the batch for a
minimum of 20 minutes or until no particles or lumps are present. Once the mix
is complete,
take a sample and visually inspect the premix. Check that it is completely
white and not hazy
or gray. Also check that the premix viscosity is thin and milk-like and not
overly viscous. If
the premix is not thin and milky white, continue mixing vigorously for an
additional 20
minutes and resample.
[0196] Once the premix is completely uniform, reduce agitation (turbine
mixer at
moderate counterclockwise direction; side sweep mixer at moderate clockwise
direction) and
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
57
begin cooling to 86 - 113 F (30 - 45 C). Maintain mixing and temperature until
the premix is
ready to be added to the main compounding tank.
[0197] Into the main stainless steel compounding tank, charge water, set at
180 - 185 F
(82 - 85 C), with moderate mixing (turbine mixer at moderate counterclockwise
direction;
side sweep mixer at moderate clockwise direction).
[0198] Slowly add the following items to the main compounding tank:
disodium EDTA;
aspartic acid. After the items have been added, begin heating the batch to 180
- 185 F (82 -
85 C), as necessary. (Turbine mixer at moderate counterclockwise direction;
side sweep
mixer at moderate clockwise direction). Continue heating the batch to 180 -
185 F (82 -
85 C). Mix the batch for a minimum of 5 minutes or until the solids are
completely
dissolved.
[0199] Once the batch temperature is 176 F (80 C) or above, add the
stearamidopropyl
dimethylamine to the main compounding tank and mix until it is completely
melted (turbine
mixer at moderate counterclockwise direction; side sweep mixer at moderate
clockwise
direction). Continue heating the batch to 180 - 185 F (82 - 85 C). Mix the
batch for a
minimum of 5 minutes or until the solids are completely melted.
[0200] Once the batch temperature is 180 - 185 F (82 - 85 C), add the
following items to
the main compounding tank: cetyl alcohol; glyceryl stearate; aminopropyl
dimethicone.
[0201] Once the batch temperature is again 180 - 185 F (82 - 85 C),
maintain this
temperature and mix for 30 minutes (turbine mixer at moderate counterclockwise
direction;
side sweep mixer at moderate clockwise direction). Mix the batch while holding
it between
180 - 185 F (82 - 85 C). Mix the batch for a minimum of 30 minutes.
[0202] After the hot mix, take a sample from the main compounding tank and
visually
verify that all of the solids have been melted and that the batch is smooth
and uniform. If
there remains any undissolved materials or particles, continue vigorous mixing
and resample
periodically until all of the waxes and particles are dissolved and the batch
is uniform.
[02031 After the hot mix, begin cooling the batch to 104 - 113 F (40 - 45
C) and reduce
the turbine and side sweep agitator speeds to moderate/slow to help de-aerate
the batch
(turbine mixer at moderate counterclockwise direction; side sweep mixer at
slow clockwise
direction).
[0204] While cooling and once the batch temperature is 167 F (75 C) or
below, add the
propylene glycol to the main compounding tank (turbine mixer at moderate
counterclockwise
direction; side sweep mixer at moderate clockwise direction).
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
58
[0205] Once the main batch temperature is 150 F (65 C) or below, turn off
the side
sweep agitator, reverse the direction of the turbine agitator and increase
mixing to create a
slight vortex (turbine mixer at moderate clockwise direction; side sweep mixer
off). Add the
Salcare SC-96 to the main compounding tank and continue cooling to 104 - 113
F (40 -
45 C).
[0206] Once all of the material has been incorporated into the batch and is
no longer
sitting on the surface, reverse turbine agitator and turn on side sweep
agitator (turbine mixer
at moderate counterclockwise direction; side sweep mixer at moderate clockwise
direction).
[0207] Once the main batch temperature is 131 F (55 C) or below, and the
PEC Actives
Premix is ready, add the premix to the main compounding tank. While the premix
is being
added, turn off the turbine mixer or reduce it to slow as the liquid level
passes the top set of
turbine blades to minimize aeration.
[0208] Once the premix has been added, rinse the premix tank with cold
water set at 77 -
95 F (25 - 35 C) and add it to the main compounding tank. The batch viscosity
will decrease
as the PEC Actives Premix is mixed into the batch. Adjust mixer speeds
accordingly to avoid
splashing (turbine mixer at moderate counterclockwise direction; side sweep
mixer at
moderate clockwise direction).
[0209] Once all of the PEC Actives Premix has been added, charge cold
water, set at 77 -
95 F (25 - 35 C) below the surface of the batch, to minimize aeration, if
possible. Mix the
batch for a minimum of 15 minutes or until the batch is uniform. Continue
cooling to 104 -
113 F (40- 45 C).
[0210] In a suitable stainless steel phase vessel or container, premix the
following items
with vigorous agitation: cyclopentasiloxane mixture; dimethicone. Once the
premix is
unifoini, add it to the main compounding tank and allow the premix container
to drain out as
much as possible into the main batch tank (turbine mixer at vigorous
counterclockwise
direction; side sweep mixer at moderate clockwise direction). Increase mixing
as necessary
to mix in the silicones.
[0211] When the batch temperature is 113 F (45 C) or below, add the
following
ingredients to the main compounding tank: DC-8500; fragrance; DMDM hydantoin,
coconut
oil, keratin amino acids, flower extract mixture. Continue mixing and cooling
to 95 - 104 F
(35 - 40 C).
[0212] Mix vigorously (turbine mixer at vigorous counterclockwise
direction; side sweep
mixer at moderate clockwise direction) for a minimum of 45 minutes or until
all of the lumps
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
59
have been removed and the batch is smooth and uniform. The batch may be
recirculated
through an 80 Mesh Filter throughout this Final Mix to help break down the
lumps.
Although shear (increased mixing and/or recirculating) should be used to break
down the
lumps, minimize aeration as much as possible. Mix for a minimum of 45 minutes.
When the batch temperature is 95 - 104 F (35 - 40 C), sample composition.
Discontinue
mixing and cooling.
[0213] Adjustments that may be made are the following. If the pH is low,
add sodium
hydroxide (20%) at a maximum of 5% of the total batch requirement. Remix and
resample.
If the pH is high, add aspartic acid at a maximum of 7.5% of the total batch
requirement.
Remix and resample. If the viscosity is low, mix an additional 60 minutes and
resample.
Batch may also be recirculated through an 80 Mesh Filter.
[0214] Pumps that should be used for pumping material into the tanks
include air
diaphragm and positive displacement. Filters that should be used include 80
mesh for all
transfer operations. The fill temperature should be 90-99 F (32-37 C). Do
not reheat batch
if product temperature falls below 90 F (32 C).
EXAMPLE 2
[0215] This example demonstrates production of hair care compositions
comprising a
polyelectrolyte complex using a one-tank process.
[0216] The process of Example 1 describes a two-tank process, where the
polyelectrolyte
complex is prepared in one tank, the remaining components are mixed in a
separate tank, and
the polyelectrolyte complex and the remaining components are combined. To
simplify the
process to one tank, the process is performed as described in Example 1,
except the
polyelectrolyte complex is first prepared in the tank and the additional
components are added
directly to the same tank after the polyelectrolyte complex forms. The final
viscosity of the
composition may be lower than if prepared in two tanks. To compensate, add
additional
Salcare SC 96.
EXAMPLE 3
[0217] This example demonstrates the compatibility of polyelectrolyte
complexes (PECs)
with certain charged compounds and polymers.
[0218] Visual Appearance: The visual appearance of PECs in solution with
charged
particles was characterized. When PVMMA and polyquat-28 are individually
solvated in
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
water, the compositions are clear. When PVMMA and polyquat-28 are present as
PECs
solvated in water, the composition becomes hazy and/or milky in appearance.
After adding
to the PECs another charged species that produces a clear composition when
solvated in
water, the milky/hazy opacity is expected to decrease (and in some cases turn
back to clear).
This is a visual indication of the PEC complexation process reversing. The
milky opaque
appearance of 1 wt. % and 2 wt. % PVMMA/polyquat-28 PECs disappears in the
presence of
greater than 0.5 wt. % polyquatemium-4 (Celquat L-200; Akzo Nobel, Amsterdam,
Netherlands). This indicates that the structure of the PECs has been
disrupted. Below 0.5 wt.
% Ceiquat L-200, the PECs are not disrupted. Celquat H-100 at 0.5 wt. % did
not disrupt
the PECs. Celquat L-200 and H-100 are similar, but L-200 has lower viscosity
and higher
cationic activity.
[0219] Thickening: Tinovis GTC/Acrylates/Beheneth-25 Methacrylate Copolymer
(2.3%) in compositions with and without PECs was tested. The composition
without PECs
gave a viscosity of 40,000-60,000 cps. The composition with PECs was water
thin. Since
Tinovis is an associative thickener and the composition without PECs did not
thicken, the
Tinovis was thought to be rendered ineffective by PECs.
102201 Split-end Mending: Table 11 shows charged compounds and polymers
that were
combined with PECs. These compositions showed no deleterious effects of split-
end
mending.
[0221] Table 11
Compound/Polymer Amount (wt. %)
Stearamidopropyl
Dimethyl amine 2
(neutralized with Aspartic Acid)
Bis(C13-15 Alkoxy) PG-
1
Amodimethicone
Aminopropyl Dimethicone 0.5
Polyquatemium-37 0.65-3.25
Polyquatemium-7 0.085
Polyquatemium-39 0.0425
DC 5-7113
(Silicone Quaternium-16 (and)
undeceth-11 (and) butyloctanol
1
(and) undeceth-5;
Dow Corning, Midland, MI,
USA)
Abil T Quat 60
(Silicone Quatemium-22; 1
Evonik, Essen, Germany)
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
61
Quaternium-80 0.5
Merquat 2001
(Polyquaternium-47; 0.5
Nalco, Naperville, IL, USA)
Vinyl
Caprolactum/VP/Dimethyl-
aminoethyl Methacrylate 0.25
Copolymer (in acid
environment)
N-Hance SP 100
(Acrylamidopropyltrimonium
0.1-0.2
Chloride/Acrylates Copolymer;
Aqualon)
Acrylic Acid/VP Crosspolymer 1
Varisoft EQ 65 (Distearoylethyl
Dimonium Chloride, Cetearyl 0.5
Alcohol; Evonik)
EXAMPLE 4
[0222] This example illustrates formulations comprising polyelectrolyte
complexes and
charged polymers.
10223] All Compositions 4B-4E exhibited freeze-thaw stability. The present
inventors
also surprisingly found that Composition 4D, which contains Salcare SC 96,
exhibited
superior long-term controlled viscosity (wherein the viscosity remained stable
long-term),
relative to Compositions 4B, 4C, and 4E.
[0224] Comparative Composition 4A does not include PECs, whereas
Compositions 4B-
4E comprise PVMMA:polyquat-28 PECs and charged compounds and/or polymers. All
compositions are rinse-out conditioners. The sodium hydroxide/citric
acid/aspartic acid are
adjusted to achieve the proper pH, if necessary.
102251 "MS" represents Match Standard.
[0226] Compositions 4A-4E
Ingredients
Comparative Composition Composition Composition Composition
Composition 4B 4C 4D 4E
4A (wt. %) (wt. %) (wt. %) (wt. %)
(wt. %)
DI Water 82.805 67.55 67.95 62.95 65.97
Citric Acid 0.1 0 0 0
L-Aspartic Acid 0.6 0.75 0.75 0.75 0.75
Stearamidopropyl 2 2 2 2 2
Dimethylamine
Cetyl Alcohol 2.714 7 5 4 4
Stearyl Alcohol 5.286 0 0 1 0
Glyceryl Stearate 0 1.4 1 1 0.8
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
62
Isostearamidopropyl 0.145 0 0 0 0
Ethyldimonium
Ethosulfate, PEG-9
Crodamol STS 0 0 0 2 0
Montanov 202 0 0 0 0 1.18
Propylene Glycol 0 10 10 10 10
PVMMA (Gantrez ¨ 0 0.2 0.2 0.2 0.2
S-97 BF)
NaOH (20% active) 0 0.25 0.25 0.25 0.25
Polyquaternium-28 0 9 9 9 9
(Conditioneze NT-
20, 20% actives)
Abil T Quat 60 0 1 0 0 0
Quaternium-80, 0 0 1 0 0
Propylene Glycol
Quat-18, Water 0.5 0 0 0 0
Salcare SC 96 0 0 0 1 0
Merquat 2001 0 0 0 0 0.5
Dimethicone 0 0 1 0 1
DC-8500 0 0 1 0 1
D5, D6, 0 0 0 5 0
Dimethicone
Aminopropyl 0 0 0 0 0.5
Dimethicone
1)5, Dimethiconol 0 0 0 0 2
Cyclopentasiloxane, 5 0 0 0 0
Cyclohexasiloxane,
Dimethicone
Disodium EDTA 0.05 0.05 0.05 0.05 0.05
DMDM Hydantoin 0.2 0.2 0.2 0.2 0.2
Fragrance 0.6 0.6 0.6 0.6 0.6
Target Specifications 4A:
pH: 4.00-5.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C):
bulk: 5,000-9,000 cps
w/ shear (finished goods): 10,000-30,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
Target Specifications 4B:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C):
bulk: 7,000-15,000 cps
w/ shear (finished goods): 20,000-35,000 cps
Color: White (MS)
Odor: MS
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
63
Appearance: Viscous, opaque emulsion
Target Specifications 4C:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C):
bulk: 7,000-15,000 cps
w/ shear (finished goods): 20,000-35,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
Target Specifications 4D:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C):
bulk: 7,000-15,000 cps
w/ shear (finished goods): 20,000-35,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
Target Specifications 4E:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C):
bulk: 7,000-15,000 cps
w/ shear (finished goods): 20,000-35,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
EXAMPLE 5
[0227] This example demonstrates methods of making the compositions of
Example 4.
[0228] For Comparative Composition 4A, start heating container to 80-85 C
and add the
following: DI water, citric acid, and disodium EDTA. Check that that the
temperature is 80-
85 C and add the following: Quat-18/water, stearamidopropyl dimethylamine,
cetyl alcohol,
and stearyl alcohol. Vigorously mix for 30 minutes at 80-85 C. Cool the
mixture. At 57-60
C, slowly add the L-aspartic acid. At 45 C or below, add the following:
isostearamidopropyl ethyldimonium ethosulfate/PEG-9,
cyclopentasiloxane/cyclohexasiloxane/dimethicone, fragrance, and DMDM
hydantoin.
[0229] Compositions 4B, 4C, and 4E are prepared using two phases. For
Composition
4B, in the Main Phase, add 52.05 wt. % (of the final total wt. % of the
composition) of DI
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
64
water. Start heating to 80-85 C. Add the following one at a time and mix
until fully
dissolved and solution becomes clear: disodium EDTA and L-aspartic acid. Add
the
following one at a time at 80-85 C and mix until melted: stearamidopropyl
dimethylamine
(check to make sure solution has turned clear), eetyl alcohol, and glyceryl
stearate.
Vigorously mix for 30 minutes at 80-85 C. After 30 minutes, turn off heat,
slow the mixing
speed, and allow the composition to slowly cool. In the Side Phase, add 15.5
wt. % (of the
final total wt. % of the composition) of DI water and slowly add the
following, and mix until
hydrated: PVMMA Copolymer (Gantrez S-97 BF; ISP Corp., Wayne, NJ, USA) and
sodium hydroxide (20% active). The solution will slightly thicken. The in-
process pH
should be 6.90-7.00. Heat the Side Phase to 50-55 C. Slowly add the
Polyquaternium-28
(Conditioneze NT-20; ISP Corp.) under very vigorous mixing. The solution will
turn
opaque and become less viscous. Cool the Side Phase, and at < 45 C add 0.05
wt. % (of the
final total wt. % of the composition) of DMDM hydantoin. Slowly add the Side
Phase to the
Main Phase at < 45 C. Then add the following: Abil T Quat 60 (silicone
quaternium-22;
Evonik, Essen, Germany), propylene glycol, fragrance, and 0.15 wt. % (of the
final total wt.
% of the composition) of DMDM hydantoin.
10230] For Composition 4C, in the Main Phase, add 52.45 wt. A (of the
final total wt. %
of the composition) of DI water. Start heating to 80-85 C. Add the following
one at a time
and mix until fully dissolved and solution becomes clear: disodium EDTA and L-
aspartic
acid. Add the following one at a time at 80-85 C and mix until melted:
stearamidopropyl
dimethylamine (check to make sure solution has turned clear), cetyl alcohol,
and glyceryl
stearate. Vigorously mix for 30 minutes at 80-85 C. After 30 minutes, turn
off heat, slow
the mixing speed, and allow the composition to slowly cool. In the Side Phase,
add 15.5 wt.
% (of the final total wt. % of the composition) of DI water and slowly add the
following, and
mix until hydrated: PVMMA Copolymer (Gantrez S-97 BF; ISP Corp., Wayne, NJ,
USA)
and sodium hydroxide (20% active). The solution will slightly thicken. The in-
process pH
should be 6.90-7.00. Heat the Side Phase to 50-55 C. Slowly add the
Polyquaternium-28
(Conditioneze NT-20; ISP Corp.) under very vigorous mixing. The solution will
turn
opaque and become less viscous. Cool the Side Phase, and at < 45 C add 0.05
wt. % (of the
final total wt. % of the composition) of DMDM hydantoin. Slowly add the Side
Phase to the
Main Phase when at < 45 C. Pre-mix the quaternium-80/propylene glycol and
dimethicone
and then add to the combined Main and Side Phase. Then add the following: DC-
8500 (Bis
(C13-15 Alkoxy) PG Amodimethicone; Dow Corning, Midland, MI, USA), propylene
glycol,
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
fragrance, and 0.15 wt. % (of the final total wt. % of the composition) of
DMDM hydantoin.
102311 For Composition 4D, add 40 wt. % (of the final total wt. % of the
composition) of
DI water. Slowly add the following, and mix until hydrated: PVMMA Copolymer
(Gantrez
S-97 BF (ISP)) and sodium hydroxide (20% active). The solution will slightly
thicken. The
in-process pH should be 6.90-7.00. Heat to 50-55 C, and slowly add the
Polyquatemium-28
(Conditioneze NT-20 (ISP)) under very vigorous mixing. The solution will turn
opaque and
become less viscous. Start heating to 80-85 C, and add the following one at a
time, mixing
until fully dissolved: disodium EDTA, L-aspartic acid, and 22.95 wt. % (of the
final total wt.
% of the composition) of DI water. Add the following one at a time at 80-85
C, and mix
until melted: stearamidopropyl dimethylamine, cetyl alcohol, stearyl alcohol,
glyceryl
stearate, Crodamol STS (PPG-3 Benzyl Ether Myristate; Croda Inc., Edison, NJ,
USA),
Salcare SC 96 (65% polyquatemium-37, 25% propylene glycol
dicaprylate/dicaprate, 10%
PPG-1 trideceth-6; Ciba /BASF, Basel, Switzerland). Mix vigorously for 30
minutes at 80-
85 C. Reduce the mixing speed and allow the composition to cool. When the
temperature is
<45 C, add the following: D5/D6/Dimethicone, propylene glycol, fragrance, and
DMDM
hydantoin.
[0232] For Composition 4E, in the Main Phase, add 50.47 wt. % (of the final
total wt. %
of the composition) of DI water. Start heating to 80-85 C. Add the following
one at a time
and mix until fully dissolved and solution becomes clear: disodium EDTA and L-
aspartic
acid. Add the following one at a time at 80-85 C and mix until melted:
stearamidopropyl
dimethylamine (check to make sure solution has turned clear), cetyl alcohol,
glyceryl
stearate, Montanov 202 (arachidyl alcohol and behenyl alcohol and arachidyl
glucoside;
SEPPIC, Paris, France), and aminopropyl dimethicone. Vigorously mix for 30
minutes at 80-
85 C. After 30 minutes, turn off heat, slow the mixing speed, and allow the
composition to
slowly cool. In the Side Phase, add 15.5 wt. % (of the final total wt. % of
the composition) of
DI water and slowly add the following, and mix until hydrated: PVMMA Copolymer
(Gantrez S-97 BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20%
active). The
solution will slightly thicken. The in-process pH should be 6.90-7.00. Heat
the Side Phase to
50-55 C. Slowly add the Polyquaternium-28 (Conditioneze NT-20; ISP Corp.)
under very
vigorous mixing. The solution will turn opaque and become less viscous. Cool
the Side
Phase, and at < 45 C add 0.05 wt. % (of the final total wt. % of the
composition) of DMDM
hydantoin. Slowly add the Side Phase to the Main Phase when at < 45 C. At 45
C or
below, add the Merquat 2001 (polyquatemium-47; Nalco, Naperville, IL, USA).
Pre-mix
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
66
the D5/dimethiconol and dimethicone and then add to the combined Main and Side
Phase.
Then add the following: DC-8500 (Bis (C13-15 Alkoxy) PG Amodimethicone; Dow
Corning, Midland, MI, USA), propylene glycol, fragrance, and 0.15 wt. % (of
the final total
wt. % of the composition) of DMDM hydantoin.
EXAMPLE 6
[0233] This example demonstrates the mending of split-ends of hair
fibers using a test
method of the present invention.
[0234] Below compares the compositions used in this study that are
presented in
Figure 1. The sodium hydroxide/aspartic acid are adjusted to achieve the
proper pH, if
necessary.
[0235] Compositions 6A-6D
Ingredients Composition Composition Composition
Composition
6A 6B 6C 6D
(wt. %) (wt. %) (wt. %) (wt. %)
DI Water 69.95 67.95 62.95 65.97
L-Aspartic Acid 0.75 0.75 0.75 0.75
Stearamidopropyl 2 2 2 2
Dimethylamine
Cetyl Alcohol 5 5 4 4
Stearyl Alcohol 0 0 1 0
Glyceryl Stearate 1 1 1 0.8
Crodamol STS 0 0 2 0
Montanov 202 0 0 0 1.18
Propylene Glycol 10 10 10 10
PVMMA (Gantrez 0.2 0.2 0.2 0.2
S-97 BF)
NaOH (20% active) 0.25 0.25 0.25 0.25
Polyquaternium-28 9 9 9 9
(Conditioneze NT-
20)
Abir T Quat 60 1 0 0 0
Quatemium-80, 0 1 0 0
Propylene Glycol
Salcare SC 96 0 0 1 0
Merquat 2001 0 0 0 0.5
Dimethicone 0 1 0 1
DC-8500 0 1 0 1
D5, D6, 0 0 5 0
Dimethicone
Aminopropyl 0 0 0 0.5
Dimethicone
D5, Dimethiconol 0 0 0 2
Disodium EDTA 0.05 0.05 0.05 0.05
DMDM Hydantoin 0.2 0.2 0.2 0.2
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
67
Fragrance 0.6 0.6 0.6 0.6
102361 Below compares compositions used in this study as presented in
Figure 2. The
sodium hydroxide/citric acid/aspartic acid are adjusted to achieve the proper
pH, if necessary.
102371 Compositions 6E to 6J
Ingredients Compo- Compo- Compo- Compo- Compo- Compo-
sition 6E sition 6F sition 6G sition 6H sition 61
sition 6J
(wt. %) (wt. %) (wt. %) (wt. %) (wt. %)
(wt. %
finished
product)
DI Water 79.6 76.35 68.3 60.82 80.54 75.0752
L-Aspartic Acid 0 0.75 0.75 0.75 0 0
Citric Acid 0 0 0 0 0 0.0184
Stearamidopropyl 0 2 2 2 0 0
Dimethylamine
Cocamidopropyl 0 0 0 0 0 0.368
betaine, water,
sodium chloride
Cetyl Alcohol 0 1 1 4 0 0
Stearyl Alcohol 0 0 0 0 0 0
Glyceryl Stearate 0 0.2 0.2 0.8 0 0
Crodamol STS 0 0 0 2 0 0
Aminomethyl 0 0 0 0 0.46 0
Propanol (AMP-95)
PEG-40 0 0 0 0 0.6 0
hydrogenated castor
oil
Montanov 202 0 0 0 1.18 0 0
Glycerin 1 1 0 0 0 0
Sorbitol (70%) 0 0 0 0 0.5 0
Propylene Glycol 0.5 0.5 10 10 1 2.07
(USP)
Polysorbate 20, 0 0 0 0 0 0.644
water
PVMMA (Gantrez 0.2 0.2 0.2 0.2 0.2 0.2
S-97 BF)
NaOH (20% active) 0.25 0.25 0.25 0.25 0.25 0.25
Polyquaternium-28 9 9 9 9 9 9
(Conditioneze NT-
20, 20% active)
Salcarc SC 96 3 3 3 1 0 0
Polyquaternium-4 0 0 0 0 0.5 0
(Celquat H-100)
Polyquaternium-4 0 0 0 0 0 0.46
(Celquat L-200)
PVP K-90 (20%) 0 0 0 0 1 0
Luviset Clear 0 0 0 0 3.5 0
Polyquaternium-39 0 0 0 0 0.5 0
UltrathixTM P-100 0 0 0 0 1 0
Advantage S 0 0 0 0 0 0.23
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
68
---- ¨
Polyquaternium-11, 0 0 0 0 0 1.4444
water
Polyquaternium-7 0 0 0 0 0 0.92
Dimethicone 3 2 1 1.5 0 0
(DC-200, (60,000
20 cst) cst)
Cyclopentasiloxane, 1 0 0 0 0 0
dimethiconol
DC 2-8566 0 0 0 2 0 0
(Amodimethicone)
DC-8500 0 0 1 0 0 0
DC-190 0 0 0 0 0.1 0
Aminopropyl 0 0 0.5 0.75 0 0
Dimethicone
Phenyl trimethicone 2 2 0 0 0 0
(DC-556)
D5, Dimethiconol 0 1 2 3 0 0
(DC-1501)
DC 5-7113 silicone 0 0 0 0 0 0.92
quat microemulsion
Disodium EDTA 0.05 0.05 0.05 0.05 0.05 0
DMDM Hydantoin 0.2 0.2 0.25 0.2 0.2 0
Fragrance 0.2 0.5 0.5 0.5 0.6 0.4
Isobutene and 0 0 0 0 0 8
propane and 152A
[0238] Figure 1
shows the results of mending for conditioners when using twice-bleached
European hair with split-ends produced mechanically. The results show about
80% mending
with the rinse-off conditioners in three cycles.
[0239] Figure 2 shows the results of various compositions when using twice-
bleached
European hair with split-ends produced mechanically. The results are based on
the
assumption that all formulas are left in, including Night Repair. The results
show greater
than 80% for all leave-in compositions in one treatment.
EXAMPLE 7
[0240] This example demonstrates the mending of split-ends of hair fibers
using a test
method of the present invention.
[0241] Below compares compositions uscd in this study. The sodium
hydroxide/aspartie
acid are adjusted to achieve the proper pH, if necessary.
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
69
[0242] Compositions 7A-7D
Ingredients Composition Composition Composition
Composition
7A 7B 7C 7D
(wt. %) (wt. %) (wt. %) (wt. %)
DI Water 76.3497 41.2837 62.9497
68.3497
Disodium EDTA 0.05 0.1 0.05 0.05
L-Aspartic Acid 0.75 0 0.75 0.75
Stearamidopropyl 2 0 2 2
Dimethylamine
Cetyl Alcohol 1 0 4 1
Stearyl Alcohol 0 0 1 0
Glyceryl Stearate 0.2 0 1 0.2
Crodamol STS 0 0 2 0
Cocamidopropyl 0 8.2 0 0
betaine, water, sodium
chloride
PVM/MA Copolymer 0.2 0.001 0.2 0.2
(Gantrez S-97 BF
(ISP))
Sodium Hydroxide 0.25 0.15 0.25 0.25
(20% active)
Polyquatcrnium-28 9 0.045 9 9
(Conditioneze NT-20
(ISP), 20% active)
Dimethicone (60,000 2 0 0 1
est)
Phenyl Trimethicone 2 0 0 0
(DC-556)
D5, Dimethiconol 1 0 0 0
(DC-1501)
Fluid Blend 0 0 5 0
DC-8500 0 0 0 1
Aminopropyl 0 0 0 0.5
dimethicone
Abil OSW 5 0 0 0 2
Glycerin 1 0 0 0
Propylene Glycol 0.5 0 10 10
Fragrance 0.5 0.7 0.6 0.5
DMDM Hydantoin 0.2 0 0.2 0.2
Cocos Nucifera 0.0001 0.0001 0.0001 0.0001
(Coconut) Oil
Keratin Amino Acids 0.0001 0.0001 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001 0.0001
Salcare SC-96 3 0 1 3
Polyquaternium-10 0 0.8 0 0
Sodium laureth 0 32 0 0
sulfate-1 mole (25%)
Disodium laureth 0 12.8 0 0
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
sulfosuccinate (about
34% active)
Styrene/VP 0 0.75 0 0
copolymer (40%),
water
PEG-6 caprylic/capric 0 0.6 0 0
triglyceride
Kathon CG 0 0.07 0 0
Sodium chloride 0 2.5 0 0
Target Specifications 7A:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 5,000-15,000 cps
Color: White (MS)
Odor: MS
Appearance: Opaque emulsion
Target Specifications 7B:
pH: 5.5-6.5
Viscosity (LVT/spindle 4/30 rpm/ 1 min, 25C): 15,000-20,000 cps
Color: White/Off white (MS)
Odor: MS
Appearance: Viscous, opaque liquid
Target Specifications 7C:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 15,000-25,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
Target Specifications 7D:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 mm, 25C): 10,000-20,000 cps
Color: White (MS)
Odor: MS
Appearance: Opaque emulsion
[0243] Fifty hair fibers containing split-ends were removed from hair
tresses. The hair
fiber samples were placed on glass slides aligned along a strip of double
stick tape for optical
imaging. Each fiber selected with a split-end was individually photographed
and the image
was stored before product application, using a WILD stereomicroscope at a
magnification of
about 25X with transmitted light emanating. The fibers were also rotated prior
to image
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
71
capture to make sure that the split-ends were in view.
[0244] The product application protocol listed below was followed. In each
case, the 50
selected fibers with split-ends were placed respectively in five different
tresses and then the
product applied. Optical images of tip ends of the respective selected fibers
were obtained
again to examine and assess extent of split-end mending. The results appear in
Table 12.
[0245] Table 12 shows a summary of the split-end data study comparing the
total number
of split-ends before treatment (50) to the number of split-ends repaired after
treatment. (The
split-ends for the repeat study, category 6, were prepared by a separate
method).
[0246] Table 12
Initial Mended
Number Number
Cate-Number Number Number
(Mended
Composition Partially Not
gory Of Split- Mended Broke
Mended Mended
Ends
Partially
Mended)
Leave in Treatment
1 50 32 13 3 2 94
(Composition 7A)
Shampoo
(Composition
7B)+Conditioner
2 (Composition 50 33 13 4 0 92
7C)+Leave in
Treatment
(Composition 7A)
Overnight
3 Treatment 50 30 16 3 1 94
(Composition 7D)
Conditioner
4 49 39 3 7 0 86
(Composition 7C)
Shampoo
(Composition
50 29 4 14 3 70
7B)+Conditioner
(Composition 7C)
Shampoo
(Composition
6 7B)+Conditioner 50 30 8 12 0 76
(Composition 7C)
(Repeat) new stock
[0247] All categories show ability to mend split-ends in hair fibers, three
of them
showing improvements of 90% or more.
[0248] Product Application Protocol
[0249] Protocols are listed in the order presented in Table 12. To achieve
80% dry
tresses for some compositions (as noted below), blow drying time was changed
from 5
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
72
minutes to 20 minutes because of the nature of the blow dryer (mild air flow).
[0250] A. Pre-cleansing the Hair
1. Clean the wax-strip bound Platinum (2x) bleached hair by soaking in a 5%
w/w solution of Sodium Lauryl Ether Sulfate (1M) solution. The solution to
hair ratio is
40:1. Soak for 30 minutes at room temperature, and then massage the hair by
hand for 3
minutes before rinsing under 40 C tap water until all the bubbles are rinsed
out.
2. Blot the hair dry with tissue paper or a towel, comb straight, and leave
the hair
to dry at ambient room temperature overnight.
[0251] B. Causing Split-Ends ¨ Mechanically
1. The tresses are swatched by International Hair Importers in a way that
the
density of the hair is linear. Prepare 5 tresses that are 1.5" wide, cut and
tape so that there is
6g of hair in each tress.
2. Attach each tress to the repeated combing machine and comb the tress
1500
times per side for a total of 3000 combings per tress.
3. During the combing, the blow dryer is positioned 8 inches from the tress
and
turned on high heat setting. The air flow is directed towards the bottom of
the hair tress so
that the hair is pushed towards the comb during repeated combing.
[0252] C. Selecting the Split-Ends from the Tress and Taking Initial
Pictures
1. Using a magnifying glass, examine the tip of the tresses to find hair
fibers with
split-ends. Select and remove 50 fibers with split-ends from the tress by the
root. Select 10
split-end fibers out of each tress so that 50 fibers can be pulled from the
five tresses.
2. Crimp the fibers at the root end using metal crimps, and then line up
the
crimps to be placed on tape so that there are 10 fibers on each tape strip.
Cover up the crimps
using another tape so that they can be easily picked up together.
3. Number all 50 fibers and take optical images of 10 out of the 50 hair
fibers for
before and after pictures.
4. Using a red pernianent marker, mark each of the selected 50 fibers up to
the
beginning of the split.
5. Take optical images of 10 split-ends by mounting the split-ends on glass
slides. A stereomicroseope at a magnification of 50X with transmitted light
emanating from
under the stage of the microscope is used to take the pictures.
6. Examine the other 40 fibers with split-ends using the stereomicroscope,
but
they do not need to be photographed.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
73
7. The strip of tape that contains split-ends is placed back in the middle
1.5"
tress.
8. Clamp the tress with the split-end fibers using a large clip such as a
binder
clip.
[0253] D. Composition Application - Category 1
1. Wet the hair tress for 30 seconds under 35-40 C water at 1 GPM.
2. Apply 1.5 ml of a non-conditioning shampoo to the 1.5 inch tress and
massage
for 1 minute.
3. Rinse the tress for 30 seconds under 35-40 'V water at 1 GPM.
4. Wring out the excess water by sliding the tress between fingers.
5. Mount the top of the tress to a stand for blow drying.
6. Clip the tress at 1/4 of its length with a hair clip to avoid flyway
hair.
7. Blow dry the tress at medium heat with the dryer being 2 ft away from
the
tress for about 3 minutes.
8. Apply 1.5 ml of Composition 7A, leave in treatment, to the 1.5 inch damp
tress evenly on both sides. Massage for 1 minute focusing to the ends and
split-end prone
areas.
9. Comb once on each side of the tress.
10. Mount the top of the tress to a stand for blow drying.
11. Clip the tress at 3/4 of its length with a hair clip to avoid flyway
hair.
12. Blow dry the tress at medium heat (mild air flow) with the dryer being
2 ft
away from the tress until it is 80% dry for about 20 minutes.
13. After blow drying, comb the tress once on each side.
[0254] D. Composition Application - Category 2
1. Wet the hair tress for 30 seconds under 35-40 C water at 1 GPM.
2. Apply 1.5 ml of Composition 7B (shampoo) to the 1.5 inch tress and
massage
for 1 minute.
3. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM.
4. Wring out the excess water by sliding the tress between fingers.
5. Apply 1.5 ml of Composition 7C (conditioner) to the 1.5 inch tress and
stroke
the tress 9 times from top to bottom and let it stand for 1 minute.
6. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM.
7. Blot dry the tress gently using Kim Wipes.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
74
8. Mount the top of the tress to a stand for blow drying.
9. Clip the tress at 1/4 of its length with a hair clip to avoid flyway
hair.
10. Blow dry the tress at medium heat with the dryer being 2 ft away from
the
tress for 3 minutes.
11. Apply 1.5 ml of Composition 7A, leave in treatment, to the 1.5 inch
damp
tress. Massage for 1 minute focusing on the ends and split-end prone areas.
12. Comb the tress once on each side.
13. Mount the top of the tress to a stand for blow drying.
14. Clip the tress at 3/4 of its length with a hair clip to avoid flyway
hair.
15. Blow dry the tress at medium heat (mild air flow) with the dryer being
2 ft
away from the tress until it is 80% dry for about 20 minutes.
16. After blow drying, comb through the tress twice on each side.
[0255] D. Composition Application ¨ Category 3
1. Wet the hair tress for 30 seconds under 35-40 C water at 1 GPM.
2. Apply 1.5 ml of a non-conditioning shampoo to the 1.5 inch tress and
massage
for 1 minute.
3. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM.
4. Wring out the excess water by sliding the tress between fingers.
5. Mount the top of the tress to a stand for blow drying.
6. Clip the tress at 3/4 of its length with a hair clip to avoid flyway
hair.
7. Blow dry the tress at medium heat with the dryer being 2 ft away from
the
tress for about 3 minutes.
8. Apply 1.5 ml of Composition 7D, overnight treatment, to the damp 1.5
inch
tress to both sides of the tress. Massage for 1 minute focusing on the ends
and split-end prone
areas.
9. Comb the tress once on each side.
10. Let the composition stand on the hair for 8 hours since this is an
overnight
treatment.
11. Clip the tress at 3/4 of its length with a hair clip to avoid flyway
hair.
[0256] D. Composition Application ¨ Category 4
1. Wet the hair tress for 30 seconds under 35-40 C water at 1 GPM.
2. Apply 1.5 ml of a non-conditioning shampoo to the 1.5 inch tress and
massage
for 1 minute.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
3. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM,
4. Wring out the excess water by sliding the tress between fingers.
5. Apply 1.5 ml of Composition 7C to the 1.5 inch tress and stroke the
tress 9
times from top to bottom and let it stand for 1 minute.
6. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM.
7. Blot dry the tress gently using Kim Wipes.
8. Mount the top of the tress to a stand for blow drying.
9. Clip the tress at 3/4 of its length with a hair clip to avoid flyway
hair.
10. Blow dry the tress at medium heat with the dryer being 2 ft away from
the
tress until it is 80% dry for about 5 minutes.
11. Comb through the tress twice on each side.
12. Reapply the red markings on the fiber after blow drying
13. Repeat steps 1 to 12 for an additional 2 more cycles, so there is total
of three
treatments.
[0257] D. Composition Application ¨ Category 5
1. Wet the hair tress for 30 seconds under 35-40 C water at 1 GPM.
2. Apply 1.5 ml of Composition 7B (shampoo) to the 1.5 inch tress and
massage
for 1 minute.
3. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM.
4. Wring out the excess water by sliding the tress between fingers.
5. Apply 1.5 ml of Composition 7C (conditioner) to the 1.5 inch tress and
stroke
the tress 9 times from top to bottom and let it stand for 1 minute.
6. Rinse the tress for 30 seconds under 35-40 C water at 1 GPM.
7. Blot dry the tress gently using Kim Wipes.
8. Comb through the tress once on each side.
9. Mount the top of the tress to a stand for blow drying.
10. Clip the tress at 1/4 of its length with a hair clip to avoid flyway
hair.
11. Blow dry the tress at medium heat (mild air flow) with the dryer being
2 ft
away from the tress until it is 80% dry for about 20 minutes.
12. Comb through twice on each side.
13. Repeat steps 1 to 12 for an additional 2 more cycles, so there is a
total of three
treatments.
[0258] E. Selecting the Split-ends from the Tress and Taking Final Pictures
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
76
1. Remove the strip of tape that contains split-ends from the middle of the
1.5"
tress.
2. Using the stereomicroseope, take the after treatment optical images of
the 10
hair fibers with split-ends by mounting the split-ends on glass slides.
3. Examine the other 40 fibers with split-ends using the stereomicroscope.
4. Count the number of fibers that have been mended to determine % mending.
EXAMPLE 8
[0259] This example demonstrates methods of communicating split-end mending
to
consumers.
[0260] Figure 3 is a schematic showing the mending of a split-end using
polyelectrolyte
complexes (PECs). The PECs are shown here in a possible mechanism of action
where they
attach to the site of the split-end, form a network with themselves and the
fiber assembly, and
shrink as they dry binding the split end from within.
[0261] Figures 4A-4D show still photography of the mending of a variety of
split-end
types using methods as described herein with compositions as described herein.
[0262] Figure 5 shows still frames from a video of the mending of split-
ends through the
process of mending method as described herein.
EXAMPLE 9
[0263] This example demonstrates additional compositions of the present
invention.
[0264] Composition 9A
Main Phase wt%
DI Water 45.0397
Aminomethyl Propanol (AMP-95) 0.02
Add the following under very vigorous mixing for 30 mins.
"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1
Add the following and mix until uniform
Aminomethyl Propanol (AMP-95) 0.44
Side Phase 1
DI Water 20
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5
Disodium EDTA 0.05
Liquid Additions:
PVP K-90 (20% active) 1
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
77
VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset
Clear" (BASF)) - 20% active 3.5
Polyquaternium-39 (8.5% active) 0.5
Propylene Glycol 1
Sorbitol (70%) 0.5
Add Side Phase 1 to main tank and mix until uniform
Side Phase 2
DI Water 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2
Sodium Hydroxide (20% active) 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 9
(solution will turn opaque and become less viscous)
DMDM Hydantoin 0.05
Slowly add Side Phase 2 to main tank and mix until uniform
<45C
Pre-mix next two and fragrance
PEG-40 Hydrogenated Castor Oil 0.6
PEG/PPG-18/18 Dimethicone (DC-190) 0.1
Fragrance 0.6
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
DMDM Hydantoin 0.15
Target Specifications 9A:
pH: 6.0-7.0
Viscosity (RV T-C, 5 rpm, 1
min, 25C): 40,000-80,000
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque (hazy)
gel
[0265] Compositions 9B-1 and 9B-2
9B-1 9B-2
Main Phase wt% wt%
DI Water 64.755325 59.5249
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
78
Add the following under vigorous mixing, mix until hydrated
(clear)
Polyquaternium-4 (Celquat L-200) 0.5 0.46
Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate
Copolymer ("Advantage S" (ISP)) 0.25 0.23
Citric Acid 0.02 0.0184
Liquid Additions:
POLYQUATERNIUM-11, WATER (21.5% active) 1.57 1.4444
POLYQUATERNIUM-7 (8.5% active) 1 0.92
DC 5-7113 Silicone Quat Microemulsion - Dow Corning (66%
Water, 25% Silicone Quaternium-16, 7.4% Undeceth-11, 4.5%
Butyloctanol, 3.5% Undeceth-5)
1 0.92
PROPYLENE GLYCOL, USP 2.25 2.07
COCAMIDOPROPYL BETATNE (-30% active), WATER,
SODIUM CHLORIDE 0.4 0.368
Side Phase
DI Water 16.847826 15.55
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.217391 0.2
Sodium Hydroxide (20% active) 0.271739 0.25
(solution will slightly thicken)
1n-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 9.782609 9
(solution will turn opaque and become less viscous)
Slowly add side phase to main phase
Pre-Mix polysorbate 20 and Fragrance
POLYSORBATE 20 0.7 0.644
Fragrance 0.434783 0.4
Cocos Nucifera (Coconut) Oil 0.000109 0.0001
Keratin Amino Acids 0.000109 0.0001
Flower/Leaf Extract 0.000109 0.0001
Propellant Charge
Isobutane and Propane and 152A (78.5% A46; 28.5% HFC
152A) 0 8
Target Specifications 9B:
(Bulk) (Finished Goods)
pH: 5.0-6.5 5.0-6.5
Color: off white (MS) white (ms)
Odor: MS MS
Appearance: hazy liquid dense foam, non-watery, non-runny
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
79
Non-Volatiles:
Foam Stability: 200 seconds min.
Vacuum: 16-18 in.
Vapor Pressure at 70F: 69-74 psig
Vapor Pressure at 130F: 140-145 psig
Spray Pattern/Diameter: Foam
[0266] Composition 9C-1
Item wt%
Main Phase
DI Water 93.33163
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.001
NaOH, 20% 0.00125
Add the following and mix vigorously
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20%
active) 0.045
Disodium EDTA 0.02
PVP 0.45
Stearalkonium Chloride 1 _
Heat to 170-175F and mix for 30 min
Cool the batch down to 90-95F
Glycerin 1
[DC-949]
60% Amodimethicone, 5% Trideceth-12, 5% Cetrimonium
Chloride, 30% Water 2
PEG-12 Dimethicone 0.5
Propylene Glycol 0.5
Triethanolamine 0.00001
Citric Acid 0.00001
DMDM Hydantoin 0.3
Hydrolyzed Silk 0.05
Water, Polysorbate20, Ascorbic Acid, Panthenol,
Tocopherol Acetate, Biotin, Niacinamide 0.001
Water, Polyglyceiy1-3 Distearate, Polysorbate 60, Myristic
Acid, Palmitic Acid, Stearic Acid, Guar
Hydroxypropyltrimonium Chloride, Triticum Vulgare
(Wheat) Flour Lipids, Ceramide 3, Persea Gratissima
(Avocado) Oil, Tetrahexyldecyl Ascorbate, Glycine Soja
(Soybean) Sterols, Alpha-Glucan Oligosaccharide,
Ethylhexyl Methoxycinnamate, Butyl
Methoxydibenzoylmethane, Tocopheryl Acetate 0.0001
Premix the following and add to the batch
Polysorbate20 0.4
Fragrance 0.4
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
Target Specification 9C-1:
pH: 4.0-5.0
Color: Cloudy/Pale white
Odor: To match reference
Appearance: Milky liquid
[0267] Composition 9C-2
Item wt%
Side Phase
DI Water 7.75
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
After material has hydrated, adjust pH to 6.9-7 using the
following
Na0H(20%) 0.125
Heat to 50-55C. Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20) 4.5
Main Phase
= DI Water 79.7247_
Heat to 80-85C then added the following
Panthenol 1
Glycerin 3
Cctyl Alcohol 1
Stearyl Alcohol 0.25
Steareth-21 0.15
Polyquatemium-37, Propylene Glycol
Dicaprylate/Dicaprate, PPG-1 Trideceth-6 (Saleare SC-
96) 0.5
Mix for 30 min at 80-85C
Cool batch to below 45C
DMDM Hydantoin 0.2
Fragrance 0.2
Premix the following and add to the batch
Phenyl Trimethicone 0 .5
Cyclopentasiloxane, Dimethiconol, Dimethicone 1
Amodimethiconc (DC 2-8566 Amino Fluid) 0.0001
Target Specification 9C:
pH: 4.5-6
Color: White
Odor: To match reference
Appearance: Milky liquid
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
81
[02681 Compositions 9D-1 and 9D-2
9D-1 9D-2
Main Phase wt% wt%
DI Water 78.287935 72.0249
Add the following under vigorous mixing, mix until hydrated
(clear)
Polyquaternium-4 (Celquat H-100) 0.5 0.46
Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate
Copolymer ("Advantage S" (ISP)) 0.25 0.23
Citric Acid 0.02 0.0184
Liquid Additions:
POLYQUATERNIUM-11, WATER (21.5% active) 1.57 1.4444
POLYQUATERNIUM-7 (8.5% active) 1 0.92
DC 5-7113 Silicone Quat Microemulsion - Dow Corning (66%
Water, 25% Silicone Quaternium-16, 7.4% Undeceth-11, 4.5%
Butyloctanol, 3.5% Undeceth-5) 1 0.92
PROPYLENE GLYCOL, USP 2.25 2.07
COCAMIDOPROPYL BETAINE (-30% active), WATER,
SODIUM CHLORIDE 0.4 0.368
Side Phase
DI Water 8.423913 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.108696 0.1
Sodium Hydroxide (20% active) 0.13587 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.891304 4.5
(solution will turn opaque and become less viscous)
Add the following at < 45C
DMDM Hydantoin 0.027174 0.025
Slowly add side phase to main phase
Pre-Mix polysorbate 20 and Fragrance
POLYSORBATE 20 0.7 0.644
Fragrance 0.434783 0.4
Cocos Nucifera (Coconut) Oil 0.000109 0.0001
Keratin Amino Acids 0.000109 0.0001
Flower/Leaf Extract 0.000109 0.0001
Propellant Charge
Isobutane and Propane and 152A (78.5% A46; 28.5% HFC
152A) 0 8
Target Specifications 9D:
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
82
Bulk
Color: off white (MS)
Odor: MS
Appearance: hazy liquid
pH: 5.0-6.5
Specific
Gravity:* 0.986
Non-Volatiles: 4.4-4.9%
(T=4.66)
Finished Product
Color: white (MS)
Odor: MS
Appearance: dense foam, non-
watery, non-
runny
pH: 5.0-6.5
Foam Stability: 200 seconds min
Foam Density:* 0.039 g/ml,
Specific
Gravity:* 0.941
4.3-4.8%
Non-Volatiles: (T=4.58)
* for reference
[0269] Composition 9E
Main Phase wt%
DI Water 57.5647
Aminomethyl Propanol (AMP-95) 0.02
Add the following under very vigorous mixing for 30 mills.
"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1
Add the following and mix until uniform
Aminomethyl Propanol (AMP-95) 0.44
Side Phase 1
DI Water 20
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5
Liquid Additions:
PVP K-90 (20% active) 1
VP/MethaerylamideNinyl Imidazole Copolymer ("Luviset
Clear" (BASF)) - 20% active 3.5
Polyquaternium-39 (8.5% active) 0.5
Propylene Glycol 1
Sorbitol (70%) 0.5
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
83
Add Side Phase 1 to main tank and mix until uniform
Side Phase 2
DI Water 7.75 _
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5
(solution will turn opaque and become less viscous)
Add the following at < 45C
DMDM Hydantoin 0.025
Slowly add Side Phase 2 to main tank and mix until uniform
<45C
Pre-mix next two and fragrance
PEG-40 Hydrogenated Castor Oil 0.6
PEG/PPG-18/18 Dimethicone (DC-190) 0.1
Fragrance 0.6
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
DMDM Hydantoin 0.175
Target Specifications 9E:
pH: 6.0-7.0
Viscosity (RV T-C, 5 rpm, 1 min, 25C): 40,000-80,000
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque (hazy)
gel
102701 Compositions 9F-1 through 9F-4
9F-1 9F-2 9F-3 9F-4
Item wt% wt% wt% wt%
Main Phase
DI Water 74.2247 73.2247 71.2247
69.2247
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5 0.5 0.5 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl
Methacrylate Copolymer ("Advantage S" (ISP)) 0.5 0.25 1 0.5
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
84
Liquid Additions
POLYQUATERN1UM-11, WATER (20% active) 2.5 2.5 2.5 5
VP/Methacrylamide/Vinyl Imidazole Copolymer
("Luviset Clear'' (BASF)) - 20% active 2.5 3.75 5 5
Polyquaternium-39 (8.5% active) 0.5 0.5 0.5 0.5
Propylene Glycol 1 1 1 1
Sorbitol (70%) 0.5 0.5 0.5 0.5
Side Phase
DI Water 7.75 7.75 7.75 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.10 0.1
Sodium Hydroxide (20% active) 0.125 0.125 0.125 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous
mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP),
20% active) 4.5 4.5 4.5 4.5
(solution will turn opaque and become less
viscous)
(mix for'-10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025 0.025 0.025 0.025
Slowly add side phase to main phase at < 45C
<45C
Pre-mix next two and fragrance
PEG-40 Hydrogenated Castor Oil 0.5 0.5 0.5 0.5
PEG/PPG-18/18 Dimethicone (DC-190) 0.1 0.1 0.1 0.1
Fragrance 0.5 0.5 0.5 0.5
DMDM Hydantoin 0.175 0.175 0.175 0.175
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
Add the following and mix until uniform
"Sepigel 305" 4 4 4 4
Mix until uniform
Target Specifications 9F:
pH: 7.00-7.50
Viscosity (RV T-C, 5 rpm, 1 min, 25C): 50,000-100,000 cps
Color: clear-semi white
Odor: MS
Appearance: thick gel
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
[0271] Compositions 9G-1 through 9G-4
9G-1 9G-2 9G-3 9G-4
Item wt% wt% wt% wt%
Main Phase
DI Water 71.325 _____________________________________ 70.325 68.325
66.325
__ Sprinkle in the following and mix until clear
Polyquatemium-4 (Celquat H-100) 0.5 0.5 0.5 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl
Methacrylate Copolymer ("Advantage S" (ISP)) 0.5 0.25 1 0.5
Liquid Additions:
POLYQUATERNIUM-11, WATER (20% active) 2.5 2.5 2.5 5
VP/MethacrylamideNinyl Imidazole Copolymer
("Luviset Clear" (BASF)) - 20% active 2.5 3.75 5 5
Side Phase
DI Water 7.75 7.75 7.75 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125 0.125
0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP)) 4.5 4.5 4.5 4.5
(solution will turn opaque and become less viscous)
DMDM Hydantoin 0.025 0.025 0.025
0.025
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1 Trideceth-6) 3 3 3 3
Mix until uniform
<45C
Silicone Premix
Dimethicone (60,000 cst) 2 2 2 2
Phenyl Trimethicone (DC-556) 2 2 2 2
Cyclopentasiloxane, Dimethiccmol 1 1 1 1
Glycerin 1 1 1 1
Propylene Glycol 0.5 0.5 0.5 0.5
Fragrance 0.5 0.5 0.5 0.5
DMDM Hydantoin 0.175 0.175 0.175
0.175
Target Specifications 9G:
pH: 5.00-6.50
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
86
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 20,000-40,000 cps
Color: Semi-Translucent - white (MS)
Odor: MS
Appearance: Viscous, opaque gel
102721 Compositions 9H-1 and 9H-2
9H-1 9H-2
Item wt% wt%
Main Phase
DI Water 75.625 74.125
Sprinlde in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate
Copolymer ("Advantage S" (ISP)) 0 0.25
POLYQUATERNIUM-11, WATER (20% active) 2.5 1.25
VP/Methaerylamide/Vinyl Imidazole Copolymer
(''Luviset Clear" (BASF)) - 20% active 0 2.5
PEC Pre-mix
DI Water 7.75 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125
(solution will slightly thicken)
___________ In-process pH specification: 6.90-7.00
Heat to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP)) 4.5 4.5
(solution will turn opaque and become less viscous)
mix for 10 minutes
Add the following at < 45C
DMDM Hydantoin 0.025 0.025
Slowly add side phase to main phase at < 45C
<45C
Silicone Premix
Dimethiconc (60,000 cst) 2 2
Phenyl Trimethicone (DC-556) 2 2
Cyclopentasiloxane, Dimethiconol 1 1
Glycerin 1 1
Propylene Glycol 0.5 0.5
Fragrance 0.2 0.2
DMDM Hydantoin 0.175 0.175
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
87
"Salcare SC-96" - Ciba/BASF (65% Polyquaternium-37,
25% Propylene Glycol Dicaprylate Dicapratc, 10% PPG-1
Trideceth-6) 2 2
Mix until uniform
Target Specifications 9H:
pH: 5.00-6.50
Viscosity (RV T-B, 10 rpm, 1 mm, 25C): 5,000-15,000 cps
Color: Semi-Translucent white (MS)
Odor: MS
Appearance: Viscous, milky liquid
[0273] Compositions 91-1 through 91-3
91-1 91-2 91-3
Item wt% wt% wt%
Main Phase
DI Water 51.3247 62.3247 68.3247
Sprinkle in the following and mix until clear
Polyquatemium-4 (Celquat H-100) 0.5 0.5 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate
Copolymer ("Advantage S" (ISP)) 0.25 0.25 0.25
Disodium EDTA 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75
Add the following one at a time at 80-85C and mix until
melted/homogeneous
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 1 1 1
Glyccryl Stcaratc 0.2 0.2 0.2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed; allow to cool and foam to reduce
Liquid Additions:
POLYQUATERNIUM-11, WATER (20% active) 1.25 1.25 1.25
VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset Clear''
(BASF)) - 20% active 2.5 2.5 2.5
Side Phase
DI Water 7.75 7.75 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (1SP)) 0.1 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125 0.125
(solution will slightly thicken)
In-process pH seecification: 6.90-7.00
Heat Side Phase to 50-55C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
88
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 4.50 4.5 4.5
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025 0.025 0.025
Slowly add side phase to main phase at 45C
<45C
'Abil OSW 5'' - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 20 10 5
"DC-8500" - Dow Coming (82% Bis(C13-15 Alkoxy) PG-
Amodimethicone, 18% C14-15 Alcohols) 2 1.5 1
Phenyl Trimethicone (DC-556) 2 1.5 1
Fragrance 0.5 0.5 0.5
DMDM Hydantoin 0.175 0.175 0.175
Cocos Nucifera (Coconut) Oil 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001
0.0001
Add the following and mix until unifolin
"Salcare SC-96" - Ciba/BASF (65% Polyquatemium-37, 25%
Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1 Trideceth-
6) 3 3 3
Mix until uniform
Target Specifications 91:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 20,000-30,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous opaque lotion
[0274] Compositions 9J-1 through 9J-3
9J-1 9J-2 9J-3
Item wt% wt% wt%
Main Phase
DI Water 25.8247 25.8247
25.8247
Glycerin 35 0 35
Propylene Glycol 0 35 0
Silicone Pre-Mix
"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 22 20 20
Amodimethicone (ADM 1100 (Wacker)) 2 2 2
Phenyl Trimethicone (DC-556) 0 2 2
Fragrance 0.5 0.5 0.5
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
89
DMDM Hydantoin 0.175 0.175
0.175
Cocos Nucifcra (Coconut) Oil 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001
0.0001
Sepigel 305 2 2 2
Mix moderately for ¨30 minutes and until smooth
Side Phase
DI Water 7.75 7.75 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125
0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5 4.5
4.5
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025 0.025 0.025
Slowly add side phase to main phase at < 45C
Mix until unifoiin
Target Specifications 9J:
pH: 7.0-8.0
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 5,000-15,000 cps
Color: colorless-slightly yellow
Odor: MS
Appearance: slightly hazy oily liquid
10275] Compositions 9K-1 through 9K-3
9K-1 9K-2 9K-3
Item wt% wt% wt%
_________________ Main Phase
DI Water 21.3247 31.3247 36.3247
Sprinklc in the following and mix until clear
Polyquatemium-4 (Celquat H-100) 0.5 0.5 0.5
Vinyl Caprolactum/VP/Dimethylaminocthyl Methacrylate
Copolymer ("Advantage S" (ISP))
0.25 0.25 0.25
Glycerin 35 35 35
POLYQUATERNIUM-11, WATER (20% active) 1.25 1.25 1.25
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
VP/Methacrylamide/Vinyl Imidazole Copolymer (''Luviset Clear"
(BASF)) - 20% active 2.5 2.5 2.5
Side Phase
DI Water 7.75 7.75 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5 4.5
4.5
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025 0.025 0.025
Slowly add side phase to main phase at < 45C
<45C
"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 20 10 5
"DC-8500" - Dow Coming (82% Bis(C13-15 Alkoxy) PG-
Amodimethicone, 18% C14-15 Alcohols) 2 1.5 1
Phenyl Trimethicone (DC-556) 2 1.5 1
Fragrance 0.5 0.5 0.5
DMDM Hydantoin 0.175 0.175 0.175
Cocos Nucifera (Coconut) Oil 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001
0.0001
Add the following and mix until uniform
"Sepigel 305" 2 3 4
Target Specifications 9K:
pH: 7.0-8.0
Viscosity (RV T-C, 10 rpm, 1 min, 25C): 50,000-100,000 cps
Color: clear-semi white
Odor: MS
Appearance: thick gel-thin liquid
[0276] Composition 9L
Item wt%
Main Phase
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
91
DI Water 31.325
PEG-90M 0.5
Heat to 90-95C
(glycerin can be added while heating)
Glycerin 12
Side Phase 1
Add the following in an appropriate side phase container, heat
to 90-95C, and mix under very moderate mixing
Mineral Oil (Paraffinum Liquidum) 9
Isocctcth-20 22
Oleth-2 8
After fully homogenous, add side phase to main phase
Mix vigorously for 45 mins at 90-95C, then allow to slowly
cool
Side Phase 2
DI Water 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5
(solution will turn opaque and become less viscous)
Add the following at < 45C
DMDM Hydantoin 0.025
Slowly add side phase to main phase at 60-70C
VP/MethacrylamiderVinyl Imidazole Copolymer ("Luviset
Clear" (BASF)) - 20% active 0.2
VP/VA Copolymer, Water 2.8
Methoxy PEG/PPG-7/3 Aminopropyl Dimethicone 1
Add the following at 45C
DMDM IIydantoin 0.175
Fragrance 0.5
Target Specifications 9L:
pH: 3.20-4.50
Penetration (50g weight w/ cone) 18-24mm
Color: Colorless
Odor: MS
Appearance: thick gel wax
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
92
[0277] Composition 9M
Item wt%
Main Phase
DI Water 31.2837
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.001
NaOH, 20% 0.00125
Add the following and mix vigorously
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 0.045
Slowly add the following, mix until hydrated
Polyquaternium 10 0.8
Heat to 50C and mix until clear
Disodium EDTA 0.1
COCAMIDOPROPYL BETAINE (-30% active), WATER,
SODIUM CHLORIDE 8.2
NaOH, 20% 0.14875
Sodium Laureth Sulfate- 1 mole (25%) 32
Disodium Laureth Sulfosuccinate (-34% active) 12.8
Styrene/ VP Copolymer (40%), Water 0.75
PEG-6 Caprylic/Capric Triglyceride 0.6
Kathon CG 0.07
Fragrance 0.7
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
Premix the following and add to the batch
DI Water 10
Sodium Chloride 2.5
Target Specifications 9M:
pH: 5.5-6.5
Viscosity (LVT/spindle 4/ 30 rpm/1 mm, 25C): 15,000-20,000 cps
Color: White/Off white (MS)
Odor: MS
Appearance: Viscous, opaque liquid
102781 Compositions 9N-1 and 9N-2
9N-1 9N-2
Item wt% wt%
Main Phase
DI Water 47.4497 60.2497
Start heat to 80-85C
Add the following one at time, mix until fully dissolved.
Disodium EDTA 0.05 0.05
L-Aspartic Acid 0.75 0.75
Add the following one at a time at 80-85C and mix until melted
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
93
Stearamidopropyl Dimethylamine 2 2
Cetyl Alcohol 4 1
Stearyl Alcohol 1 0
Glyceryl Stearate 1 0.2
"Crodamol STS'' (100% PPG-3 Benzyl Ether Myristate) 2 0
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 10 0
Side Phase
DI Water 15.5 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 9 9
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.05 0.05
Slowly add side phase to main phase at 45C
<45C
Fluid Blend 5 5
Fragrance 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001
DMDM Hydantoin 0.15 0.15
Add the following and mix until uniform
"Salcare" SC-96" - Ciba/BASF (65% Polyquatemium-37, 25%
Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1 Trideceth-6) 1 5
Target Specifications 9N:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 15,000-25,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
94
[0279] Composition 90
Item wt%
Main Phase
D1 Water 60.8497
Disodium EDTA 0.05
L-Aspartic Acid 0.75
Add the following one at a time at 80-85C and mix until
melted/homogeneous
Stearamidopropyl Dimethylamine 2
Cetyl Alcohol 1
Glyceryl Stearate 0.2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed; allow to cool and foam to reduce
Side Phase
DI Water 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2
Sodium Hydroxide (20% active) 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 9
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.05
Slowly add side phase to main phase at < 45C
<45C
Silicone Pre-Mix
Dimethicone (60,000 cst) 2
Phenyl Trimethicone (DC-556) 2
D5, Ditnethiconol (DC-1501) 1
Glycerin 1
Propylene Glycol 0.5
Fragrance 0.5
DMDM Hydantoin 0.15
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65% Polyquatemium-37, 25%
Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1 Trideceth-
6) 3
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
Target Specifications 90:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 mm, 25C): 5,000-15,000 cps
Color: White (MS)
Odor: MS
Appearance: opaque emulsion
[0280] Composition 9P
Item wt%
Main Phase
DI Water 52.8497
Disodium EDTA 0.05
L-Aspartic Acid 0.75
Add the following one at a time at 80-85C and mix until
melted/homogeneous
Stearamidopropyl Dimethylamine 2
Cetyl Alcohol 1
Glyceryl Stearate 0.2
Aminopropyl Dimethicone 0.5
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed; allow to cool and foam to reduce
Side Phase
DI Water 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2
Sodium Hydroxide (20% active) 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 9
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydanto in 0.05
Slowly add side phase to main phase at < 45C
<45C
Silicone Pre-Mix
"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 2
Dimethicone (60,000 cst) 1
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
96
"DC-8500" - Dow Corning (82% Bis(C13-15 Alkoxy) PG-
Amodimethicone, 18% C14-15 Alcohols) 1
Propylene Glycol 10
Fragrance 0.5
DMDM Hydantoin 0.15
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65% Polyquaternium-37, 25%
Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1 Trideceth-
6) 3
Target Specifications 9P:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 mm, 25C): 10,000-20,000 cps
Color: White (MS)
Odor: MS
Appearance: opaque emulsion
10281] Composition 9Q
Item wt%
Main Phase
DI Water 52.8
Disodium EDTA 0.05
L-Aspartic Acid 0.75
Add the following one at a time at 80-85C and mix until
melted/homogenous
Stearamidopropyl Dimethylamine 2
Cetyl Alcohol 1
Glyceryl Stearate 0.2
Aminopropyl Dimethiconc 0.5
Mix Vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool _______________________
Side Phase
DI Water 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BS (ISP)) 0.2
Sodium Hydroxide (20% Active) 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat side Phase to 50-55C
Slowly add the following under very rigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% Active) 9
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
97
(solution will turn opaque and become less viscous)
Add the following at < 45C
DMDM Hydantoin 0.05
Slowly add side phase to main phase at <45C
<45C
Pre-mix next two
DS, Dimethiconol 2
Dimethicone 1
DC-8500 1
Propylene Glycol 10
Fragrance 0.5
DMDM Hydantoin 0.2
Salcare SC-96 3
Target Specifications 9Q:
pH: 4.50-6.00
Viscosity (RV T-8, 10 rpm, 1 min, 25C):
bulk: 7,000-15,0000 cps
Color: White (MS)
Odor: MS
Appearance: opaque emulsion
[0282] Composition 9R
Item wt% _
Main Phase
DI Water 40.55
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BS (ISP)) 0.2
Sodium Hydroxide (20% Active) _________________________________ 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat to 50-55C
Slowly add the following under very rigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% Active) 9
(solution will turn opaque and become less viscous)
Start heat to 80-85C
Add the following one at a time, mix until fully dissolved.
Disodium EDTA 0.05
L-Aspartic Acid 0.75
DI Water 20.27
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
98
Add the following one at a time at 80-85C and mix until
melted/homogenous
Stearamidopropyl Dimethylamine 2
Cetyl Alcohol 4
"Montanov 202" 1.18
Glyceryl Stearate 0.80
"Crodamol STS" (Benzyl Ether Myristate) 2
Salcare SC-96 1
Aminopropyl Dimethicone 0.75
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool.
<45C
Pre-mix next two
DS, Dimethiconol 3
Dimethicone 1.5
DC 2-8566 (Amodimethicone) 2
Propylene Glycol 10
Fragrance 0.5
DMDM Hydantoin 0.2
Target Specifications 9R:
1-1- 4 50 6 00
Viscosity (RV T-8, 10 rpm, 1 min,
25C):
bulk: 15,0000-25,000 cps
Color: White (MS)
Odor: MS
Appearance: opaque emulsion
[0283] Compositions 9S-I through 9S-6
9S-1 9S-2 9S-3 9S-4 9S-5 9S-6
Main Phase wt% wt% wt% wt% wt% wt%
DI Water 64.75565217
59.5252 64.86434783 59.6252 64.75565217 59.5252
Add the following under
vigorous mixing, mix
until hydrated (clear)
Polyquaternium-4
(Celquat L-200) 0.5 0.46 0.5 0.46 0.5 0.46
"Advantage S" (ISP) 0.25 0.23 0.25 0.23 0.25 0.23
Citric Acid 0.02 0.0184 0.02 0.0184 0.02
0.0184
Liquid Additions:
POLYQUATERNIUM-
11, WATER (AQUA) 1.57 1.4444 1.57 1.4444 1.57
1.4444
POLYQUATERNIUM-7 1 0.92 1 0.92 1 0.92
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
99
DC S-7113 Silicone
Quat Microemulsion
(Dow Corning) 1 0.92 1 0.92 1 0.92
PROPYLENE
GLYCOL, USP 2.25 2.07 2.25 2.07 2.25 2.07
COCAMIDOPROPYL
BETAINE, WATER,
SODIUM CHLORIDE 0.4 0.368 0.4 0.368 0.4 0.368
Side Phase
DI Water 16.84782609 15.55 16.84782609 15.55
16.84782609 15.55
Slowly add the
following, mix until
hydrated.
PVM/MA Copolymer
(Gantrez S-97 BS (ISP)) 0.2173913 0.2 0.2173913 0.2
0.2173913 0.2
Sodium Hydroxide (20%
Active) 0.27173913
0.25 0.27173913 0.25 0.27173913 0.25
(solution will slightly
thicken)
in-process pH
specification: 6.90-7.00
Heat to 50-55C
Slowly add the following
under very rigorous
mixing
Polyquaternium-28
(Conditioneze NT-20
(ISP)) 9.7826087 9 9.7826087 9
9.7826087 9
(solution will turn
opaque and become less
viscous)
Slowly add side phase to
main phase.
Pre-mix next and
Fragrance
POLYSORI3ATE 20,
WATER 0.70 0.644 0.70 0.644 0.7
0.644
Fragrance 0.43478261 0.4 0.32608696
0.3 0.43478261 0.4
Propellant Charge
Isobutane and Propane
and 152A 0 8 0 8 0 8
Target Specifications 9S (also for Composition 6J):
(Bulk) (Finished Goods)
pH: 5.0-6.5 5.0-6.5
color: off white (MS) white (ms)
odor: MS MS
appearance: hazy milky liquid dense foam, non-watery, non-runny
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
100
[0284] Composition 9T
Item wt%
Main Phase
DI Water 40.55
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2
Sodium Hydroxide (20% active) 0.25
(solution with slightly thicken)
In-process pH specification: 6.90-7.00
Record pH: 6.95
Heat to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP)) 9
(solution will turn opaque and become less viscous)
DI Water 39.05
Disodium EDTA 0.05
Salcare SC-96 3
Mix until uniform
<45C
Dimethicone (DC-200, 20 cst) 3
Phenyl Trimethicone (DC-556) 2
Cyclopentasiloxane, Dimethiconol 1
Glycerin 1
=
Propylene Glycol 0.5
Fragrance 0.2
DMDM Hydantoin 0.2
Target Specifications 9T:
pH 5.00-6.50
Viscosity (RV T-B, 10 rpm, 1 min, 25C)
Bulk: 7,000-15,000 cps
Color Semi-Translucent white (MS)
Odor MS
Appearance Viscous, milky fluid
[0285] Composition 9U
Item wt%
Main Phase
DI Water 60.85_
Disodium EDTA 0.05
L-Aspartic Acid 0.75
Add the following one at a time at 80-85C and mix until
melted/homogenous
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
101
Stearamidopropyl Dimethylamine 2
Cetyl Alcohol 1
Glycerol Stearate 0.2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed; allow to cool and foam to reduce
Side Phase
DI Water 15.50
Slowly add the following; mix until hydrated
PVM/MA Copolymer (Gantrez S-97)BF (ISP)) 0.2
Sodium Hydroxide (20% active) 0.25
(solution will slightly thicken)
In-process pH specification 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP)) 9
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
add the following at <45C
DMDM Hydantoin 0.05
Slowly add side phase to main phase at <45C
<45C
Silicone Pre-Mix
Dimethicone (60,000 cst) 2
Phenyl Trimethicone (Dc-556) 2
DS, Dimethiconol (DC-1501) 1
Glycerin 1
Propylene Glycol 0.5
Fragrance 0.5
DMDM Hydantoin 0.15
Salcare SC-96 3
Target Specifications 9U:
pH 4.5-6.50
Viscosity (RV T-B, 10 rpm, 1 min, 25C)
Bulk: 8,000-16,000 cps
Color White (MS)
Odor MS
Appearance opaque emulsion
[0286] Compositions 9V-1 through 9V-3
9V-1 9V-2 9V-3
Item wt% wt% wt%
Main Phase
DI Water 24.99 24.99 24.99
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
102
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5 0.5 0.5
Disodium EDTA 0.05 0.05 0.05
Liquid Additions:
PVP K-90 (20%) 1 1 1
"Luviset Clear" (BASF) 3.5 3.5 3.5
Polyquaternium 39 0.5 0.5 0.5
Propylene Glycol 1 1 1
Sorbitol 70% 0.5 0.5 0.5
Aminomethyl Propanol (AMP -95) 0.15 0.15 0.15
Side Phase 1
DI Water 40 40 40
Aminomethyl Propanol (AMP-95) 0.02 0.02 0.02
Add the following under very vigorous mixing for 30 mins.
"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1 1 1
Add the following and mix until uniform
Aminomethyl Propanol (AMP-95) 0.15 0.15 0.15
Add Side Phase 1 to main tank and mix until uniform
Add the following and mix until uniform
Aminomethyl Propanol (AMP-95) 0.14 0.14 0.14
Side Phase 2
DI Water 15.55 15.55 15.55
Slowly add the following; mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP)) 9 9 9
(solution will turn opaque and become less viscous)
Slowly add Side Phase 2 to main tank
<45C
Pre-mix next two and fragrance
PEG-40 Hydrogenated Castor Oil 0.6 0.6 0.6
DC-190 0.1 0.1 0.1
Fragrance 0.6 0.6 0.6
DMDM Hydantoin 0.2 0.2 0.2
Target Specifications 9V:
pH: 6.5-7.5
Viscosity (RV T-C, 5 rpm, 1 min, 25C):
bulk: 40,000-90,000
Color: White (MS)
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
103
Odor: MS
Appearance: Viscous, opaque gel
[0287] Compositions 9W-1 through 9W-3
9W-1 9W-2 9W-3
Item wt% wt% wt%
Main Phase
DI Water 47.4497 60.2497 60.25
Start heat to 80-85C
Add the following one at a time, mix until fully dissolved
Disodium EDTA 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75
Add the following one at a time at 80-85C and mix until
melted
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 4 1 1
Stearyl Alcohol 1 0 0
Glyceryl Stearate 1 0.2 0.2
"Crodamol STS" (100% PPG-3 Benzyl Ether Myristate) 2 0 0
Mix Vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 10 0 0
Side Phase
DI Water 15.5 15.5 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BS (TSP)) 0.2 0.2 0.2
Sodium Hydroxide (20% Active) 0.25 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat side Phase to 50-55C
Slowly add the following under very rigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20%
Active) 9 9 9
(solution will turn opaque and become less viscous)
(mix for "10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.05 0.05 0.05
Slowly add side phase to main phase at <43C
<45C
Fluid Blend 5 5 5
Fragrance 0.6 0.6 0.6
Coco Nucifera (Coconut) Oil 0.0001 0.0001 0
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
104
Keratin Amino Acids 0.0001 0.0001 0
Flower/Leaf Extract 0.0001 0.0001 0
DMDM Hydantoin 0.15 0.15 0.15
Add the following and mix until uniform
Salcare SC-96 - Ciba/BASF (65% Polyquatemium-37,
25% Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 5 5
Target Specifications 9W:
PH 4.5-6.00
Viscosity (RV T-8, 10 rpm, 1 min, 25C) 15,000-25,000 cps
Color White (MS)
Odor MS
Appearance Viscous, opaque emulsion
[0288] Compositions 9X-1 and 9X-2
9X-1 9X-2
Item wt% wt%
Main Phase
DI Water 54.45 52.05
Start heat to 80-85C
Add the following one at a time, mix until fully dissolved and
solution becomes clear
Disodium EDTA- 0.05 0.05
L-Aspartie Acid 0.75 0.75
Add the following one at a time at 80-85C and mix until melted
Stearamidopropyl Dimethylaminc 2 2
Check to make sure solution has turned clear
Cetyl Alcohol 5 ____ 7
Glyceryl Stearate 1 1.4
Vigorously mix for 30 minutes at 80-85C
After 30 minutes, turn off heat, slow mixing speed and
allow to slowly cool
Side Phase
DI Water 15.5 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP)) 9 9
(solution will turn opaque and become less viscous)
Add the following at <45C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
105
DMDM Hydantoin 0.05 0.05
Slowly add side phase to main phase at <45C
Abil T Quat 60 (Evonik) ¨ Silicone Quatemium ¨ 22 1 1
Propylene Glycol 10 10
Fragrance 0.6 0.6
DMDM Hydantoin 0.15 0.15
Target Specifications 9X:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1
min, 25C):
Bulk: 7,000-15,000 cps
w/ shear (finished goods): 20,000-35,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous, opaque emulsion
EXAMPLE 10
[0289] This example demonstrates exemplary addition rates, addition times,
temperatures, mixing speeds, and mixing times for producing PECs.
[0290] - Water Densities: Perry's Chemical Engineer's Handbook.
[0291] - densities for NaOH 20% = 1.2191 kg/L and Conditioneze = 1.042
kg/L.
[0292] One 270-kg batch
the PEC Complex in 113-liter / 30-gallon premix vessel with center turbine
agitator only
main batch in 227-liter / 60-gallon mixing vessel with center turbine and side
sweep agitators
Processing Parameters for PEC Complex:
[0293] Initial Water Charge = 42.02 L (41.85 kg)
Addition Rate = 28 L/min (28 kg/min)
Total Addition Time = 1.5 minutes
Initial Water Temperature = 29 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
106
[0294] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)
Addition Rate = 0.6 kg/min
Total Addition Time = 1 minute
Temperature = 30 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Dispersion Mix Time = 30 minutes
[0295] Sodium Hydroxide, 20% = 0.55 L (0.675 kg)
Addition Rate = 0.6 L/min (0.7 kg/min)
Total Addition Time = 1 minute
Temperature = 30 C
Center Turbine Agitator = Slow (RPM) clockwise direction
Side Sweep Agitator ¨ None in Pilot Premix Tank
Hydration Mix Time = 20 minutes
In-Process pH Check = 6.90
Heat Premix for 10 minutes to 51 C
[0296] Polyquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)
Addition Rate = 3.33 L/min (3.47 kg/min)
Total Addition Time = 7 minutes
Temperature = 49 C
Center Turbine Agitator = Moderate/High (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Complex Mix Time = 40 minutes
[0297] Premix Cool Down
Cool to 29 C
Center Turbine Agitator = Very Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Cool Down Mix Time = 60 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
107
[0298] One 11,800-kg batch
The PEC Complex in 5,678-liter / 1,500-gallon premix vessel with center
turbine and side
sweep agitators
main batch in MO1 12,113-liter / 3,200-gallon mixing vessel with center
turbine and side
sweep agitators
Processing Parameters for PEC Complex:
[0299] Initial Water Charge = 1840.9 L (1835 kg)
Addition Rate = 526 L/min (524 kg/min)
Total Addition Time = 3.5 minutes
Temperature = 26 C
Center Turbine Agitator ¨ 25 RPM counter-clockwise direction
Side Sweep Agitator = 7 RPM clockwise direction
[0300] PVM/MA Copolymer (Gantrez S-97 BF) = 23.6 kg (solid)
Addition Rate = 7.87 kg/min
Total Addition Time = 3 minutes
Temperature = 27 C
Center Turbine Agitator = 20 RPM counter-clockwise direction
Side Sweep Agitator = 7 RPM clockwise direction
Dispersion Mix Time = 30 minutes
[0301] Sodium Hydroxide, 20% = 24.2 L (29.5kg)
Addition Rate = 12.1 L/min (14.75 kg/min)
Total Addition Time = 2 minute
Temperature = 27 C
Center Turbine Agitator = 20 RPM counter-clockwise direction
Side Sweep Agitator = 7 RPM clockwise direction
Hydration Mix Time = 10 minutes
In-Process pH Check = 6.72. Add additional 118 grams (0.001 wt%) of NaOH and
pH =
6.80. Add additional 118 grams (0.001 wt%) of NaOH and pH = 6.90. Total of
29.736 kg of
NaOH
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
108
Heat Premix for 18 minutes to 55 C
[0302] Polyquaternium 28 (Conditioneze NT-20) = 1019 L (1062 kg)
Addition Rate = 29.1 L/min (30.3 kg/min)
Total Addition Time = 35 minutes
Temperature = 54 C
Center Turbine Agitator = 28 RPM counter-clockwise direction
Side Sweep Agitator = 7 RPM clockwise direction
Complex Mix Time = 30 minutes
[0303] Premix Cool Down
Cool to 35 C
Center Turbine Agitator = 18 RPM counter-clockwise direction
Side Sweep Agitator = 7 RPM clockwise direction
Cool Down Mix Time = 240 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
[0304] One 270-kg batch
The PEC Complex in 113-liter / 30-gallon premix vessel with center turbine
agitator only
the main batch in 227-liter / 60-gallon mixing vessel with center turbine and
side sweep
agitators
Processing Parameters for PEC Complex:
[0305] Initial Water Charge = 42.04 L (41.84 kg)
Addition Rate = 28 L/min (28 kg/min)
Total Addition Time = 1.5 minutes
Initial Water Temperature = 31 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Heat Premix for 10 minutes to 52 C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
109
[0306] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)
Addition Rate = 0.6 kg/min
Total Addition Time = 1 minute
Temperature = 52 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Dispersion Mix Time = 25 minutes
[0307] Sodium Hydroxide, 20% = 0.56 L (0.688 kg)
Addition Rate = 0.6 L/min (0.7 kg/min)
Total Addition Time = 1 minute
Temperature = 52 C
Center Turbine Agitator = Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Hydration Mix Time = 15 minutes
In-Process pH Check = 6.93
[0308] Polyquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)
Addition Rate =4.66 L/min (4.86 kg/min)
Total Addition Time = 5 minutes
Temperature = 53 C
Center Turbine Agitator = Moderate/High (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Complex Mix Time = 40 minutes
[0309] Premix Cool Down
Cool to 29 C
Center Turbine Agitator = Very Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Cool Down Mix Time = 100 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
110
[0310] One 270-kg batch
The PEC Complex in 113-liter / 30-gallon premix vessel with center turbine
agitator only)
the main batch in 227-liter / 60-gallon mixing vessel with center turbine and
side sweep
agitators
Processing Parameters for PEC Complex:
[0311] Initial Water Charge = 42.03 L (41.85 kg)
Addition Rate = 28 L/min (28 kg/min)
Total Addition Time ¨ 1.5 minutes
Initial Water Temperature = 30 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
[0312] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)
Addition Rate = 0.6 kg/min
Total Addition Time = 1 minute
Temperature = 30 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Dispersion Mix Time = 30 minutes
[0313] Sodium Hydroxide, 20% = 0.56 L (0.68 kg)
Addition Rate = 0.6 L/min (0.7 kg/min)
Total Addition Time = 1 minute
Temperature = 31 C
Center Turbine Agitator = Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Hydration Mix Time = 6 minutes
In-Process pH Check = Original 6.83. Add additional 2.7 grams (0.001 wt%) of
NaOH and
pH = 6.95. Total of 682.7 g of NaOH
Heat Premix for 10 minutes to 57 C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
111
[0314] Polyquatemium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)
Addition Rate = 3.33 L/min (3.47 kg,/min)
Total Addition Time = 7 minutes
Temperature = 56 C
Center Turbine Agitator -= Moderate/High (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Complex Mix Time = 30 minutes
[0315] Premix Cool Down
Cool to 27 C
Center Turbine Agitator = Very Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Cool Down Mix Time = 120 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
[0316] One 1,250-kg batch
The PEC Complex in 379-liter / 100-gallon premix vessel with center turbine
and side sweep
agitators
the main batch in 1,893-liter / 500-gallon mixing vessel with center turbine
and side sweep
agitators
Processing Parameters for PEC Complex:
[0317] Initial Water Charge = 195.2 L (194.4 kg)
Addition Rate = 97.6 L/min (97.2 kg/min)
Total Addition Time = 2 minutes
Temperature = 29 C
Center Turbine Agitator = 60 RPM counter-clockwise direction
Side Sweep Agitator = 10 RPM clockwise direction
[0318] PVM/MA Copolymer (Gantrez S-97 BF) = 2.5 kg (solid)
Addition Rate = 1.3 kg/min
Total Addition Time = 2 minutes
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
112
Temperature = 31 C
Center Turbine Agitator = 60 RPM counter-clockwise direction
Side Sweep Agitator = 10 RPM clockwise direction
Dispersion Mix Time = 26 minutes
[0319] Sodium Hydroxide, 20% = 2.56 L (3.125 kg)
Addition Rate = 3 L/min (4 kg/min)
Total Addition Time = 1 minute
Temperature = 33 C
Center Turbine Agitator = 20 RPM counter-clockwise direction
Side Sweep Agitator = 10 RPM clockwise direction
Hydration Mix Time = 11 minutes
In-Process pH Chcck = 6.90
Heat Premix for 10 minutes to 52 C
[0320] Polyquaternium 28 (Conditioneze NT-20) = 108.0 L (112.5 kg)
Addition Rate = 9.0 L/min (9.4 kg/min)
Total Addition Time = 12 minutes
Temperature = 54 C
Center Turbine Agitator = 58 RPM counter-clockwise direction
Side Sweep Agitator = 15 RPM clockwise direction
Complex Mix Time ¨ 31 minutes
[0321] Premix Cool Down
Cool to 35 C
Center Turbine Agitator = 18 RPM counter-clockwise direction
Side Sweep Agitator = 8 RPM clockwise direction
Cool Down Mix Time = 135 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
[0322] One 270-kg batch
The PEC Complex in 113-liter / 30-gallon premix vessel with center turbine
agitator only
the main batch in 227-liter / 60-gallon mixing ves el with center turbine and
side sweep
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
113
agitators
Processing Parameters for PEC Complex:
[0323] Initial Water Charge = 42.01 L (41.84 kg)
Addition Rate = 28 L/min (28 kg/min)
Total Addition Time = 1.5 minutes
Initial Water Temperature = 29 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Heat Premix for 10 minutes to 52 C
[0324] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)
Addition Rate = 0.6 kg/min
Total Addition Time = 1 minute
Temperature = 52 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Dispersion Mix Time = 25 minutes
[0325] Sodium Hydroxide, 20% = 0.57 L (0.69 kg)
Addition Rate = 0.6 L/min (0.7 kWmin)
Total Addition Time = 1 minute
Temperature = 53 C
Center Turbine Agitator = Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Hydration Mix Time = 5 minutes
In-Process pH Check = 6.95
[0326] Polyquatemium 28 (Conditioneze NT-20) --- 23.32 L (24.30 kg)
Addition Rate = 4.66 L/min (4.86 kg/min)
Total Addition Time = 5 minutes
Temperature = 53 C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
114
Center Turbine Agitator = Moderate/High (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Complex Mix Time = 35 minutes
[0327] Premix Cool Down
Cool to 30 C
Center Turbine Agitator = Very Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Cool Down Mix Time = 90 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
[0328] One 270-kg batch
The PEC Complex in 113-liter / 30-gallon premix vessel with center turbine
agitator only
the main batch in 227-liter / 60-gallon mixing vessel with center turbine and
side sweep
agitators
Processing Parameters for PEC Complex:
[0329] Initial Water Charge = 42.01 L (41.84 kg)
Addition Rate = 28 L/min (28 kg/min)
Total Addition Time = 1.5 minutes
Initial Water Temperature = 29 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
[0330] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)
Addition Rate = 0.6 kg/min
Total Addition Time = 1 minute
Temperature = 30 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Dispersion Mix Time ¨ 30 minutes
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
115
[0331] Sodium Hydroxide, 20% = 0.56 L (0.68 kg)
Addition Rate = 0.6 L/min (0.7 kg/min)
Total Addition Time = 1 minute
Temperature = 30 C
Center Turbine Agitator = Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Hydration Mix Time = 20 minutes
In-Process pH Check = Original 6.81. Add additional 3.4 grams (0.00126 wt%) of
NaOH
and pH = 6.92. Total of 683.4 g of NaOH
Heat Premix for 10 minutes to 54 C
[0332] Polyquatemium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)
Addition Rate = 3.33 L/min (3.47 kg/min)
Total Addition Time = 7 minutes
Temperature = 54 C
Center Turbine Agitator = Moderate/High (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Complex Mix Time = 35 minutes
[0333] Premix Cool Down
Cool to 35 C
Center Turbine Agitator = Very Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Cool Down Mix Time = 260 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
[0334] One 3,772-kg batch
The PEC Complex in 1,893-liter / 500-gallon premix vessel with center turbine
and side
sweep agitators
the main batch in 3,785-liter! 1000-gallon mixing vessel with center turbine
and side sweep
agitators)
Processing Parameters for PEC Complex:
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
116
[0335] Initial Water Charge = 588.93 L (586.546 kg)
Addition Rate = 392.6 L/min (391 kg/min)
Total Addition Time = 1.5 minutes
Temperature = 29 C
Center Turbine Agitator = 46 RPM counter-clockwise direction
Side Sweep Agitator = 10 RPM clockwise direction
[0336] PVM/MA Copolymer (Gantrez S-97 BF) = 7.544 kg (solid)
Addition Rate = 3.77 kg/min
Total Addition Time = 2 minutes
Temperature = 29 C
Center Turbine Agitator = 46 RPM counter-clockwise direction
Side Sweep Agitator = 10 RPM clockwise direction
Dispersion Mix Time = 60 minutes
[0337] Sodium Hydroxide, 20% = 7.735 L (9.430 kg)
Addition Rate = 3.9 L/min (4.7 kg/min)
Total Addition Time = 2 minute
Temperature = 30 C
Center Turbine Agitator = 25 RPM counter-clockwise direction
Side Sweep Agitator = 10 RPM clockwise direction
Hydration Mix Time = 10 minutes
In-Process pH Check = 6.91
Heat Premix for 10 minutes to 52 C
[0338] Polyquaternium 28 (Conditioneze NT-20) = 325.80 L (339.48 kg)
Addition Rate = 16.3 L/min (17.0 kg/min)
Total Addition Time = 20 minutes
Temperature = 50 C
Center Turbine Agitator = 35 RPM counter-clockwise direction
Side Sweep Agitator = 6 RPM clockwise direction
Complex Mix Time = 40 minutes
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
117
103391 Premix Cool Down
Cool to 40 C
Center Turbine Agitator = 14 RPM counter-clockwise direction
Side Sweep Agitator = 6 RPM clockwise direction
Cool Down Mix Time = 55 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
103401 One 270-kg batch
The PEC Complex in 113-liter / 30-gallon premix vessel with center turbine
agitator only
the main batch in 227-liter / 60-gallon mixing vessel with center turbine and
side sweep
agitators
Processing Parameters for PEC Complex:
103411 Initial Water Charge = 42.01 L (41.84 kg)
Addition Rate = 28 L/min (28 kg/min)
Total Addition Time = 1.5 minutes
Initial Water Temperature = 29 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Heat Premix for 10 minutes to 52 C
[0342] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)
Addition Rate = 0.6 kg/min
Total Addition Time = 1 minute
Temperature = 52 C
Center Turbine Agitator = Moderate (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Dispersion Mix Time = 20 minutes
103431 Sodium Hydroxide, 20% = 0.57 L (0.69 kg)
Addition Rate = 0.6 L/min (0.7 kg/min)
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
118
Total Addition Time = 1 minute
Temperature = 53 C
Center Turbine Agitator = Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Hydration Mix Time = 6 minutes
In-Process pH Check = 6.98
[0344] Polyquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)
Addition Rate = 4.66 L/min (4.86 kg/min)
Total Addition Time = 5 minutes
Temperature = 53 C
Center Turbine Agitator = Moderate/High (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Complex Mix Time = 35 minutes
[0345] Premix Cool Down
Cool to 29 C
Center Turbine Agitator = Very Slow (RPM) clockwise direction
Side Sweep Agitator = None in Pilot Premix Tank
Cool Down Mix Time = 100 minutes*
(*Note: Mix time reflects time required to get main batch to addition point
for PEC Premix)
EXAMPLE 11
[0346] This example describes exemplary compositions of the present
invention
(Compositions 11A-11G).
[0347] The hair mending efficacy of some of these compositions (with
Composition 1C)
is summarized in Tables 13 and 14. The high humidity curl retention of some of
these
compositions is shown in Figure 7.
[0348] Composition 11A
Item wt%
Main Phase
DI Water 66.525
Sprinkle in the following and mix until clear
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
119
Polyquaternium-4 (Celquat H-100) 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl
Methacrylate Copolymer ("Advantage S" (ISP)) 0.5
Liquid Additions:
POLYQUATERNIUM-11, WATER (20%
active) 5
VP/Methacrylamide/Vinyl Imidazole Copolymer
("Luviset Clear" (BASF)) - 20% active 5
Side Phase
DI Water 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat to 50-55C
Slowly add the following under very vigorous
mixing
Polyquatcrnium-28 (Conditioneze NT-20 (ISP)) 4.5
(solution will turn opaque and become less
viscous)
DMDM Hydantoin 0.025
Slowly add side phase to main phase at < 45C
"Sa'care SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Di caprylate Dicaprate, 10% PPG-1 Trideceth-6) 3
Mix until uniform
<45C
Silicone Premix
Dimethicone (60,000 cst) 2
Phenyl Trimethicone (DC-556) 2
Cyclopentasiloxane, Dimethiconol 1
Glycerin 1
Propylene Glycol 0.5
Fragrance 0.3
DMDM Hydantoin 0.175
Target Specifications 11A:
pH: 5.00-6.50
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 20,000-40,000 cps
Color: Semi-white (MS)
Odor: MS
Appearance: Viscous, opaque gel
103491 Composition 11B
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
120
Item wt%
Main Phase
DI Water 69.4247
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl
Methacrylate Copolymer ("Advantage S"
(ISP)) 0.5
Liquid Additions
POLYQUATERNIUM-11, WATER (20%
active) 5
VP/Methacrylamide/Vinyl Imidazole
Copolymer ("Luviset Clear" (BASF)) - 20%
active 5
Polyquaternium-39 (8.5% active) 0.5
Propylene Glycol 1
Sorbitol (70%) 0.5
Side Phase
DI Water 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous
mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 4.5
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025
Slowly add side phase to main phase at < 45C
<45C
Pre-mix next two and fragrance
PEG-40 Hydrogenated Castor Oil 0.4
PEG/PPG-18/18 Dimethicone (DC-190) 0.1
Fragrance 0.4
DMDM Hydantoin 0.175
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
121
Add the following and mix until uniform
Polyacrylamide, C13-14 Isoparaffin, Laureth-7
("Sepigel 305") 4
Target Specifications 11B:
pH: 6.0-7.5
Viscosity (RV T-C, 5 rpm, 1 min, 25C): 50,000-100,000 cps
Color: Semi-white
Odor: MS
Appearance: Thick gel
[0350] Composition 11C
Item wt%
Main Phase
DI Water 75.725
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5
POLYQUATERNIUM-11, WATER (20% active) 2.5
PEC Pre-mix
DI Water 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-procesS pH specification: 6.90-7.00
Heat to 50-55C
Slowly add the following under very vigorous
mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP)) 4.5
(solution will turn opaque and become less viscous)
mix for 10 minutes
1--
Add the following at < 45C
DMDM Hydantoin 0.025
Slowly add side phase to main phase at < 45C
<45C
Silicone Premix
Dimethicone (60,000 cst) 2
Phenyl Trimethicone (DC-556) 2
Cyclopentasiloxane, Dimethiconol 1
Glycerin 1
Propylene Glycol 0.5
Fragrance 0.1
DMDM Hydantoin 0.175
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
122
"Salcare SC-96" - Ciba/BASF (65% Polyquatemium-
37, 25% Propylene Glycol Dicaprylate Dicaprate,
10% PPG-1 Trideceth-6) 2
Mix until uniform
Target Specifications 11C:
pH: 5.00-6.50
Viscosity (RV T-B, 10 rpm, 1 mm, 25C): 5,000-15,000 cps
Color: Semi-translucent white (MS)
Odor: MS
Appearance: Viscous, milky liquid
103511 Composition 11D
11D-1 11D-2
Item wt% wt%
Main Phase
DI Water 67.5247 55.0497
Sprinkle in the following and mix until clear
Polyquaternium-4 (Celquat H-100) 0.5 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate
Copolymer ("Advantage S" (ISP)) 0.25 0.25
Disodium EDTA 0.05 0.05
L-Aspartic Acid 0.75 0.75
Add the following one at a time at 80-85C and mix until
melted/homogeneous
Stearamidopropyl Dimethylamine 2 2
Cetyl Alcohol 1 1
Glyceryl Stearate 0.2 0.2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed; allow to cool and foam to reduce
Liquid Additions:
POLYQUATERNIUM-11, WATER (20% active) 1.25 1.25
VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset
Clear" (BASF)) - 20% active 2.5 2.5
Side Phase
DI Water 7.75 15.5
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.2
Sodium Hydroxide (20% active) 0.125 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
123
Slowly add the following under very vigorous mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5 9
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025 0.05
Slowly add side phase to main phase at < 45C
<45C
"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 3 3
"DC-8500" - Dow Coming (82% Bis(C13-15 Alkoxy) PG- 1
Amodimethicone, 18% C14-15 Alcohols)
Phenyl Trimethicone (DC-556) 2 2
Fragrance 0.3 0.3
DMDM Hydantoin 0.175 0.15
Cocos Nucifera (Coconut) Oil 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65% Polyquatemium-37,
25% Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 5 5
_________________ Mix until uniform
Target Specifications 11D:
pH: 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 20,000-30,000 cps
Color: White (MS)
Odor: MS
Appearance: Viscous opaque lotion
[0352] Composition 11E
Item wt%
Main Phase __________________________________________________
DI Water 26.2247
Propylene Glycol 35
Silicone Pre-Mix
"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 20
Amodimethicone (ADM 1100 (Wacker)) (410.50/kg) 2
Phenyl Trimethicone (DC-556) 2
Fragrance 0.1
DMDM Hydantoin 0.175
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
124
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
Polyacrylamide, C13-14 lsoparaffin, Laureth-7 ("Sepigel
305") 2
Mix moderately for ¨30 minutes and until smooth
Side Phase
DI Water 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (1SP), 20% active) 4.5
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025
Slowly add side phase to main phase at < 45C
Mix until uniform
Target Specifications 11E:
pH: 6.5-7.5
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 5,000-15,000 cps
Color: Colorless-slightly yellow
Odor: MS
Appearance: Slightly hazy oily liquid
[0353] Composition 11F
Item wt%
Main Phase
DI Water 17.7747
Propylene Glycol 35
VP/Methacrylamide/Vinyl lmidazole Copolymer ("Luviset
Clear" (BASF)) - 20% active 3.75
VP/VA Copolymer, Water 1.5
Silicone Pre-Mix
"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%
Dimethiconol, 1% Dimethicone) 22
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
125
Phenyl Trimethicone (DC-556) 2
Fragrance 0.3
DMDM Hydantoin 0.175
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
Polyacrylamide, C13-14 Isoparaffin, Laureth-7 ("Sepigel
305") 5
Mix moderately for ¨30 minutes and until smooth
Side Phase
DI Water 7.75
Slowly add the following, mix until hydrated
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1
Sodium Hydroxide (20% active) 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous mixing
Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5
(solution will turn opaque and become less viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025
Slowly add side phase to main phase at < 45C
Mix until uniform
Target Specifications 11F:
pH: 6.5-7.5
Viscosity (RV T-C, 5 rpm, 1 min, 25C): 50,000-100,000 cps
Color: Colorless-slightly yellow
Odor: MS
Appearance: Slightly hazy viscous wax
[0354] Compositions 11G-1 through 11G-4
11G-1 11G-2 11G-3 11G-4
Main Phase wt% wt% wt% wt%
DI Water 76.803586 70.6593 76.803586
70.6593
Add the following under vigorous mixing,
mix until hydrated (clear)
Polyquaternium-4 (Celquat H-100) 0.543478 0.5 0.543478 0.5
Vinyl Caprolactum/VP/Dimethylaminoethyl
Methacrylate Copolymer ("Advantage S"
(ISP)) 0.543478 0.5 0.543478 0.5
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
126
Citric Acid 0.02 0.0184 0.02
0.0184
Liquid Additions:
POLYQUATERNIUM-11, WATER (21.5%
active) 2.717391 2.5 2.717391 2.5
POLYQUATERNIUM-7 (8.5% active) 1 0.92 1 0.92
DC 5-7113 Silicone Quat Microemulsion -
Dow Coming (66% Water, 25% Silicone
Quatemium-16, 7.4% Undeceth-11, 4.5%
Butyloctanol, 3.5% Undeceth-5) 1 0.92 1 0.92
PROPYLENE GLYCOL, USP 2.25 2.07 2.25 2.07
COCAMIDOPROPYL BETAINE (-30%
active), WATER, SODIUM CHLORIDE 0.4 0.368 0.4 0.368
Side Phase
DI Water 8.423913 7.75 8.423913
7.75
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.108696 0.1 0.108696 0.1
Sodium Hydroxide (20% active) 0.13587 0.125 0.13587
0.125
(solution will slightly thicken) _______________________________________
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquatemium-28 (Conditioneze NT-20
(ISP), 20% active) 4.891304 4.5 4.891304 4.5
(solution will turn opaque and become less
viscous)
Add the following at < 45C
DMDM Hydantoin 0.027174 0.025 0.027174
0.025
Slowly add side phase to main phase
Pre-Mix next and Fragrance
POLYSORBATE 20 0.7 0.644 0.7 0.644
Fragrance 0.434783 0.4 0.434783 0.4
Cocos Nucifera (Coconut) Oil 0.000109 0.0001 0.000109
0.0001
Keratin Amino Acids 0.000109 0.0001 0.000109
0.0001
Flower/Leaf Extract 0.000109 0.0001 0.000109
0.0001
Propellant Charge
Isobutane and Propane and 152A (78.5%
A46; 28.5% HFC 152A) 0 8 0 8
Target Specifications Bulk:
pH: 5.0-6.5
Color: Off white (MS)
Odor: MS
Appearance: Hazy liquid
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
127
Target Specifications Finished Product:
pH: 5.0-6.5
Color: White (MS)
Odor: MS
Appearance: Dense foam, non-watery, non-runny
Foam stability: 200 seconds min
Spray diameter (at 8"): foam
Spray pattern (at 8"): foam
10355] Table 13
Tress#
Composition 11C Composition 11A Composition 11B Composition
11E
Fiber >'\ 3 4 5 6 7 8 9 10
1 1 1 1 1 1 1 1 1
2 1 1 1 1 I 1 1 1
3 1 0.5 1 1 1 0 0.5 1
4 1 1 1 1 1 1 1 1
1 1 1 0.5 1 1 1 1
6 1 1 0.5 1 1 1 1 1
7 1 0.5 1 1 1 1 1 1
8 1 1 1 1 1 1 1 1
9 1 1 1 1 0 1 1 1
1 1 1 1 0 1 1 1
Total 10 9 9.5 9.5 8 9 9.5 10
%
Mended 0.95 0.95 0.85 0.975
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
128
[0356] Table 14
Tress # Composition 11F Composition 110-2 Composition
11D-1 Composition IC
Fiber # 11 12 13 14 15 16 17 18
1 0.5 1 1 1 1 1 1 1
2 1 1 1 1 1 1 1 1
3 1 1 1 1 1 1 1 0.5
4 1 1 1 1 1 1 1 1
1 1 1 1 1 0.5 1 1
6 1 0.5 1 1 1 0.5 0.5 1
7 1 1 1 1 1 1 1 1
8 1 1 0.5 1 1 1 1 1
9 I 1 0.5 1 1 1 1 1
1 1 1 1 0.5 1 0.5 1
Total 9.5 9.5 9 10 9.5 9 9 9.5
%
Mended 0.95 0.95 0.925 0.925
EXAMPLE 12
[0357] This example demonstrates alleviation of weakening of hair, due to
hot flat
ironing, by compositions of the present invention.
[0358] Comparative Composition 12A
Main Phase wt%
DI Water 69.9897
Aminomethyl Propanol (AMP-95) 0.02
Add the following under very vigorous mixing for 30
mins.
"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) I
Add the following and mix until uniform
Aminomethyl Propanol (AMP-95) 0.44
Side Phase 1
DI Water 20
Sprinkle in the following and mix until clear
Polyquatemium-4 (Celquat H-100) 0.5
Disodium EDTA 0.05
Liquid Additions:
PVP K-90 (20% active) 1
VP/Methacrylamide/Vinyl Imidazole Copolymer
("Luviset Clear" (BASF)) - 20% active 3.5
Polyquatemium-39 (8.5% active) 0.5
Propylene Glycol 1
Sorbitol (70%) 0.5
Add Side Phase 1 to main tank and mix until uniform
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
129
<45C
Pre-mix next three
PEG-40 Hydrogenated Castor Oil 0.6
PEG/PPG-18/18 Dimethicone (DC-190) 0.1
Fragrance 0.6
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
DMDM Hydantoin 0.2
Specifications 12A:
pH: 6.0-7.0
Viscosity (RV T-C, 5 rpm, 1 mm, 25C): 40,000-80,000
Color: White (MS)
Odor: MS
Viscous, opaque (hazy)
Appearance: gel
[0359] Comparative Composition 12B
Ingredients % wt.
Water (Aqua, Eau) 39.52699
Aminomethyl Propanol, Water (about 5% water) 0.02
Acrylic Acid/VP Crosspolymer 1
Water (Aqua, Eau) 23.2
Aminomethyl Propanol, Water (about 5% water) 0.44
Water (Aqua, Eau) 20
Water (Aqua, Eau) 0.013
Dye 0.000013
Polyquatemium-4 0.5
Disodium EDTA 0.05
PVP (20%), Water (Aqua, Eau) 4
VP/Methacrylamide/Vinyl Imidazole Copolymer (about 20%),
water 3.5
Polyquaternium-39 (8.58%), Water 0.5
Propylene Glycol 1
Sorbitol, Water (30% Water) 0.5
Aminomethyl Propanol, Water (about 5% water) 0.15
Water (Aqua, Eau) 4.8
Oleth-20 0.45
Fragrance 0.15
DMDM Hydantoin (55%), Water 0.2
[0360] Into a main stainless steel compounding tank, charge cold water, set
at 68 - 86 F
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
130
(20 ¨ 86 C) with vigorous mixing (turbine mixer at vigorous counterclockwise
direction; side
sweep mixer at moderate clockwise direction).
[0361] Add the first Aminomethyl Propanol (AMP-95) addition to the main
compounding tank and mix until completely dispersed.
[0362] Next, slowly sprinkle the acrylic acid/VP crosspolymer powder into
the main
compounding tank with vigorous agitation (vortex where possible; turbine mixer
at vigorous
counterclockwise direction; side sweep mixer at moderate clockwise direction).
An eductor
or any other in-line disperser may be used for this addition. Use caution
during addition of
the powder, as it will clump if added too quickly. Mix the batch for a minimum
of 45
minutes or until the polymer is completely dispersed and no particles or lumps
are present.
While mixing, begin preparing the Celquat Premix.
[0363] Take a sample from the main compounding tank and visually verify
that all of the
polymer has been dispersed and there are no particles or lumps. If particles
or lumps remain,
continue vigorous mixing and resample periodically until the batch is uniform.
[0364] Next, after the dispersion has been visually approved, charge DI
water to the main
compounding tank with moderate agitation (turbine mixer at moderate
counterclockwise
direction; side sweep mixer at slow clockwise direction). Use care when
charging the water,
and reduce the mixing to avoid aeration. This water charge should bring the
batch level
above the top blades to avoid splashing and aeration during the neutralization
step. Mix the
batch for a minimum of 15 minutes or until the batch is smooth and
homogeneous.
[0365] Once the batch is uniform after the DI water charge, continue to mix
moderately
(turbine mixer at moderate counterclockwise direction; side sweep mixer at
moderate
clockwise direction) and add the second Aminomethyl Propanol (AMP-95) addition
to the
main compounding tank to neutralize the polymer. The solution will eventually
turn clear
and the viscosity will increase dramatically. Mix the batch for a minimum of
20 minutes or
until the batch is uniform.
[0366] In a suitable, stainless steel premix tank, charge the following
cold Water set at 68
- 86 F (20 - 30 C). Begin vigorous mixing (turbine mixer at vigorous
counterclockwise
direction; side sweep mixer at moderate clockwise direction, if available).
[0367] In a suitable stainless steel container, premix dye in wan-n water,
set at 104 -
113 F (40 - 45 C), where available. Mix until the dye is completely dissolved
and uniform.
Mix until the premix is uniform and free of any undissolved particles. Once
the Dye Premix
is ready, add this solution to the phase tank.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
131
[0368] Next, slowly sprinkle the Polyquatemium-4 powder into the phase tank
with
vigorous agitation (vortex where possible; turbine mixer at vigorous
counterclockwise
direction; side sweep mixer at moderate clockwise direction, if available). An
eductor or any
other in-line disperser may be used for this addition. Use caution during
addition of the
powder, as it will clump if added too quickly. Mix the batch for a minimum of
30 minutes or
until there are no particles or lumps.
[0369] Take a sample from the phase tank and visually verify that all of
the polymer has
been dispersed and there are no particles or lumps. If particles or lumps
remain, continue
vigorous mixing and resample periodically until the batch is uniform.
[0370] Once the phase is clear and uniform, add the following items to the
premix tank
(turbine mixer at vigorous counterclockwise direction; side sweep mixer at
moderate
clockwise direction, if available): disodium EDTA; PVP K-90 (20% solution);
VP/Methacrylamide/Vinyl Imidazole Copolymer; polyquatemium-39; propylene
glycol;
sorbitol; aminomethyl propanol.
[0371] Once the premix is ready, add it to the main compounding tank. Rinse
the premix
tank with cold water set at 68 - 86 F (20 - 30 C) and add it to the main
compounding tank
(turbine mixer at moderate counterclockwise direction; side sweep mixer at
moderate
clockwise direction, if available). Mix the batch for a minimum of 20 minutes
or until the
batch is uniform.
[0372] Prepare the following fragrance premix in a suitable, sanitized
container equipped
with an electric or air mixer: oleth-20; fragrance. Oleth-20 should be pre-
melted at 95 ¨
104 F (35 ¨ 40 C) for homogeneity and ease of handling. Do not mix this
ingredient with
fragrance if it is above 110 f (43 c) or the fragrance will flash off. Mix
this premix
vigorously until it is clear and free of any undissolved material. Visually
verify that it is clear
and free of particles and then add it to the main compounding tank with
moderate agitation.
[0373] Check that the batch temperature is 104 F (40 C) or below (cool the
batch if
necessary), and then add the DMDM hydantoin to the main compounding tank with
moderate
agitation (turbine mixer at moderate counterclockwise direction; side sweep
mixer at
moderate clockwise direction). Mix for a minimum of 30 minutes or until the
batch is
completely uniform. Sample the composition. Discontinue mixing and cooling (if
applicable).
[0374] Adjustments that may be made are the following. If the pH is low,
add
aminomethyl propanol at a maximum of 5% of the total batch requirement. If the
pH is high,
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
132
add citric acid at a maximum of 0.1% of the total batch size, premixing in
water first (20%
solution). if the viscosity is low, mix an additional 60 minutes and resample.
Pumps that
should be used for pumping material into the tanks include air diaphragm and
positive
displacement. Filters that should be used include 80 mesh for all transfer
operations. The fill
temperature should be 68-95 F (20-35 C).
[0375] Composition 12C
Main Phase wt%
DI Water 45.0397
Aminomethyl Propanol (AMP-95) 0.02
Add the following under very vigorous mixing for
30 mins.
Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1
Add the following and mix until uniform
Aminomethyl Propanol (AMP-95) 0.44
Side Phase 1
DI Water 20
Sprinkle in the following and mix until clear
Polyquatemium-4 (Celquat H-100) 0.5
Disodium EDTA 0.05
Liquid Additions:
PVP K-90 (20% active) 1
VP/Methacrylamide/Vinyl Imidazole Copolymer
("Luviset Clear" (BASF)) - 20% active 3.5
Polyquatemium-39 (8.5% active) 0.5
Propylene Glycol 1
Sorbitol (70%) 0.5
Add Side Phase 1 to main tank and mix until
uniform
Side Phase 2
DI Water 15.5
Slowly add the following, mix until hydrated _
PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2
Sodium Hydroxide (20% active) 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very vigorous
mixing
Polyquatemium-28 (Conditioneze NT-20 (ISP), 20%
active) 9
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
133
(solution will turn opaque and become less viscous)
Slowly add Side Phase 2 to main tank and mix until
uniform
<45C
Pre-mix next three
PEG-40 Hydrogenated Castor Oil 0.6
PEG/PPG-18/18 Dimethicone (DC-190) 0.1
Fragrance 0.6
Cocos Nucifera (Coconut) Oil 0.0001
Keratin Amino Acids 0.0001
Flower/Leaf Extract 0.0001
DMDM Hydantoin 0.2
Specifications 12C:
pH: 6.0-7.0
Viscosity (RV T-C, 5 rpm, 1 min, 25C): 40,000-80,000
Color: White (MS)
Odor: MS
Viscous, opaque (hazy)
Appearance: gel
[0376] Comparative Composition 12D: Rhodapex ES-2 (sodium laureth sulfate)
from
Rhodia, diluted with water to 12% active.
[0377] Quantification of Fiber Fragmentation:
Shampoo tress with sodium lauryl ether sulfate.
Apply a set quantity of test material to damp hair and distribute uniformly.
Blow dry tress without combing.
Flat Iron at 205 C. Pull the flat iron from the top to the bottom of the
tress in
approximately 12 seconds; repeat 5 times for a total of one minute. Let tress
cool. Repeat
thermal process for another 3 minutes (total of 4 minutes).
Repeat all of the above three times.
Shampoo tress with sodium lauryl ether sulfate.
Blow Dry w/o combing
Place translucent plastic under tress.
Comb 100 times with fine teeth of comb (realistic strokes, i.e. rate of
stroking).
Tape over plastic to secure fragments.
Number all collected hair fragments.
Calculate percent reduction in hair breakage (protection):
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
134
% hair breakage reduction =[(C ¨ T)/C] x 100
C = # of hair pieces collected for the control
T = # of hair pieces collected for the test
[0378] Equipment used for spectrofluorimetry-tryptophan degradation is a
Spectrofluorimeter-Horiba Jobin Yvon FluoroMax 4. Measurements are taken on
five
different locations in a window 2.3 cm in width and 1.7 cm in height located
in the upper part
or root section of the tress which is 2 inches from the bottom of the binding
of the tress to the
mid-point of the window. Settings of the equipment during measurements are:
Excitation: 290 nm wavelength; 5mm slit
Emission: from 300-400 nm; 5 mm slit; mm increments
Measurements of the emission spectra from 300-400 nm are recorded in
increments of 1 nm.
Five measurements at 336 nm (the maximum point for tryptophan emission) are
then
averaged. This is done for the initial reading as well as after the hot
ironing process. Percent
degradation is calculated as follows:
(Are.5 ellit1S19 Siang ar 336 nen before tresitemeta- AVR.S gm-mission
readings at 33 6 ram after treatmen joali
Ave. 5 eintniss fang at 3315 nm before treatment
Percent protection is calculated as:
r Degradation of control - ty, degradation of experimental))
X 10007
% degradation of control
[0379] Humidity conditions: Hair tresses are stored overnight at 22% RH (76
C dry
bulb; 54 C wet bulb). Combing tests are conducted at 30% RH (75 C dry bulb;
56 C wet
bulb).
[00100] Tables 15 and 16 show the anti-breakage data. Table 15 shows the
number of hair
pieces. Table 16 shows percent reduction in breakage versus Composition 12D.
[00101] Table 15
Regimen Tress 1 Tress 2 Tress 3 Tress 4 Tress 5
12A 352 338 408 202 140
12B 327 294 241 272 172
12C 154 82 157 121 128
12C 412 503 234 289 342
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
135
[0380] Table 16
% Reduction vs.
Regimen Ave. (n = 5) Std. dev. 12D
12A 288.0 112.1 19.1
12B 261.2 58.9 26.6
12C 128.4 30.3 63.9
12D 356.0 105.3
[0381] Figure 8 shows percent thermal protection via tryptophan
measurements.
Composition 12C significantly decreases tryptophan degradation. Also, the
trend in percent
tryptophan loss correlates well with quantification of fiber fragmentation.
[0382] This examples shows that the gel with PEC significantly reduced
fiber
fragmentation from combing and percent tryptophan loss.
EXAMPLE 13
[0383] This
example demonstrates freeze-thaw stability of exemplary compositions of the
present invention.
[0384] Compositions 13A-13D
Composition Composition Composition Composition
13A 13B 13C 13D
Item wt% wt% wt% wt% _
Main Phase
DI Water 69.9497 64.9497 59.9497
64.9497
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2 2
Cetyl Alcohol 4 4 4 4
Stearyl Alcohol 1 1 1 1
Glyccryl Stcaratc 1 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 2 2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
136
Add the following at 65-70C
Propylene Glycol 0 5 10 0
Glycerin 0 0 0 5
Sorbitol (70%) 0 0 0 0
Side Phase
DI Water 7.75 7.75 7.75 7.75
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.1 0.1 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125 0.125 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquatemium-28 (Conditioneze NT-20
(ISP), 20% active) 4.5 4.5 4.5 4.5
(solution will turn opaque and become less
viscous)
(mix for -10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.025 0.025 0.025 0.025
Slowly add side phase to main phase at <
45-65C
<45C
"Fluid Blend" 5 5 5 5
Fragrance 0.6 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
DMDM Hydantoin 0.15 0.15 0.15 0.15
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65%
Polyquatemium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 1 1
[0385] Compositions 13E-13G
Composition Composition Composition
13E 13F 13G
Item wt% wt% wt%
Main Phase
DI Water 59.9497 62.8097 55.6697
Start heat to 80-85C
Add the following one at time, mix until
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
137
fully dissolved.
Disodium EDTA 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 4 4 4
Stearyl Alcohol 1 1 1
Glyceryl Stearate 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool _________________________
Add the following at 65-70C
Propylene Glycol 0 0 0
Glycerin 10 0 0
Sorbitol (70%) 0 7.14 14.28
Side Phase
DI Water 7.75 7.75 7.75
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.1 0.1 0.1
Sodium Hydroxide (20% active) 0.125 0.125 0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquatemium-28 (Conditioneze NT-20
(ISP), 20% active) 4.5 4.5 4.5
(solution will turn opaque and become less
viscous)
(mix for -10 minutes)
Add the following at < 45C
DMDM Hydantoin 0,025 0.025 0.025
Slowly add side phase to main phase at <
45-65C
<45C
"Fluid Blend" 5 5 5
Fragrance 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
DMDM IIydantoin 0.15 0.15 0.15
Add the following and mix until uniform
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
138
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 1
Specifications 13C-131: 24 hour specifications
13C-131:
pH: 4.50-6.00 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min, 25C): 15,000-25,000 cps 20,000-30,000cps
Color: White (MS) White (MS)
Odor: MS MS
Appearance: Viscous, opaque emulsion Viscous, opaque emulsion
103861 Compositions 13H-13K
Composition Composition Composition Composition
13H 131 13.1 13K
Item wt% wt% wt% wt%
Main Phase
DI Water 57.4497 52.4497 47.4497
52.4497
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Steararnidopropyl Dimethylamine 2 2 2 2
Cetyl Alcohol 4 4 4 4
Stearyl Alcohol 1 1 1 1
Glyccryl Stearate 1 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 2 2
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 0 5 10 0
Glycerin 0 0 0 5
Sorbitol (70%) 0 0 0 0
Side Phase
DI Water 15.5 15.5 15.5 15.5
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.2 0.2 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25 0.25 0.25
(solution will slightly thicken)
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
139
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 9 9 9 9
(solution will turn opaque and become less
viscous)
(mix for -10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.05 0.05 0.05 0.05
Slowly add side phase to main phase at <
45-65C
<45C
Fluid Blend" 5 5 5 5
Fragrance 0.6 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
DMDM Hydantoin 0.15 0.15 0.15 0.15
Add thc following and mix until uniform
"Salcare SC-96" - Ciba/l3ASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 11
[0387] Compositions 13L-13N
Composition Composition Composition
13L 13M 13N
Item wt% wt% wt%
Main Phase
DI Water 47.4497 50.3097 43.1697
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75
Add thc following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 4 4 4
Stearyl Alcohol 1 1 1
Glyceryl Stearate 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 2
Mix vigorously for 30 minutes at 80-85C
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
140
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 0 0 0
Glycerin 10 0 0
Sorbitol (70%) 0 7.14 14.28
Side Phase
DI Water 15.5 15.5 15.5
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.2 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 9 9 9
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Add the following at < 45C
DMDM Hydantoin 0.05 0.05 0.05
Slowly add side phase to main phase at 5_
45-65C
<45C
"Fluid Blend" 5 5 5
Fragrance 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
DMDM Hydantoin 0.15 0.15 0.15
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 1
Specifications 13J-13P: 24 hour specifications 13J-13P:
pH: 4.50-6.00 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min,
25C): 15,000-25,000 cps 20,000-30,000cps
Color: White (MS) White (MS)
Odor: MS MS
Appearance: Viscous, opaque emulsion Viscous, opaque emulsion
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
141
[0388] Compositions 130-13R
Composition Composition Composition Composition
130 13P 13Q 13R
Item wt% wt% wt% wt%
Main Phase
DI Water 38.4497 50.9247 55.2497 67.7247
Side Phase
DI Water 15.5 7.75 15.5 7.75
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.2 0.1 0.2 0.1
Sodium Hydroxide (20% active) 0.25 0.125 0.25
0.125
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquatemium-28 (Conditioneze NT-20
(ISP), 20% active) 9 4.5 9 4.5
(solution will turn opaque and become less
viscous)
(mix for -10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2 2
Cetyl Alcohol 4 4 1 1
Stearyl Alcohol 1 1 0 0
Glyceryl Stearate 1 1 0.2 0.2
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 0 0
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 10 10 0 0
<45C
''Fluid Blend" 5 _____ 5 5 5
Fragrance 0.6 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
142
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
DMDM Hydantoin 0.2 0.2 0.2 0.2
Add the following and mix until uniform
Notes: Leave 10% hole. Post add
Water/Salcare" SC-96 for varying levels of
Salcare (1-10%) to achieve final viscosity
spec. 10 10 10 10
DI Water
'Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6)
Initial Specifications 130- 24 hour specifications
13T: 130-13T:
pH: 4.50-6.00 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1 min,
25C): 15,000-25,000 cps 20,000-30,000cps
Color: White (MS) White (MS)
Odor: MS MS
Appearance: Viscous, opaque emulsion Viscous, opaque emulsion
[0389] Compositions 13S-13V
Comparative Comparative
Composition Composition Composition Composition
13S 13T 13U 13V
Item wt% wt% wt% wt%
Main Phase
DI Water 85.3997 60.3997 60.3997
84.3997
Side Phase
DI Water 0 15.55 0 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0.2 0 _______ 0
,
Sodium Hydroxide (20% active) 0 0.25 0 0
(solution will slightly thicken)
In-process p1-1 specification: 6.90-7.00
____ Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquatemium-28 (Conditioneze NT-20
(ISP), 20% active) 0 9 0 0
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
143
fully dissolved.
Disodium EDTA 0.05 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2 2
Cetyl Alcohol 4 4 4 4
Stearyl Alcohol 1 1 1 1
Glyceryl Stearate 1 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 0 0 0 0
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0 0 1
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 0 0 0 0
Side Phase
DI Water 0 0 15.55 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0 0.2 0
Sodium Hydroxide (20% active) 0 0 0.25 0
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 0 9 0
(solution will turn opaque and become less
viscous)
(mix for -10 minutes)
Slowly add side phase to main phase at
45-65C
<45C
"Fluid Blend" 5 5 5 5
Fragrance 0.6 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
DMDM Hydantoin 0.2 0.2 0.2 0.2
Add the following and mix until uniform
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
144
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0 0 0
[0390] Compositions 13W-13Z
Comparative
Composition Composition Composition Composition
13W 13X 13Y 13Z
Item wt% wt% wt% wt%
Main Phase
DI Water 59.3997 59.3997 84.3997
59.3997
Side Phase
DI Water 15.55 0 0
15.55
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.2 0 0 0.2
Sodium Hydroxide (20% active) 0.25 0 0 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquatemium-28 (Conditioneze NT-20
(ISP), 20% active) 9 0 0 9
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2 2
Cetyl Alcohol 4 4 4 4
Stearyl Alcohol 1 1 1 1
Glyceryl Stearate 1 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 0 0 0 0
"Salcare" SC-96" - Ciba/BASF (65%
Polyquatemium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 0 0
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
145
Add the following at 65-70C
Propylene Glycol 0 0 0
Side Phase
DI Water 0 15.55 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0.2 0 0
Sodium Hydroxide (20% active) 0 0.25 0 0
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 9 0 0
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Slowly add side phase to main phase at 5._
45-65C
<45C
"Fluid Blend" 5 5 5 5
Fragrance 0.6 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
DMDM Hydantoin 0.2 0.2 0.2 0.2
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0 1 1
[0391] Compositions 13AA-13CC
Composition Composition Composition
13AA 13BB 13CC
Item wt% wt% wt%
Main Phase
DI Water 59.3997 57.3997 49.3997
Side Phase
DI Water 0 0 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0 0
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
146
Sodium Hydroxide (20% active) 0 0 0
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
_______ Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 0 0
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 4 4 4
Stearyl Alcohol 1 1 1
Glyccryl Stearate 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 0 2 0
"Salcare" SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0 0
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 0 0 10
Side Phase
DI Water 15.55 15.55 15.55
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.2 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 9 9 9
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
147
Slowly add side phase to main phase at <
45-65C
<45C
"Fluid Blend" 5 5 5
Fragrance 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
DMDM Hydantoin 0.2 0.2 0.2
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 1
[0392] Compositions 13DD and 13EE
Composition Composition
13DD 13EE
Item wt% wt%
Main Phase
DI Water 47.3997 60.1997
Side Phase
DI Water 0 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrcz S-97 BF
(ISP)) 0 0
Sodium Hydroxide (20% active) 0
(solution will slightly thicken)
In-process p1-1 specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 0
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
_________________ fully dissolved.
Disodium EDTA 0.05 0.05
L-Aspartic Acid 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
148
Stearamidopropyl Dimethylamine 2 2
Cetyl Alcohol 4 1
Stearyl Alcohol 1 0
Glyceryl Stearate 1 0.2
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 0
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 10 0
Side Phase
DI Water 15.55 15.55
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0.2 0.2
Sodium Hydroxide (20% active) 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 9 9
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Slowly add side phase to main phase at <
45-65C
<45C
"Fluid Blend" 5 5
Fragrance 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001
DMDM Hydantoin 0.2 0.2
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 5
Initial Specifications 24 hour
specifications
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
149
13U-13GG: 13U-13GG:
1-1- 4 50 6 00 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1
min, 25C): 15,000-25,000 cps 20,000-30,000cps
Color: White (MS) White (MS)
Odor: MS MS
Appearance: Viscous, opaque emulsion Viscous, opaque emulsion
[0393] Compositions 13FF-13HH
Comparative
Composition Composition Composition
13FF 13GG 13HH
Item wt% wt% wt%
Main Phase
DI Water 72.3997 47.3997 47.3997
Side Phase
DI Water 0 15.55 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0.2 0
Sodium Hydroxide (20% active) 0 0.25 0
(solution will slightly thicken)
hi-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 9 0
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium EDTA 0.05 0.05 0.05_
L-Aspartic Acid 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2
Cetyl Alcohol 4 4 4
Steaul Alcohol 1 1 1
Glyceryl Stearatc 1 1 1
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 2
"Salcare SC-96" - Ciba/BASF (65%
Polyquatemium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1 1 1 1
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
150
Trideceth-6)
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 10 10 10
Side Phase
DI Water 0 0 15.55
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0 0.2
Sodium Hydroxide (20% active) 0 0 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 0 9
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Slowly add side phase to main phase at <
45-65C
<45C
"Fluid Blend" 5 5 5
Fragrance 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
DMDM Hydantoin 0.2 0.2 0.2
Add the following and mix until uniform
"Salcare SC-96" - Ciba/F3ASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0 0
[0394] Compositions 1311-13 LL
Comparative
Composition Composition Composition Composition
1311 13JJ 13KK. 13LL
Item wt% wt% wt% wt%
Main Phase
DI Water 72.3997 47.3997 47.3997 61.4997
Side Phase
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
151
DI Water 0 15.55 0 0
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0.2 0 0
Sodium Hydroxide (20% active) 0 0.25 0 0
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 9 0 0
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Start heat to 80-85C
Add the following one at time, mix until
fully dissolved.
Disodium FDTA 0.05 0.05 0.05 0.05
L-Aspartic Acid 0.75 0.75 0.75 0.75
Add the following one at a time at 80-85C
and mix until melted
Stearamidopropyl Dimethylamine 2 2 2 ______ 2
Cetyl Alcohol 4 4 4 0
Stearyl Alcohol 1 1 1 0
Glyceryl Stearate 1 1 1 0
"Crodamol STS" (100% PPG-3 Benzyl
Ether Myristate) 2 2 2 0
"Salcare SC-96" - Ciba/BASF (65%
Polyquaternium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 0 0 0 0
Mix vigorously for 30 minutes at 80-85C
Reduce mixing speed and allow to cool
Add the following at 65-70C
Propylene Glycol 10 10 10 0
Side Phase
DI Water 0 0 15.55 15.5
Slowly add the following, mix until
hydrated
PVM/MA Copolymer (Gantrez S-97 BF
(ISP)) 0 0 0.2 0.2
Sodium Hydroxide (20% active) 0 0 0.25 0.25
(solution will slightly thicken)
In-process pH specification: 6.90-7.00
Heat Side Phase to 50-55C
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
152
Slowly add the following under very
vigorous mixing
Polyquaternium-28 (Conditioneze NT-20
(ISP), 20% active) 0 0 9 9
(solution will turn opaque and become less
viscous)
(mix for ¨10 minutes)
Slowly add side phase to main phase at <
45-65C
<45C
"Fluid Blend" 5 5 5 5
Fragrance 0.6 0.6 0.6 0.6
Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001
0.0001
Keratin Amino Acids 0.0001 0.0001 0.0001
0.0001
Flower/Leaf Extract 0.0001 0.0001 0.0001
0.0001
DMDM Hydantoin 0.2 0.2 0.2 0.15
Add the following and mix until uniform
"Salcare SC-96" - Ciba/BASF (65%
Polyquatemium-37, 25% Propylene Glycol
Dicaprylate Dicaprate, 10% PPG-1
Trideceth-6) 1 1 1 5
Initial Specifications 131114- 24 hour specifications
13MM: 13HH-13MM:
pH: 4.50-6.00 4.50-6.00
Viscosity (RV T-B, 10 rpm, 1
min, 25C): 15,000-25,000 cps 20,000-30,000cps
Color: White (MS) White (MS)
Odor: MS MS
Appearance: Viscous, opaque emulsion Viscous, opaque emulsion
103951 The procedure for the freeze/thaw stability studies is as follows:
1. Fill the finished product in a glass jar. If running package stability,
fill product in a
container of appropriate packaging.
2. After jar and package have been filled, label each. Tape around the labels
to ensure they
stay in place throughout the stability study.
Record an initial pH, viscosity, appearance, color and odor for the batch
before placing
into freezer.
3. Place all of the jars/packages into a freezer for a period of 24 hours.
4. After a period of 24 hours take samples out of the freezer and set them
on a bench either
in a plastic bin or on a paper towel. Let the samples thaw for 24 hours.
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
153
5. After another period of 24 hours check the appearance, color and odor of
the sample. If
applicable, measure pH and viscosity. Record results.
[0396] Measuring the viscosity uses the following parameters: RV, T-bar B,
lOrpm, 60
sec, 25 C (except when over 40,000 cps, where the method was RV, T-bar C, 5
rpms, 60 sec,
25 C).
[0397] Tables 17-20 show viscosity (cps) and pH readings of several of the
compositions
described above.
[0398] Table 17
13A 13B 13C 13D 13E 13F 130
Initial pH 4.92 4.94 4.88 4.79 4.69 4.77 4.75
Vise. 22,000 20,000 19,600 18,200 15,600 16,800 19,200
24 hr pH 4.90 4.91 4.86 4.77 4.73 4.73 4.81
Vise. 25,200 24,800 23,600 19,600 22,800 29,600 31,600
[0399] Table 18
131 13J 13K 13L 13M 13N
24 hr pH 4.90 4.87 4.93 4.86 5.04 4.90
Vise. 20,600 22,000 26,400 23,600 28,400 35,600
[0400] Table 19
Composition 130 Composition 13P
Initial 24h Initial 24h
% SC
96 pH Viscosity pH Viscosity pH Viscosity pH
Viscosity
1 4.87 5200 4.88 5600 4.78 10400 4.81 12100
2 4.93 18200 4.95 18900 4.79 18000 4.80 19200
3 4.94 19700 4.95 21800 4.81 70400 4.83 79000
4 4.96 118000 4.97 128000 4.83 392000 4.84 412000
4.87 146000 4.89 159000 4.85 528000 4.87 534000
6 4.98 392000 5.00 401000 4.80 810000 4.81 n/a
7 4.97 930000 5.01 n/a 4.80 n/a 4.82 n/a
8 4.93 n/a 4.94 n/a 4.80 n/a 4.80 n/a
9 5.00 n/a 4.98 n/a 4.81 n/a 4.80 n/a
4.97 , n/a 4.87 n/a 4.84 n/a 4.84 n/a
n/a = greater than 1 MM
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
154
[0401] Table 20
Composition 13Q Composition 13R
Initial 24h Initial 24h
% SC
96 pH Viscosity pH Viscosity pH Viscosity pH
Viscosity
1 4.74 1600 4.77 1600 4.72 600 4.68 600
2 4.76 2400 4.77 2800 4.73 2800 4.67 2400
3 4.78 6800 4.85 7200 4.72 7600 4.67 7600
4 4.79 11600 4.82 12200 4.71 16400 4.67 16000
5 4.80 19600 4.81 20000 4.70 24400 4.66 24200
6 4.80 26600 4.80 26800 4.66 26800 4.62 26800
7 4.79 28400 4.80 29200 4.65 30400 4.62 30600
8 4.74 36800 4.76 36800 4.66 38400 ' 4.61 38800
9 4.69 76800 4.71 75200 4.61 64800 4.59 64600
10 4.69 144800 4.71 146200 4.61 73600 4.58 73800
[0402] Salcare SC-96 recommendations regarding Compositions 130-13R: use 1-
5% for
130, 0.5-3% for 13P, 2-10% for 13Q, 2-12% for 13R.
[04031 Figure 9 shows a comparison of Compositions 13H-13J and 13EE for
evaluation
of the effectiveness of varying glycols on freeze/thaw stability. Composition
13H does not
exhibit freeze thaw stability. Adding 5% propylene glycol (Composition 131)
does not
greatly improve freeze/thaw stability. Adding 10% propylene glycol
(Composition 13J) or
lowering cetyl alcohol to 1% with Salcare SC 96 (Composition 13EE) shows
freeze/thaw
stability.
[0404] Figure 10 shows a comparison of Compositions 13K-13N. Different
glycols, such
as glycerin and sorbitol, are not as effective as propylene glycol in
improving freeze/thaw
stability.
[0405] Figure 11 shows a comparison of Compositions 13A-13C. Lowering the
Polyelectrolyte Complex to 1% shows less severe freeze/thaw instability, but
freeze/thaw
stability is not optimal (13A vs. 13H). Five percent propylene glycol (13B)
shows some
improvement; 10% (13C) shows positive results.
[0406] Figure 12 shows a comparison of Compositions 13D-13G. Glycerin and
sorbitol
do not show freeze/thaw stability, even when Polyelectrolyte Complex is
lowered to 1%.
104071 Figure 13 shows a comparison of Compositions 13S-13U. Adding
Polyelectrolyte
Complex to emulsion "crashes" the viscosity (13S (no PEC) vs. 13T (with PEC)
vs. 13U
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
155
(with PEC)). Adding Polyelectrolyte Complex after emulsion phase is complete
(13U) has
slightly less effect than adding it before (13T).
[0408] Figure 14 shows a comparison of Compositions 13V-13X. Adding Salcare
SC-96
before the emulsion phase can be used to thicken an emulsion, when the
Polyelectrolyte
Complex is added before or after the emulsion (13W and 13X vs. 13T and 13U).
However,
initial viscosity is low and final viscosity takes about 72 hours to build,
which is not preferred
in a production environment. Also, 13X is not preferred in a production
environment because
the batch is too thick and hard to mix during the emulsion phase (does not
have the additional
water and PEC to lower viscosity in the batch). Freeze/thaw stability and
spreadability can
be improved by the addition of propylene glycol or Crodamol STS.
[0409] Figure 15 shows a comparison of Compositions 13FF-13HH. Adding
propylene
glycol and Crodamol STS does not negatively affect emulsion viscosity (similar
results to
13V, 13W, 13X, except viscosity is thicker initially). 13GG is a possible
candidate for a one
tank process, however, its final viscosity is lower than 13DD/13KK. 13HH is
still not
preferred in production because the batch is too thick during emulsion phase.
[0410] Figure 16 shows a comparison of Compositions 13Y-13AA. Adding
Salcare SC-
96 after the emulsion phase also can be used to thicken an emulsion when
Polyelectrolyte
Complex is added before or after the emulsion (13Z and 13AA vs. 13T and 13U).
13AA is
preferred over 13X from a production standpoint because the batch is not too
thick and can be
properly mixed. The Polyelectrolyte Complex can be added after the emulsion
for a thick
final product (13AA vs. 13Z). Like 13W and 13X, the Freeze/Thaw stability and
spreadability can be improved with the addition of propylene glycol or
Crodamol STS.
[0411] Figure 17 shows a comparison of Compositions 131I-13KK. Adding
propylene
glycol and Crodamol STS improves initial and final emulsion viscosity (13JJ
and 13KK vs.
13Z and 13AA). Complex addition before the emulsion is not preferred because
viscosity is
thin (13JJ vs. 131(K).
[0412] Figure 18 shows a comparison of compositions 13BB-13DD. Both
propylene
glycol and Crodamol STS increase viscosity individually, as well as
collectively.
[0413] Figure 19 shows a comparison of compositions 13EE and 13LL. Crodamol
STS
and propylene glycol can be removed if cetyl alcohol is lowered to 1% and
Salcare SC-96 is
increased to 5% (13EE). Not including cetyl alcohol yields a product that
lacks fundamental
"conditioner characteristics" (opaqueness, emulsion body) (13LL).
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
156
EXAMPLE 14
[0414] This example demonstrates split-end mending of exemplary
compositions of the
invention.
[0415] Composition 14A
I. Prepare 2% active PVM/MA copolymer
Part A
DESCRIPTION
DEIONIZED WATER 94.4
20% NaOH 3.6
GANTREZ S-97 BF Polymer 2
Adjust pH to 6.95+/- 0.05 with NaOH if
necessary
II. Prepare 2% active Polyquat-28
Part B
DESCRIPTION
DEIONIZED WATER 90.25
CONDITIONEZE NT-20 9.755
III. Combine A&B (Complex Concentrate)
Part C
DESCRIPTION
Part A 5
Part B 45
IV. Prepare conditioner formulation
Part D
DESCRIPTION
Start heating to 75-80C
DEIONIZED WATER 39.67
L-ASPARTIC ACID 0.8
HYDROXYETHYL
CELLULOSE 0.5
XANTHAN GUM 0.05
DISODIUM EDTA 0.03
Complex Concentrate (*Part C) 50.1
Heat ff in separate container to
80C
CETYL ALCOHOL 5
STEARAMIDOPROPYL
DIMETHYLAMINE 2
GLYCERYL STEARATE 0.2
then add back to water phase and
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
157
mix at 75-80C
add;
Cocamidopropyl Betaine 1
cool down to 45C then add rest of
the ingredients
DMDM 0.2
FRAGRANCE 0.45
adjust with Citric Acid to around
pH=5
[0416] The "without complex" composition was prepared as above but with
water in
place of Part C. The control was Tresemme Anti-Breakage Conditioner.
[0417] Methodology: Use five, 1" wide bleached, damaged tresses (from Int'l
Hair
Importers), tag 10 fibers from each swatch with split ends and label
appropriately. Take
initial photos under microscope. Shampoo using standard procedure (1 mL on 1"
tress, lmin
contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temp at
rate of 2 gal/min).
Condition (1 mL on 1" tress, lmin contact time, 10 strokes on each side, 20
sec rinses, 35-
40C water temp at rate of 2 gal/min). Comb through wet hair once with wide-
tooth end
another time using narrow-end. Blow-dry at high heat until fully dry then comb
through
again twice, once with wide tooth end and another with narrow end. Count the
number of
fibers mended after the third and sixth treatments. Take final photos.
[0418] Calculations:
% mended = [(total number of tagged fibers before treatment - number of fibers
broken off
after treatment) - number of split ends after treatment] / (total number of
tagged
fibers before treatment - number of fibers broken off after treatment)
% breakage = 100 X (number of fibers broken off/ total number of tagged fibers
before
treatment)
[0419] Table 21 shows the results.
[0420] Table 21
% MENDING % BREAKAGE
after 3 after 6 after 3 after 6
treatments treatments treatments treatments
Composition 14A 36 48 Composition 14A 10 16
Control Conditioner 6 14 Control Conditioner 22 22
Without complex 30 18 Without complex 36 42
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
158
EXAMPLE 15
[0421] This example demonstrates split-end mending of exemplary
compositions of the
invention.
[0422] Compositions 15A-15D
Composition 15A 15B 15C 15D
PEC % 0.5 1 2 3
I. Prepare 4% active PVM/MA copolymer
Part A
DESCRIPTION
DEIONIZED WATER 98.9 96.6 84.73 89.5
10% NaOH 0.1 1.4 11.27 4.5
GANTREZ S-97 BF Polymer 1 2 4 6
Adjust pH to 6.95+/- 0.05 with NaOH if necessary
pH 7.21 7.06 7.12 6.90
II. Prepare 4% active Polyquat-28
Part B
DESCRIPTION
DEIONIZED WATER 95.12 90.25 80.49
70.74
CONDITIONEZE NT-20 4.88 9.76 19.51 29.27
pH 7.31
III. Combine A&B (Complex Concentrate) pH 7.21
Part C
DESCRIPTION
Part A 5 5 5 5
Part B 45 45 45 45
pH 7.31 7.79
IV. Prepare conditioner formulation
Part D
DESCRIPTION
Start heating to 75-80C
DEIONIZED WATER 40.22
E-ASPARTIC ACID 0.4
HYDROXYETHYL CELLULOSE 0.5
XANTHAN GUM 0.05
DISODIUM EDTA 0.03
Complex Concentrate (*Part C) 50.1
Heat ff in separate container to 80C
CETYL ALCOHOL 5
STEARAMIDOPROPYL DIEMTHYLAMINE 2
GLYCERYL STEARATE 0.2
then add back to water phase and mix for 15 minutes
at 75-80C, add;
COCO-BETAINE 1
cool down to 45C then add rest of the ingredients
DMDM HYDANTOIN _______________________________ 0.2
FRAGRANCE 0.3
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
159
adjust with Citric Acid to around pH=5
PH 7.8 7.98 8.07
% L-ASPARTIC ACID ADDITION ________________ 0.5 0.4 0.4 0.5
pH 5.50 5.10 4.83 4.85
[0423] Composition 15E
I. Prepare 4% active PVM/MA copolymer
Part A
DESCRIPTION
DEIONIZED WATER 84.73
10% NaOH 11.27
GANTREZ S-97 BF Polymer 4.00
Adjust pH to 6.95+/- 0.05 with NaOH if necessary
pH 7.2
II. Prepare 4% active Polyquat-28
Part B
DESCRIPTION
DEIONIZED WATER 80.49
CONDITIONEZE NT-20 19.51
III. Combine A&B (Complex Concentrate)
Part C
DESCRIPTION
Part A 5
Part B 45
IV. Prepare conditioner formulation
Part D
DESCRIPTION
Start heating to 75-80C
DEIONIZED WATER 39.62
L-ASPARTIC ACID 0.7
HYDROXYETHYL CELLULOSE 0.50
XANTHAN GUM 0.05
DISODIUM EDTA 0.03
Complex Concentrate (*Part C) 50.1
Heat ff in separate container to 80C
CETYL ALCOHOL 5
STEARAMIDOPROPYL DIMETHYLAMINE 2
GLYCERYL STEARATE 0.2
DIMETHICONE 0.3
then add back to water phase and mix for 15 minutes at 75-80C
add;
COCO-BETAINE 1
cool down to 45C then add rest of the ingredients
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
160
DMDM 01
FRAGRANCE 0.3
adjust with Citric Acid to around pH-5
pH 5.54
Vis (RVT-B, 10 rpm, 1 mm, 25C) 10,000
[0424] Test 1
[0425] From a 1" wide brown tress, tag fibers with split ends and take
initial photos.
Separately shampoo tresses with control shampoo (Alberto V05 Normal shampoo)
followed
by corresponding conditioner treatment. Repeat wash at least twice. Blow dry
tresses and
air-dry for 24 hours. Take final photos of each tagged fiber.
104261 The Test 1 results are shown in Figure 20 where the following
treatments are
shown:
Fiber 1 on Tress 1: Treated with water
Fiber 2 on Tress 2: Control Shampoo ¨ Control V05 Extra Body Conditioner
Fiber 3 on Tress 3: Control Shampoo ¨ Composition 15C
Fiber 4 on Tress 3: Control Shampoo ¨ Composition 15C
[0427] Test 2
[0428] From a 1" wide brown tress, tag five fibers with split ends and take
initial photos.
Shampoo tress with control shampoo followed by corresponding conditioner
treatment.
(Follow standard washing procedure: lmL, lmin contact time, 20 sec rinse, 35-
40 C water
temperature). Use one tress for Composition 15E and another with Composition
15C at rate
of 2 gal/min. Repeat wash at least twice. Blow dry tresses and air-dry for 24
hours. Take
final photos of each tagged fiber.
[0429] Not much conditioning benefit is provided by adding silicone but
mending of
split-ends is still apparent.
[0430] Test 3
[0431] Use three 1" wide brown tress, tag 10 fibers from each swatch with
split ends and
label appropriately. Shampoo using standard procedure (1 mL on 1" tress, lmin
contact time,
strokes on each side, 20 sec rinses, 35-40C water temperature at a rate of 2
gal/min).
Condition with Composition 15C (1 mL on 1" tress, lmin contact time, 10
strokes on each
side, 20 sec rinses, 35-40C water temperature at a rate of 2 gal/min). Comb
through wet hair
once with the wide-tooth end and another time using the narrow-end. Blow-dry
then comb
through again twice, once with the wide tooth end and another with the narrow
end. Repeat
above steps as needed. Count the number of fibers mended after each treatment.
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
161
[0432] The results are shown in Table 22.
[0433] Table 22
No. of Treatments 1 2 3 4 5 6 7 8 9 10 I
Percent Mended 17% 26% 57% 57% 57% 57% 61% 61%
61% 61%
[0434] Test 4
[0435] Use five, 1" wide bleached, damaged tresses (from Intl Hair
Importers), tag 10
fibers from each swatch with split ends and label appropriately. Take initial
photos under
microscope. Shampoo using standard procedure (1 mL on 1" tress, lmin contact
time, 10
strokes on each side, 20 sec rinses, 35-40C water temp at rate of 2 gal/min).
Condition (1 mL
on 1" tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C
water temp at
rate of 2 gal/min). Comb through wet hair once with wide-tooth end another
time using
narrow-end. Blow-dry at high heat until fully dry then comb through again
twice, once with
wide tooth end and another with narrow end. Count the number of fibers mended
after the
third, sixth and tenth treatment. Take final photos.
[0436] Calculations
% mended = 100* number of split ends after treatment /
initial number of tagged split end fibers
% breakage = 100* number of fibers broken off! initial number of tagged split
end
fibers before treatment
[0437] The results are in Table 23.
[0438] Table 23
Composition 15C Control 1
No. 3 6 10 3 6 10
Treatments
Ave Total 42 52 38 8 10 8
% Mending
Ave Total 22 28 40 44 52 54
% Breakage
[0439] Composition 15C provides excellent conditioning on bleached tresses
with easy
wet combing.
[0440] Test 5
[0441] Use two, 1" wide bleached, damaged tresses per treatment. Tag 10
fibers from
each swatch with split ends and label appropriately. Take initial photos under
microscope.
Separately shampoo tresses using standard procedure (1 mL on 1" tress, lmin
contact time,
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
162
strokes on each side, 20 see rinses, 35-40C water temperature at a rate of 2
gal/min).
Separately condition tresses with Composition 15B, 15C, or 15D (1 mL on 1"
tress, lmin
contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temperature
at rate of 2
gal/min). Comb through wet hair once with the wide-tooth end and another time
using the
narrow-end. Blow-dry at high heat until thlly dry, then comb through again
twice, once with
the wide tooth end and another with the narrow end. Count the number of fibers
mended after
the appropriate number of treatments. Take final photos.
[0442] The results are shown in Table 24.
[0443] Table 24
Composition 15B 15C 15D
Treatments 3 6 3 6 3 6
Ave Total %
Mending 55 45 42 52 50 30
Ave Total %
Breakage 10 15 22 28 15 25
[0444] Test 6
[0445] Use three 1" wide brown tresses, tag 10 fibers from each swatch with
split ends
and label appropriately. Separately shampoo tresses using standard procedure
(1 mL on 1"
tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water
temperature at a
rate of 2 gal/min). Separately condition tresses using Control 1 (Nexxus
commercial
formulation), Control 2, Composition 15A, 15B, 15C, or 15D (1 mL on 1" tress,
lmin contact
time, 10 strokes on each side, 20 sec rinses, 35-40C water temp at rate of 2
gal/min). Comb
through wet hair once with the wide-tooth end another time using the narrow-
end. Blow-dry
then comb through again twice, once with the wide tooth end and another with
the narrow
end. Repeat above steps as needed. Count the number of fibers mended after
each treatment.
Count the number of broken fibers after each treatment.
[0446] Control 2 composition
DESCRIPTION
Start heating to 75-80C
DEIONIZED WATER 89.77
L-ASPART1C ACID 0.8
HYDROXYETHYL
CELLULOSE 0.5
XANTHAN GUM _____________________________________ 0.05
DISODIUM EDTA 0.03
Heat ff in separate container to
80C
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
163
CETYL ALCOHOL 5
STEARAMIDOPROPYL
DIMETHYLAMINE 2
GLYCERYL STEARATE 0.2
then add back to water phase and
mix for 15 minutes at 75-80C
add:
Mackam CB35 (Coco Betaine) 1
cool down to 45C then add rest
of the ingredients
DMDM 0.2
FRAGRANCE 0.45
adjust with Citric Acid to around
pH=5
Specifications
pH 4.35
Vis (RVT-B, 10 rpm, 1 mm,
25C) 4,800
[0447] The results are shown in Tables 25 and 26.
[0448] Table 25
% Breakage
3 6
treatments treatments
Control 1 42 52
Control 2 (0% PEC) 30 50
__ Composition 15A (0.5% PEC) 20 40
Composition 15B (1% PEC) 10 15
Composition 15C (2% PEC) 22 28
Composition 15D (3% PEC) 15 25
[0449] Table 26
% Mending
3 6
treatments treatments
Control 1 8 10
Control 2 (0% PEC) 25 30
Composition 15A (0.5% PEC) 25 25
Composition 15B (1% PEC) 55 45
Composition 15C (2% PEC) 42 52
Composition 15D (3% PEC) 50 30
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
164
EXAMPLE 16
[0450] This example demonstrates split-end mending of exemplary
compositions of the
present invention.
[0451] Composition 16A
Item No. Material Description Wt%
1 Deionized water 7.75
2 PVM/MA Copolymer (Gantrez S-97 BF) 0.1
3 Sodium Hydroxide (20% active) 0.125
4 Polyquarternium-28 (Conditioneze NT-20) 4.5
Deionized water 77.2248
6 HEC 0.3
7 Aqu D 4272 N-Hance SP100 (polyacrylamide) 0.2
8 Disodium EDTA 0.05
9 L-Aspartic Acid 0.35
Stearamidopropyl Dimethylamine 1
11 Cetyl Alcohol 1.5
12 Glycerin 0.5
13 Caprylic/Capric Triglycerides 1
14 Distearoylethyl Dimonium Chloride; Cetearyl Alcohol (Varisoft EQ
65) 0.5
Amodimethicone (ADM 1100) 1.3
16 Salcare SC-96 1
17 D6, D5, Dimethicone 2
18 Fragrance 0.4
19 DMDM Hydantoin 0.2
Hydrolyzed Keratin 0.0001
21 Vitamin Blend
0.0001
[0452] Mixing Procedure:
1. Premix ¨ Added item #1-2 and mixed until hydrated
2. Used item #3 to adjust pH to 6.9-7, then heated 50-55C
3. Slowly added item #4 under very vigorous mixing, mix for ¨10min
4. In main vessel, added item #5 and began heating to 80-85C
5. Added items #6-7. When batch reached 80C, added #8-10 and mixed for 30 min.
6. Began cooling batch, when below 45C, added premix from step 1-3 and
remaining
ingredients
[0453] Target Specifications:
Appearance ¨ opaque, viscous liquid
Odor ¨ to match standard
pH ¨ 4.5-5.5
Viscosity ¨ 10,000-15,000 cps RVT-B 10 rpm, 60 sec
CA 02812991 2013-03-19
WO 2012/054243
PCT/US2011/055370
165
[0454] Comparative Composition 16B
Item No, Material Description Wt%
1 Deionized water
77.2248
2 HEC 0.3
3 Aqu D 4272 N-Hance SP100 (Acrylamidopropyltrimonium
Chloride/Acrylamide Copolymer) 0
4 Disodium EDTA 0.05
L-Aspartic Acid 0.35
6 Stearamidopropyl Dimethylamine 1
7 Cetyl Alcohol 1.5
8 Glycerin 0.5
9 Caprylic/Capric Triglycerides 1
Distearoylethyl Dimonium Chloride; Cetearyl Alcohol (Varisoft EQ
65) 0.5
11 Amodimethicone (ADM 1100) 1.3
12 PEC Premix 12.5
13 Salcare SC-96 (Polyquartemium-37, Propylene Glycol
Dicaprylate/Dicaprate, PPG-1 Trideceth-6) 1
14 D6, D5, Dimethicone 2
Fragrance 0.4
16 Vitamin Blend
0.0001
17 Hydrolyzed Keratin
0.0001
18 DMDM Hydantoin 0.175
[0455] Mixing Procedures:
1. In main vessel, added item #1-2 and began heating to 80-85C
2. Added item #3 when no lumps present
3. When 1-3 had no lumps, continued heating to 80-85C
4. When batch reached 80-85C, added items #4-17 and mixed for 30 minutes
5. Began cooling batch, when below 45C, added 11-18
[0456] Target Specifications:
Appearance ¨ opaque, viscous liquid
Odor ¨ to match standard
pH ¨ 4.5-5.5
Viscosity¨ 10,000-15,000 cps RVT-8 10 rpm, 60 sec
[0457] Composition 16A had a pH of 4.92 and a viscosity of 10,800 cps.
Composition
16B had a pH of 4.95 and a viscosity of 7,200 cps.
[0458] Composition 16A had much better wet and dry combing when compared
to
control.
[0459]
Double bleached hair tresses were flogged with addition of blow drying to
create
166
split ends. Ten splits were tagged in each of four 1 'A inch wide tresses. Two
tresses were
then washed with Alberto V05 Normal shampoo and conditioned with Composition
16A.
Two tresses were washed with Alberto V05 Normal shampoo and conditioned with
Comparative Composition 16B.
10460] Composition 16A gave 90% mending of split ends, and Comparative
Composition
16B gave 63% mending of split ends. The addition of N-Hance SP-100 to formula
improves
mending ability of the final formulation.
104611 The use of the terms "a" and "an" and "the" and similar referents
in the context of
describing the invention (especially in the context of the following claims)
are to be
construed to cover both the singular and the plural, unless otherwise
indicated herein or
clearly contradicted by context. The terms "comprising," "having,"
"including," and
"containing" are to be construed as open-ended terms (i.e., meaning
"including, but not
limited to,") unless otherwise noted. Recitation of ranges of values herein
are merely
intended to serve as a shorthand method of referring individually to each
separate value
falling within the range, unless otherwise indicated herein, and each separate
value is
incorporated into the specification as if it were individually recited herein.
All methods
described herein can be performed in any suitable order unless otherwise
indicated herein or
otherwise clearly contradicted by context. The use of any and all examples, or
exemplary
language (e.g., "such as") provided herein, is intended merely to better
illuminate the
invention and does not pose a limitation on the scope of the invention unless
otherwise
claimed. No language in the specification should be construed as indicating
any non-claimed
element as essential to the practice of the invention.
[0462] Preferred embodiments of this invention are described herein,
including the best
mode known to the inventors for carrying out the invention. Variations of
those preferred
embodiments may become apparent to those of ordinary skill in the art upon
reading the
foregoing description. The inventors expect skilled artisans to employ such
variations as
appropriate, and the inventors intend for the invention to be practiced
otherwise than as
specifically described herein. Accordingly, this invention includes all
modifications and
CA 2812991 2017-11-27
CA 02812991 2013-03-19
WO 2012/054243 PCT/US2011/055370
167
equivalents of the subject matter recited in the claims appended hereto as
permitted by
applicable law. Moreover, any combination of the above-described elements in
all possible
variations thereof is encompassed by the invention unless otherwise indicated
herein or
otherwise clearly contradicted by context.
