Note: Descriptions are shown in the official language in which they were submitted.
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SOLUBLE SOLID HAIR COLORING ARTICLE
FIELD OF THE INVENTION
The present invention relates to a soluble solid hair coloring article
utilizing zwitterionic
direct dyes in conjunction with, and/or incorporated into, a soluble
substrate.
BACKGROUND OF THE INVENTION
The majority of personal care products in the market today are sold as liquid
products.
While widely used, liquid products have disadvantages in terms of packaging,
storage,
transportation, and convenience of use. Liquid personal care products
typically are sold in bottles
which add significant cost as well as packaging waste, much of which ends up
in land-fills.
Solid hair dyes are known, but generally discussed in terms of powdered
oxidative dyes that
are mixed with a developer solution before application onto the hair. Such
products still require a
traditional kit of dye and developer compositions.
Solid personal care products in the form of dissolvable foams are also known.
See WO
2010/077650. US 7,225,920 B2 discusses a bleaching composition sealed into a
water soluble
pouch that is then dissolved in water. EP 1745769 B1 discusses a liquid that
is foamed and then
dries to form a hair coloring product. US 5,879,414 A discusses a hydrous
solid wash resistant hair
colorant stick composition. US 2003/0033678 discusses a shaped body useful for
forming cosmetic
preparation such as hair coloring preparations. US 5,769,901 discusses a
powdered hair dye
including an oxidative dye component, an oxidizing component and a thickening
component.
There still exists a need to provide a soluble solid hair coloring product
that is stable and
delivers desired hair color results. It has surprisingly been found that the
selection of cationic
surfactant in the porous solid must be compatible with the desired direct dyes
in order to provide a
hair colorant. Many direct dyes are essentially salts; it is not obvious as to
how such direct dyes will
affect formulated product and stability of the formulated product. A balance
must be found between
delivering the desired color results and producing a stable product that is
robust in view of the salt
levels present.
It is an object of the present invention to provide a soluble hair coloring
product from an
open-celled porous solid that can be conveniently and quickly dissolved in the
palm of the consumer
to reconstitute a liquid product for ease of application to hair while
providing sufficient topical
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delivery of active agents for partial or whole head hair applications with
similar performance as
today's liquid products. It is a further object of the present invention to
provide such a product that
can be produced by physical aeration followed by subsequent drying. It is an
even further object of
the present invention to provide such a product with desirable softness and
flexibility.
SUMMARY OF THE INVENTION
The present invention relates to a soluble solid hair coloring article
comprising: from about
0.4 to about 2.0 grams of zwitterionic direct dye; one or more soluble porous
solids comprising:
from about 10% to about 50% polymeric structurant; from about 1% to about 30%
plasticizer; and
from about 2% to about 75% nonionic surfactant, cationic surfactant, or
mixtures thereof; wherein
the density of the one or more soluble porous solids is from about 0.03 g/cm3
to about 0.15 g/cm3.
The present invention further relates to a method of coloring hair comprising
the steps of:
exposing a soluble solid hair coloring article comprising zwitterionic direct
dye and one or more
soluble porous solids to a solvent, such that the soluble solid hair coloring
article dissolves to form a
hair coloring solution, wherein the ratio of cationic direct dye to hair is
from 2:1 to 5:1; and applying
the hair coloring solution to hair.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 is a micro computed tomography system image of a soluble porous solid
having a density of
0.12 grams/cm3 (with 30 seconds mixing);
Fig. 2 is a micro computed tomography system image of a soluble porous solid
having a density of
0.08 grams/cm3 (with 60 seconds of mixing);
Fig. 3 is a micro computed tomography system image of a soluble porous solid
having a density of
0.07 grams/cm3 (with 90 seconds of mixing);
Fig. 4 is a micro computed tomography system image of a comparative example in
Table 8 and 9
having a density of 0.21 grams/cm3 with 30 seconds mixing;
Fig. 5 is a micro computed tomography system image of a comparative example in
Table 8 and 9
having a density of 0.16 grams/cm3 with 60 seconds mixing.
DETAILED DESCRIPTION OF THE INVENTION
In all embodiments of the present invention, all percentages are by weight of
the total
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composition, unless specifically stated otherwise. All ratios are weight
ratios, unless specifically
stated otherwise. All ranges are inclusive and combinable. The number of
significant digits
conveys neither a limitation on the indicated amounts nor on the accuracy of
the measurements. All
numerical amounts are understood to be modified by the word "about" unless
otherwise specifically
indicated. Unless otherwise indicated, all measurements are understood to be
made at 25 C and at
ambient conditions, where "ambient conditions" means conditions under about
one atmosphere of
pressure and at about 50% relative humidity. All such weights as they pertain
to listed ingredients
are based on the active level and do not include carriers or by-products that
may be included in
commercially available materials, unless otherwise specified.
Definitions
The term "porous solid" as used herein, unless otherwise specified, refers to
a solid,
interconnected, polymer-containing matrix that defines a network of spaces or
cells that contain a
gas, typically a gas such as air (open-celled structure), where the network of
spaces or cells is
substantially interconnected.
It is believed that such porous solids comprising predominantly open-cells
enable rapid
water flux inside the structure, exposing a multiplicity of additional solid
surface area for vastly
increased dissolution rates. This is in contrast to substrates comprised of
predominantly closed
cells, whereby the vast majority of the interior cellular surfaces are not
rapidly exposed to the water
upon wetting and with dissolution progressing mainly through surface erosion,
which results in
slower dissolution.
It has been found that a soluble solid hair coloring article can be prepared
that can be
conveniently and quickly dissolved by a consumer in their hand to form a
liquid hair coloring
product for ease of application to hair while providing sufficient topical
delivery of direct dye for
partial hair applications (such as root touch up application or
highlighting/low-lighting applications)
or whole head hair applications with similar performance as conventional
liquid hair colorant
products. It has also been found that the soluble solid hair coloring articles
can be produced in an
economical manner by physical aeration followed by subsequent drying.
The desired balance between forming a predominantly interconnected, open-
celled structure
and direct dye deposition properties after reconstitution has been achieved by
employing specifically
selected nonionic surfactant, cationic surfactant, and combinations of
cationic surfactants and
nonionic surfactants that enable foam generation under the high energy
processing conditions
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employed during aeration to produce the structure of the soluble porous solid.
The selection of surfactant for use in the soluble solid hair coloring article
is also impacted
by the presence of materials known as direct dyes, which often carry a charge
that may interact
adversely to surfactants carrying an opposite charge (e.g., cationic or basic
direct dyes with an
anionic surfactant).
Soluble Solid Hair Coloring Article
Direct Dyes
The soluble solid hair coloring article comprises at least one direct dye
suitable for
delivering shade modification or highlights. Depending upon the desired
resulting hair color,
multiple direct dyes may be combined to achieve the desired resulting hair
color.
The direct dye may be contained by the porous solid in the sense that the
porous solid forms
a holding container for the direct dye. Suitable holding container structures
include an envelope,
pouch or sandwich structure. The "envelope" and "pouch" structures may be from
a single soluble
porous solid that is folded to receive the direct dye and any other desired
components. As used
herein, "sandwich" structure refers to utilizing two soluble porous solids
that at least partially
overlap such that where the two soluble porous solids are contiguous, the
direct dye and any other
desired components are located between the two soluble porous solids.
Alternatively, the direct dye
may be incorporated as part of the processing mixture used to form the soluble
porous solid.
The amount of direct dye should be selected to give the desired amount
delivered to the hair
to be dyed. As used herein "hair" encompasses keratin fibers such as human
hair, wigs, extensions,
fur and the like. If a whole head hair application is desired, then amounts of
the direct dye should be
selected to give the delivery of 1.0 to 1.5% by weight of the hair of direct
dye to the whole head of
hair, or approximately 10 to 15 mg of direct dye per gram of hair. The amount
of hair on a whole
head may be from 5 g to 200 g and depends upon the length of the hair. The
average amount of
hair on a whole head may be from about 40 g to about 60 g. If a partial head
hair application, such
as highlighting or low lighting, is desired, then the amounts of the direct
dye should be selected to
reflect the lower weight of hair to which the direct dye will be applied.
In one embodiment, the ratio of direct dye to hair is from 3:1 to 5:1, such as
4:1. The
amount of direct dye in the soluble hair coloring article may be from about
0.4 to about 2.0 grams.
The direct dyes may be zwitterionic in nature, with or without nonionic direct
dyes, with or
without cationic direct dyes or anionic direct dyes.
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Colors resulting from the direct dyes may be influenced or controlled by the
selection of and
mixing of individual dyes to achieve the targeted end color. Direct dyes may
be selected from red,
blue and yellow color categories. The mixing of these direct dyes may be used
to achieve the hair
color desired. One example is to mix a red direct dye, a blue direct dye and a
yellow direct dye in a
5 1:1:1 mass ratio.
The following is a list of exemplary dyes:
Zwitterionic direct dyes
Name Color CAS number
4-(2-44-(dimethylamino)phenyl)diazeny1)-1-methy1-
1H-imidazol-3-ium-3-y1)butane-1-sulfonate red 904316-50-3
4-(4-((2-methy1-2-phenylhydrazono)methyl)pyridin-1-
ium-1-y1)butane-1-sulfonate yellow 953082-11-6
4-(2-44-(dimethylamino)phenyl)diazenyl)thiazol-3-
ium-3-yl)butane-l-sulfonate blue 904316-43-4
Thiazolium, 2-[2-[4-(dimethylamino)phenyl]diazeny1]-
4-methy1-3-(4-sulfobuty1)-, inner salt blue 904316-44-5
Thiazolium, 2-[2-[4-(dimethylamino)phenyl]diazeny1]-
5-methy1-3-(4-sulfobuty1)-, inner salt blue 904316-45-6
Thiazolium, 2-[2-[4-(dimethylamino)phenyl]diazeny1]-
4,5-dimethy1-3-(4-sulfobuty1)-, inner salt blue 904316-46-7
Thiazolium, 2-[2-[4-
[ethyl(phenylmethyl)amino]phenyl]diazeny1]-3-(4-
sulfobuty1)-, inner salt blue 904316-47-8
Thiazolium, 3-(4-sulfobuty1)-2-[2-(2,3,6,7-tetrahydro-
1H,5H-benzo[ij]quinolizin-9-yl)diazenyl]-, inner salt blue 904316-48-
9
Thiazolium, 2-[2-[4-(dimethylamino)phenyl]diazeny1]-
3-(3-sulfopropy1)-, inner salt blue 904316-49-0
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Pyridinium, 3-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-12-7
Pyridinium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-13-8
Pyridinium, 4-[[2-(4-
methoxyphenyl)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-14-9
Pyridinium, 4-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-15-0
Thiazolium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy1]-3-(4-sulfobuty1)-, inner
salt blue 953082-16-1
Pyridinium, 4-[[2-(3-methy1-2(3H)-
benzothiazolylidene)hydrazinylidene]methy1]-1-(4-
sulfobutyl)-, inner salt red 953082-17-2
Pyridinium, 3-[[2-(3-methy1-2(3H)-
benzothiazolylidene)hydrazinylidene]methy1]-1-(4-
sulfobutyl)-, inner salt red 953082-18-3
Pyridinium, 4-[[2-(3,4-dimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt red 953082-19-4
Pyridinium, 3-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-22-9
Pyridinium, 2-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-23-0
Pyridinium, 4-[[2-(2-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-24-1
Pyridinium, 3-[[2-(2-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-25-2
Pyridinium, 2-[[2-(2-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-26-3
Pyridinium, 4-[[2-(4-hydroxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-27-4
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Pyridinium, 3-[[2-(4-hydroxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-28-5
Pyridinium, 2-[[2-(4-hydroxypheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-29-6
Pyridinium, 4-[[2-methy1-2-(4-
methylphenyl)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-30-9
Pyridinium, 3-[[2-methy1-2-(4-
methylphenyl)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-31-0
Pyridinium, 2-[[2-methy1-2-(4-
methylphenyl)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-32-1
Pyridinium, 4-[[2-(4-chloropheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-33-2
Pyridinium, 3-[[2-(4-chloropheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-34-3
Pyridinium, 2-[[2-(4-chloropheny1)-2-
methylhydrazinylidene]methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-35-4
Pyridinium, 4-[[2-methy1-2-(4-
nitrophenyl)hydrazinylidene]methy1]-1-(4-sulfobuty1)-,
inner salt yellow 953082-36-5
Pyridinium, 3-[[2-methy1-2-(4-
nitrophenyl)hydrazinylidene]methy1]-1-(4-sulfobuty1)-,
inner salt yellow 953082-37-6
Pyridinium, 2-[[2-methy1-2-(4-
nitrophenyl)hydrazinylidene]methy1]-1-(4-sulfobuty1)-,
inner salt yellow 953082-38-7
Pyridinium, 4-[(2-phenylhydrazinylidene)methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-39-8
Pyridinium, 3-[(2-phenylhydrazinylidene)methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-40-1
Pyridinium, 2-[(2-phenylhydrazinylidene)methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-41-2
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Pyridinium, 3-[[2-(4-
methoxyphenyl)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-42-3
Pyridinium, 2-[[2-(4-
methoxyphenyl)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-43-4
Pyridinium, 4-[1-(2-methy1-2-
phenylhydrazinylidene)ethy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-44-5
Pyridinium, 3-[1-(2-methy1-2-
phenylhydrazinylidene)ethy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-45-6
Pyridinium, 2-[1-(2-methy1-2-
phenylhydrazinylidene)ethy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-46-7
Pyridinium, 4-[1-(2-phenylhydrazinylidene)ethy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-47-8
Pyridinium, 3-[1-(2-phenylhydrazinylidene)ethy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-48-9
Pyridinium, 2-[1-(2-phenylhydrazinylidene)ethy1]-1-(4-
sulfobuty1)-, inner salt yellow 953082-49-0
1H-Imidazolium, 1-methy1-2-[(2-methyl-2-
phenylhydrazinylidene)methy1]-3-(4-sulfobuty1)-, inner
salt yellow 953082-50-3
Oxazolium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy1]-3-(4-sulfobuty1)-, inner
salt yellow 953082-51-4
4H-1,2,4-Triazolium, 4-methy1-5-[(2-methy1-2-
phenylhydrazinylidene)methyl]-1-(4-sulfobuty1)-, inner
salt yellow 953082-52-5
Quinolinium, 4-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-53-6
Quinolinium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(4-sulfobuty1)-, inner
salt yellow 953082-54-7
Pyridinium, 4-[[(2,3-dihydro-1H-indo1-1-
yl)imino]methyl]-1-(4-sulfobutyl)-, inner salt yellow 953082-55-8
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Pyridinium, 4-[[(2,3-dihydro-2,2,3,3-tetramethy1-1H-
indo1-1-y1)imino]methyl]-1-(4-sulfobutyl)-, inner salt yellow 953082-56-
9
3H-Indolium, 3,3-dimethy1-2-[(2-methy1-2-
phenylhydrazinylidene)methyl]-1-(4-sulfobuty1)-, inner
salt yellow 953082-58-1
3H-Indolium, 2-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-3,3-dimethy1-1-(4-
sulfobuty1)-, inner salt yellow 953082-59-2
Pyrimidinium, 2,3-dihydro-3-methy1-6-[(2-methy1-2-
phenylhydrazinylidene)methyl]-2-oxo-1-(4-sulfobuty1)-
, inner salt yellow 953082-61-6
1H-Indazolium, 1-methy1-7-[(2-methyl-2-
phenylhydrazinylidene)methy1]-2-(4-sulfobuty1)-, inner
salt yellow 953082-62-7
Pyridinium, 4-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-64-9
Pyridinium, 3-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-65-0
Pyridinium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-66-1
Pyridinium, 4-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-68-3
Pyridinium, 3-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-70-7
Pyridinium, 2-[[2-(4-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-71-8
Pyridinium, 4-[[2-(2-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-72-9
Pyridinium, 3-[[2-(2-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-74-1
Pyridinium, 2-[[2-(2-methoxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-76-3
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Pyridinium, 4-[[2-(4-hydroxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-77-4
Pyridinium, 3-[[2-(4-hydroxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-78-5
Pyridinium, 2-[[2-(4-hydroxypheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-80-9
Pyridinium, 4-[[2-methy1-2-(4-
methylphenyl)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953082-82-1
Pyridinium, 3-[[2-methy1-2-(4-
methylphenyl)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953082-83-2
Pyridinium, 2-[[2-methy1-2-(4-
methylphenyl)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953082-84-3
Pyridinium, 4-[[2-(4-chloropheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-86-5
Pyridinium, 3-[[2-(4-chloropheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-88-7
Pyridinium, 2-[[2-(4-chloropheny1)-2-
methylhydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953082-89-8
Pyridinium, 4-[[2-methy1-2-(4-
nitrophenyl)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953082-90-1
Pyridinium, 3-[[2-methy1-2-(4-
nitrophenyl)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953082-91-2
Pyridinium, 2-[[2-methy1-2-(4-
nitrophenyl)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953082-92-3
Pyridinium, 4-[1-(2-methy1-2-
phenylhydrazinylidene)ethy1]-1-(3-sulfopropy1)-, inner
salt yellow 953082-93-4
Pyridinium, 3-[1-(2-methy1-2-
phenylhydrazinylidene)ethy1]-1-(3-sulfopropy1)-, inner
salt yellow 953082-94-5
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Pyridinium, 2-[1-(2-methy1-2-
phenylhydrazinylidene)ethy11-1-(3-sulfopropy1)-, inner
salt yellow 953082-95-6
Pyridinium, 4-[1-(2-phenylhydrazinylidene)ethy11-1-(3-
sulfopropy1)-, inner salt yellow 953082-96-7
Pyridinium, 3-[1-(2-phenylhydrazinylidene)ethy11-1-(3-
sulfopropy1)-, inner salt yellow 953082-97-8
Pyridinium, 2-[1-(2-phenylhydrazinylidene)ethy11-1-(3-
sulfopropy1)-, inner salt yellow 953082-98-9
Thiazolium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy1]-3-(3-sulfopropy1)-,
inner salt blue 953082-99-0
1H-Imidazolium, 1-methy1-2-[(2-methyl-2-
phenylhydrazinylidene)methy1]-3-(3-sulfopropy1)-,
inner salt yellow 953083-00-6
Oxazolium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy11-3-(3-sulfopropy1)-,
inner salt yellow 953083-01-7
4H-1,2,4-Triazolium, 4-methy1-5-[(2-methy1-2-
phenylhydrazinylidene)methyll-1-(3-sulfopropyl)-,
inner salt yellow 953083-02-8
Quinolinium, 4-[(2-methy1-2-
phenylhydrazinylidene)methy11-1-(3-sulfopropy1)-,
inner salt yellow 953083-03-9
Quinolinium, 2-[(2-methy1-2-
phenylhydrazinylidene)methy11-1-(3-sulfopropy1)-,
inner salt Yellow 953083-04-0
Pyridinium, 4-[[(2,3-dihydro-1H-indo1-1-
yl)iminolmethyll-1-(3-sulfopropyl)-, inner salt Yellow 953083-05-1
Pyridinium, 4-[[(2,3-dihydro-2,2,3,3-tetramethy1-1H-
indo1-1-y1)iminolmethyll-1-(3-sulfopropyl)-, inner salt yellow 953083-06-2
3H-Indolium, 3,3-dimethy1-2-[(2-methy1-2-
phenylhydrazinylidene)methyll-1-(3-sulfopropyl)-,
inner salt yellow 953083-07-3
3H-Indolium, 2-[[2-(4-methoxypheny1)-2-
methylhydrazinylidenelmethy1]-3,3-dimethy1-1-(3-
sulfopropyl)-, inner salt yellow 953083-08-4
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1H-Indazolium, 1-methy1-7-[(2-methyl-2-
phenylhydrazinylidene)methy1]-2-(3-sulfopropy1)-,
inner salt yellow 953083-09-5
Pyridinium, 3-[[2-(3,4-dimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-1-(4-
sulfobuty1)-, inner salt yellow 953083-10-8
Pyridinium, 1-(4-sulfobuty1)-4-[[2-(3,4,5-trimethyl-
2(3H)-thiazolylidene)hydrazinylidene]methy1]-, inner
salt yellow 953083-11-9
Pyridinium, 1-(4-sulfobuty1)-3-[[2-(3,4,5-trimethyl-
2(3H)-thiazolylidene)hydrazinylidene]methy1]-, inner
salt yellow 953083-12-0
1H-Imidazolium, 1-methy1-2-[[2-(3-methyl-2(3H)-
benzothiazolylidene)hydrazinylidene]methy1]-3-(4-
sulfobuty1)-, inner salt yellow 953083-13-1
1H-Imidazolium, 2-[[2-(3,4-dimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-1-methy1-3-(4-
sulfobuty1)-, inner salt yellow 953083-14-2
1H-Imidazolium, 1-methy1-3-(4-sulfobuty1)-2-[[2-
(3,4,5-trimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-, inner salt yellow 953083-15-3
Pyridinium, 4-[[2-[bis[4-
(dimethylamino)phenyl]methylene]hydrazinylidene]me
thy1]-1-(4-sulfobuty1)-, inner salt yellow 953083-16-4
Pyridinium, 3-[[2-[bis[4-
(dimethylamino)phenyl]methylene]hydrazinylidene]me
thy1]-1-(4-sulfobuty1)-, inner salt yellow 953083-17-5
Pyridinium, 4-[[2-(9H-fluoren-9-
ylidene)hydrazinylidene]methy1]-1-(4-sulfobuty1)-,
inner salt yellow 953083-18-6
Quinolinium, 4-[[2-[bis[4-
(dimethylamino)phenyl]methylene]hydrazinylidene]me
thy1]-1-(4-sulfobuty1)-, inner salt yellow 953083-19-7
Pyridinium, 4-[[2-(3-methy1-2(3H)-
benzothiazolylidene)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953083-20-0
Pyridinium, 3-[[2-(3-methy1-2(3H)-
benzothiazolylidene)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953083-21-1
Pyridinium, 4-[[2-(3,4-dimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953083-22-2
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Pyridinium, 3-[[2-(3,4-dimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-1-(3-
sulfopropy1)-, inner salt yellow 953083-23-3
Pyridinium, 1-(3-sulfopropy1)-4-[[2-(3,4,5-trimethyl-
2(3H)-thiazolylidene)hydrazinylidene]methy1]-, inner
salt yellow 953083-24-4
Pyridinium, 1-(3-sulfopropy1)-3-[[2-(3,4,5-trimethyl-
2(3H)-thiazolylidene)hydrazinylidene]methy1]-, inner
salt yellow 953083-25-5
1H-Imidazolium, 1-methy1-2-[[2-(3-methyl-2(3H)-
benzothiazolylidene)hydrazinylidene]methy1]-3-(3-
sulfopropy1)-, inner salt yellow 953083-26-6
1H-Imidazolium, 2-[[2-(3,4-dimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-1-methy1-3-(3-
sulfopropy1)-, inner salt yellow 953083-27-7
1H-Imidazolium, 1-methy1-3-(3-sulfopropy1)-2-[[2-
(3,4,5-trimethy1-2(3H)-
thiazolylidene)hydrazinylidene]methy1]-, inner salt yellow 953083-28-8
Pyridinium, 4-[[2-[bis[4-
(dimethylamino)phenyl]methylene]hydrazinyl]methy1]-
1-(3-sulfopropy1)-, inner salt yellow 953083-29-9
Pyridinium, 3-[[2-[bis[4-
(dimethylamino)phenyl]methylene]hydrazinyl]methy1]-
1-(3-sulfopropy1)-, inner salt yellow 953083-30-2
Pyridinium, 4-[[2-(9H-fluoren-9-
ylidene)hydrazinylidene]methy1]-1-(3-sulfopropy1)-,
inner salt yellow 953083-31-3
Quinolinium, 4-[[2-[bis[4-
(dimethylamino)phenyl]methylene]hydrazinyl]methy1]-
1-(3-sulfopropy1)-, inner salt yellow 953083-32-4
Preferred zwitterionic direct dyes:
4-(2-44-(dimethylamino)phenyl)diazeny1)-1-methy1-
1H-imidazol-3-ium-3-y1)butane-1-sulfonate red 904316-50-3
4-(4-((2-methy1-2-phenylhydrazono)methyl)pyridin-1-
ium-1-y1)butane-1-sulfonate yellow 953082-11-6
4-(2-44-(dimethylamino)phenyl)diazenyl)thiazol-3-
ium-3-yl)butane-l-sulfonate blue 904316-43-4
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Nonionic direct dyes:
Disperse Red 17 red 3179-89-3
Picramic Acid red 96-91-3
HC Red No. 13 red 94158-13-1
HC Red No. 7 red 24905-87-1
HC Red No. 1 red 2784-89-6
2-chloro-5-nitro-N-hydroxyethyl-p-phenylenediamine red 50610-28-1
HC Red No. 3 red 2871-01-4
4-amino-3-nitrophenol red 6 10-8 1-1
3-nitro-p-hydroxyethylaminophenol red 65235-31-6
2-amino-3-nitrophenol red 603-85-0
HC Red No. 10 red 95576-89-9
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HC Red No. 11 red 95576-92-4
2-hydroxyethyl picramic acid red 99610-72-7
2-chloro-6-ethylamino-4-nitrophenol red 131657-78-8
6-nitro-2,5-pyridinediamine red 69825-83-8
2-amino-6-chloro-4-nitrophenol red 6358-09-4
4-hydroxypropylamino-3-nitrophenol red 92952-81-3
N-(2-nitro-4-aminopheny1)-allylamine red 160219-76-1
Disperse Red 15 red 116-85-8
HC Red No. 9 red 56330-88-2
Cochenille (a.k.a. carminic acid, natural red 4,
Cochineal Red PWD) red 1260-17-9
HC Red No. 14 red 99788-75-7
orange-
4-nitro-o-phenylenediamine red 99-56-9
orange-
2-nitro-p-phenylenediamine red 5307-14-2
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2-hydroxy-1,4-naphthoquinone (a.k.a. Henna, reddish
Lawsone) brown 83-72-7
reddish
Henna Red (a.k.a. Henna) brown 253167-73-6
Disperse Violet 4 violet 1220-94-6
1,4-bis-(2'-hydroxyethylamino)-2-nitrobenzene violet 84041-77-0
HC Violet No. 1 violet 82576-75-8
Disperse Violet 1 violet 128-95-0
HC Violet No. 2 violet 104226-19-9
HC Yellow No. 5 yellow 56932-44-6
HC Yellow No. 4 yellow 59820-43-8
HC Yellow No. 2 yellow 4926-55-0
3-methylamino-4-nitrophenoxyethanol yellow 59820-63-2
6-nitro-o-toluidine yellow 570-24-1
2-nitro-5-glycerylmethylaniline yellow 80062-31-3
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HC Yellow No. 11 yellow 73388-54-2
HC Yellow No. 9 yellow 86419-69-4
4-nitrophenyl aminoethylurea yellow 27080-42-8
HC Yellow No. 6 yellow 104333-00-8
hydroxyethy1-2-nitro-p-toluidine yellow 100418-33-5
HC Yellow No. 12 yellow 59320-13-7
HC Yellow No. 7 yellow 104226-21-3
HC Yellow No. 10 yellow 109023-83-8
N-ethyl-3-nitro PABA yellow 2788-74-1
HC Yellow No. 13 yellow 10442-83-8
HC Yellow No. 15 yellow 138377-66-9
HC Yellow No. 14 yellow 90349-40-9
2,6-diamino-3-((pyridine-3-yl)azo)pyridine yellow 28365-08-4
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HC Orange No. 1 orange 54381-08-7
2-hydroxyethylamino-5-nitroanisole orange 66095-81-6
HC Orange No. 2 orange 85765-48-6
HC Orange No. 3 orange 81612-54-6
HC Blue No. 2 blue 33229-34-4
HC Blue No. 12 blue 132885-85-9
HC Blue No. 10 blue 173994-75-7
HC Blue No. 9 blue 114087-42-2
Indigo blue 482-89-3
HC Blue No. 14 blue 99788-75-7
Disperse Blue 23 blue 4471-41-4
Disperse Blue 3 blue 2475-46-9
Disperse Blue 377 blue 67674-26-4
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HC Green No. 1 green 52136-25-1
1,2,3,4-tetrahydro-6-nitrochinoxalin brown 41959-35-7
Disperse Black 9 black 20721-50-0
Preferred nonionic direct dyes:
2-amino-6-chloro-4-nitrophenol red 6358-09-4
HC Red 3 red 2871-01-4
4-nitro-o-phenylenediamine orange-red 99-56-9
Disperse Violet 1 violet 128-95-0
HC Yellow 2 yellow 4926-55-0
HC Yellow 4 yellow 59820-43-8
HC Yellow 15 yellow 138377-66-9
HC Blue 2 blue 33229-34-4
Disperse Blue 3 blue 2475-46-9
Disperse Blue 377 blue 67674-26-4
Disperse Black 9 black 20721-50-0
Cationic direct dyes (basic direct dyes):
Name Color CAS number
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2-[[4-(dimethyl-amino)phenyl]azo]-1,3-dimethy1-1H-
imidazolium chloride (basic red 51) red 77061-58-6
Basic Red 22 red 12221-52-2
Basic Red 76 red 68391-30-0
Basic Red 2 red 477-73-6
HC Red No. 8 red 123296-48-0
1-[(4-amino-2-nitrophenyl)azo]-7-(trimethylammonio)-
2-naphthol chloride (C.I. 12251:1; Basic red No. 118) red 71134-97-9
3,7-diamino-2,8-dimethy1-5-phenylphenazinium
chloride (C.I. 50240; Basic Red No. 2) red 477-73-6
1,4-dimethy1-5-[(4-(dimethylamino)phenyl)azo]-1,2,4-
triazolium chloride (C.I. 11055; Basic Red No. 22) red 113346-09-1
2-hydroxy-1[(2-methoxyphenyl)azo-7-
(trimethylammonio) naphthalene chloride (C.I. 12245;
Basic Red No. 76) red 68391-30-0
4-[(4-amino-3-methylphenyl)(4-imino-3-methy1-2,5-
cyclohexadien-1-ylidene)methy1]-2-
methylbenzenamine monohydrochloride (basic violet
2) violet 3248-91-7
Basic Violet 14 violet 632-99-5
bis[4-(dimethylamino)phenyl][4-
(methylamino)phenyl]carbenium chloride (C.I. 42535,
Basic Violet No. 1) violet 8004-87-3
tris-[4-(dimethylamino)phenyl]carbenium chloride (C.
I. 42555; Basic Violet No. 3) violet 548-62-9
2-[3,6-diethylamino) dibenzopyranium-9-y1 benzoic
acid chloride (C.I. 45170; Basic Violet No. 10) violet 81-88-9
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di(4-aminopheny1)-(4-amino-3-
methylphenyl)carbenium chloride (C.I. 42510; Basic
Violet No. 14) violet 632-99-5
2-[(4-aminophenyl)azo]-1,3-dimethy1-1H-imidazolium
chloride (basic orange 31) orange 97404-02-9
1-methy1-4-Rmethylphenyl-hydrazono)methyll-
pyridinium, methyl sulfate (basic yellow 87) yellow 68259-00-7
Basic Yellow 57 yellow 68391-31-1
Basic Yellow 29 yellow 68134-38-3
Basic Yellow 87 yellow 68259-00-7
2-[2-(2,4-dimethoxyphenyl)amino)etheny11-1,3,3-
trimethy1-3H-indol-1-ium chloride (C. I. 48055; Basic
Yellow No. 11) yellow 4208-80-4
3-methyl-l-pheny1-4-[(3-(trimethylammonio)
phenyl)azolpyrazol-5-one chloride (C.I. 12719; Basic
Yellow No. 57) yellow 68391-31-1
Basic Blue 7 blue 2390-60-5
Basic Blue 26 blue 2580-56-5
Basic Blue 99 blue 68123-13-7
1-(N-methylmorpholinium-propylamino)-4-hydroxy-
anthraquinone methylsulfate blue 38866-20-5
N,N-dimethy1-3-44-(methylamino)-9,10-dioxo-9,10-
dihydroanthracen-1-y1)amino)-N-propylpropan-1-
aminium bromide (HC blue No. 16)) blue 502453-61-4
HC Blue No. 8 blue 166377-62-4
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HC Blue No. 15 blue 5002453-61-4
9-(dimethylamino) benzo[a]phenoxazin-7-ium chloride
(C.I. 51175; Basic Blue No. 6) blue 966-62-1
di[4-diethylamino)phenyl][4-(ethylamino)naphthy1]-
carbenium chloride (C.I. 42595; Basic Blue No. 7) blue 2390-60-5
3,7-di(dimethylamino)phenothiazin-5-ium chloride,
(C.I. 52015; Basic Blue No. 9) blue 61-73-4
di[4-(dimethylamino)phenyl][4-
(phenylamino)naphthyl]carbenium chloride (C.I.
44045; Basic Blue 26) blue 2580-56-5
2-[4-(ethyl(2-hydroxyethyl)amino)phenyl)axo]-
6methoxyoxy-3-methylbenzothiazolium methylsulfate
(C.I. 11154; Basic Blue 41) blue 12270-13-2
8-amino-2-bromo-5-hydroxy-4-imino-6-[(3-
(trimethylammonio)phenyl)amino]-1(4H)-
naphthalenone chloride (C.I. 56059; Basic Blue No.
99) blue 68123-13-7
Basic Orange 31 orange 97404-02-9
Basic Brown 16 brown 26381-41-9
Basic Brown 17 brown 68391-32-2
1,3-bis[(2,4-diamino-5-methylphenyl)azo]-4-
methylbenzene (C.I. 21010, Basic Brown No. 4) brown 5421-66-9
1-[(4-aminophenyl)azo-7-(trimethylammonio)-2-
naphthol chloride (C.I. 12250, Basic Brown No. 16) brown 26381-41-9
1-[(4-aminophenyl)azo-7-(trimethylammonio)-2-
naphthol chloride (C.I. 12250, Basic Brown No. 16) brown 26381-41-9
1-[(4-amino-3-nitrophenyl)azo]-7-(trimethylammonio)-
2-naphthol chloride (C.I. 12251; Basic Brown No. 17) brown 68391-32-2
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bis-[4-(diethylamino)phenyl]phenylcarbenium
hydrogen sulfate (1:1) (C.I. 42040; Basic Green No: 1) green 633-03-4
Preferred basic (cationic) direct dyes
Basic red 51 red 77061-58-6
Basic orange 31 orange 97404-02-9
Basic yellow 87 yellow 68259-00-7
Anionic Direct Dyes (Acidic Direct Dyes):
Name Color CAS number
7-(2',4'-dimethy1-5'-sulfophenylazo)-5-sulfo-8-
hydroxynaphthalene (Ponceau SX, FD&C red 4) red 4548-53-2
Acid Red 4 red 5858-39-9
Acid Red 33 red 3567-66-6
Acid Violet 43 violet 4430-18-6
Acid Yellow 1 yellow 846-70-8
Acid Yellow 23 yellow 1934-21-0
sodium salt of mixture of mono- & disulfonic acids
(mainly the latter) of quinophthlanone or 2-
quinolylindandione yellow NA
Acid Orange 3 orange 6373-74-6
Acid Orange 7 orange 633-96-5
Acid Blue 9 blue 3844-45-9
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Acid Blue 25 blue 6408-78-2
Acid Blue 62 blue 4368-56-3
Acid Blue 199 blue 12219-28-2
Pigment Blue 15 blue 147-14-8
1-(3'-nitro-5'-sulfo-6'-oxophenylazo)-oxo-naphthalene
chromium complex brown 6370-15-6
Acid Black 1 black 1064-48-8
Acid Black 52 black 5610-64-0
Acid Black 132 black 12219-02-2
Carbonate ion source
Optionally the soluble solid hair coloring article may comprise a source of
carbonate ions or
carbamate ions or hydrogencarbonate ions or peroxymonocarbonate ions or any
mixture thereof.
The carbonate ions or carbamate ions or hydrogencarbonate ions or
peroxymonocarbonate ions may
be contained by the porous solid in the sense that the porous solid forms a
holding container for the
carbonate ions or carbamate ions or hydrogencarbonate ions or
peroxymonocarbonate ions.
Alternatively, the carbonate ions or carbamate ions or hydrogencarbonate ions
or
peroxymonocarbonate ions may be incorporated as part of the processing mixture
used to form the
porous solid.
The carbonate ions or carbamate ions or hydrogencarbonate ions or
peroxymonocarbonate ions may be located with the direct dye and any other
optional materials (e.g.,
oxidizing agents) or isolated from these materials.
The source of said ions herein is provided in the composition to provide a
carbonate ion
concentration of at least 0.2 mol/L upon admixture of the soluble solid hair
coloring article with
water. The soluble solid hair coloring article are designed to preferably
provide from about 0.4
mo1/1 to about 2.0 mol/L, more preferably from about 0.5 mol/L to about 1.5
mol/L of the source of
said ions, upon admixture of the soluble solid hair coloring article with
water.
Any source of these ions may be utilized, including solid sources. Suitable
sources for use
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herein include sodium, potassium, lithium, calcium, magnesium, barium,
ammonium salts of
carbonate, carbamate and hydrogencarbonate ions and mixtures thereof such as
sodium carbonate,
sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate,
lithium carbonate,
calcium carbonate, magnesium carbonate, barium carbonate, ammonium carbonate,
ammonium
5 hydrogen carbonate and mixtures thereof. Percarbonate salts may also be
utilized to provide both
the source of carbonate ions and oxidizing agent. Preferred solid sources of
carbonate ions,
carbamate and hydrogencarbonate ions are sodium percarbonate, potassium
percarbonate, calcium
percarbonate, and mixtures thereof.
Oxidizing agent
10 The soluble solid hair coloring article according to the present
invention may comprise at
least one source of an oxidizing agent. Preferred oxidizing agents for use
herein are solid water-
soluble peroxygen oxidizing agents. "Watr-soluble" as defined herein means
that in standard
condition at least 0.1g, preferably lg, more preferably lOg of said oxidizing
agent can be dissolved
in 1 liter of deionized water. The oxidizing agents are valuable for the
initial solubilisation and
15 decolorisation of the melanin (bleaching) in the hair shaft.
The oxidizing agents may be contained by the porous solid in the sense that
the porous solid
forms a holding container for the oxidizing agents. Alternatively, the
oxidizing agents may be
incorporated as part of the processing mixture used to form the porous solid.
The oxidizing agent
may be located with the direct dye, the carbonate ions or carbamate ions or
hydrogencarbonate ions
20 or peroxymonocarbonate ions or isolated from these other materials.
Any solid oxidizing agent known in the art may be utilized in the present
invention.
Preferred water-soluble oxidizing agents are inorganic peroxygen materials
capable of yielding
hydrogen peroxide in an aqueous solution. Water-soluble peroxygen oxidizing
agents are well
known in the art and include hydrogen peroxide, inorganic alkali metal
peroxides such as sodium
25 periodate and sodium peroxide and organic peroxides such as urea
peroxide, melamine peroxide,
and inorganic perhydrate salt bleaching compounds, such as the alkali metal
salts of perborates,
percarbonates, perphosphates, persilicates, persulphates and the like. These
inorganic perhydrate
salts may be incorporated as monohydrates, tetrahydrates etc. Alkyl and aryl
peroxides, and/ or
peroxidases may also be used. Mixtures of two or more such oxidizing agents
can be used if desired.
Preferred for use in the soluble solid hair coloring article are percarbonate
(which may be used to
provide a source of both oxidizing agent and carbonate ions), persulphates and
combinations
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thereof.
Optionally the soluble solid hair coloring article may form
peroxymonocarbonate ions.
These ions are typically formed in-situ from the reaction between a source of
hydrogen peroxide and
carbonate ion.
According to the present invention the soluble solid hair coloring article may
be designed to
provide from about 0.1% to about 10% by weight, in another embodiment from
about 1% to about
7% by weight, and in an alternate embodiment from about 2% to about 5% by
weight, of an
oxidizing agent upon admixture of the soluble solid hair coloring article with
water.
Source of ammonium ions
Optionally the soluble solid hair coloring article may comprise at least one
solid source of
ammonium ions. The source of the ammonium ions may be contained by the porous
solid in the
sense that the porous solid forms a holding container for the source of
ammonium ions. Suitable
holding container forms include an envelope, pouch or sandwich structure.
Alternatively, the source
of ammonium ions may be incorporated as part of the processing mixture used to
form the porous
solid.
Any solid source of ammonium ions is suitable for use herein. Preferred
sources include
ammonium chloride, ammonium sulphate, ammonium nitrate, ammonium phosphate,
ammonium
acetate, ammonium carbonate, ammonium hydrogen carbonate, ammonium carbamate,
ammonium
hydroxide, percarbonate salts, ammonia and mixtures thereof. Particularly
preferred are ammonium
sulfate, ammonium carbonate, ammonium carbamate, ammonia and mixtures thereof.
In one
embodiment, the source of ammonium ions and source of carbonate ions or
carbamate ions or
hydrogencarbonate ions or peroxymonocarbonate ions or any mixture thereof, are
present in the
soluble solid hair coloring article at a weight ratio of from 3:1 to 1:10,
preferably 2:1 to 1:5.
The soluble solid hair coloring articles are preferably designed to provide
from about 0.1%
to about 10% by weight, alternatively from about 0.5% to about 5% by weight,
and alternatively
from about 1% to about 3% by weight, of ammonium ions upon admixture of the
soluble solid hair
coloring article with water.
Water-Soluble Polymer ("Polymer Structurant")
The present invention comprises water-soluble polymer that functions as a
structurant. As
used herein, the term "water-soluble polymer" is broad enough to include both
water-soluble and
water-dispersible polymers, and is defined as a polymer with solubility in
water, measured at 25 C,
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of at least about 0.1 gram/liter (g/L). In some embodiments, the polymers have
solubility in water,
measured at 25 C, of from about 0.1 gram/liter (g/L) to about 500 grams/liter
(g/L). This level
indicates production of a macroscopically isotropic or transparent, colored or
colorless solution. The
polymers for making these solids may be of synthetic or natural origin and may
be modified by
means of chemical reactions. They may or may not be film-forming. These
polymers should be
physiologically acceptable, i.e., they should be compatible with the skin,
mucous membranes, the
hair and the scalp.
The terms "water-soluble polymer" and "polymer structurant" are used
interchangeably
herein. Furthermore, whenever the singular term "polymer" is stated, it should
be understood that
the term is broad enough to include one polymer or a mixture of more than one
polymer. For
instance, if a mixture of polymers is used, the polymer solubility as referred
to herein would refer to
the solubility of the mixture of polymers, rather than to the solubility of
each polymer individually.
The one or more water-soluble polymers of the present invention are selected
such that their
weighted weight average molecular weight is from about 40,000 to about
500,000, in one
embodiment from about 50,000 to about 400,000, in yet another embodiment from
about 60,000 to
about 300,000, and in still another embodiment from about 70,000 to about
200,000. The weighted
weight average molecular weight is computed by summing the weight average
molecular weights of
each polymer raw material multiplied by their respective relative weight
percentages by weight of
the total weight of polymers present within the porous solid. Suitable water-
soluble polymers are
discussed in WO 2010077650 A2 at page 19, line 26 ¨ page 22, line 12.
The water-soluble polymer may be present from about 10% to about 50% by weight
of the
porous dissolvable solid substrate of one or more water-soluble polymer, in
one embodiment from
about 15% to about 40%, and in a particular embodiment from about 20% to about
30% by weight
of the porous dissolvable solid substrate of one or more water-soluble
polymers.
The water-soluble polymer may be present from about 10% to about 50% by weight
of the
pre-mix used to form the porous dissolvable solid substrate of one or more
water-soluble polymer,
in one embodiment from about 10% to about 20%, and in another embodiment from
about 10% to
about 15%, by weight.
Water-soluble polymers of the present invention include polyvinyl alcohols,
polyvinylpyrrolidones, starch and starch derivatives, pullulan, gelatin,
hydroxypropylmethylcelluloses, methycelluloses, and carboxymethycellulo ses .
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Water-soluble polymers of the present invention include polyvinyl alcohols,
and
hydroxypropylmethylcelluloses. Suitable polyvinyl alcohols include those
available from Celanese
Corporation (Dallas, TX) under the Celvol trade name including, but not
limited to, Celvol 523,
Celvol 530, Celvol 540, Celvol 518, Celvol, 513, Celvol 508, Celvol 504, and
combinations thereof.
Suitable hydroxypropylmethylcelluloses include those available from the Dow
Chemical Company
(Midland, MI) under the Methocel trade name including, but not limited, to
Methocel E50, Methocel
E15, Methocel E6, Methocel E5, Methocel E3, Methocel F50, Methocel K100,
Methocel K3,
Methocel A400, and combinations thereof including combinations with above
mentioned
hydroxypropylmethylcelluloses.
In one embodiment polyvinyl chloride is a suitable polymer structurant.
Polymeric Structurant Additive
The porous solid of the soluble solid hair coloring article may comprise an
additive that aids
in processing, provides sensory benefits, or both. Such additives include
polyalkylene oxides
selected such that their approximate weight average molecular weight is
between about 100,000 and
about 4,000,000. The additive may provide foam boosting properties and may
also act as an
emollient, providing benefits to both the manufacture of the porous solid and
end use benefits to the
hair after application of the hair coloring article. Suitable additives may be
selected from materials
from Dow Chemical sold under the tradename POLYOX TM ex. the Dow Chemical
Company or an
affiliated company of Dow.
POLYOX Grades INCI Name Approx. Molecular Weight Viscosity (cPs)
POLYOX WSR-205 PEG-14M 600,000 4500 ¨ 8800a
POLYOX WSR-301 PEG-90M 4,000,000 1650 ¨
5500c
POLYOX WSR N-10 PEG-2M 100,000 12¨ 50a
POLYOX WSR N-80 PEG-5M 200,000 65 ¨ 115a
POLYOX WSR N-750 PEG-7M 300,000 600 ¨ 1,000a
POLYOX WSR N-3000 PEG-14M 400,000 2250 ¨ 4500a
POLYOX WSR N-12K PEG-23M 1,000,000 400 ¨ 800b
POLYOX WSR N-60K PEG-45M 2,000,000 200 ¨ 400b
a: 5% solution
b: 2% solution
c: 1% solution
The polymeric structurant additive may be present in the soluble solid hair
coloring article,
such as the porous solid, from about 0.1% to about 10% by weight of the premix
that is formed into
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the porous solid, such as from about 1% to about 8%, such as from about 2% to
about 5% by weight
of the premix that is formed into the porous solid.
Plasticizer
The porous solid of the soluble solid hair coloring article comprises a water
soluble
plasticizing agent suitable for use in the soluble hair coloring article. Non-
limiting examples of
suitable plasticizing agents include polyols, copolyols, polycarboxylic acids,
polyesters and
dimethicone copolyols.
In one embodiment, the one or more plasticizers may be present from about 1%
to about
30% by weight of the soluble solid hair coloring article, such as the porous
solid; in another
embodiment from about 3% to about 25%, in another embodiment from about 5% to
about 20%,
and in yet another embodiment from about 8% to about 15% by weight of the
soluble solid hair
coloring article, such as the porous solid.
The one or more plasticizers may be present from about 1% to about 10% by
weight of the
premix used to form the soluble solid hair coloring article, such as the
porous solid, in one
embodiment from about 3% to about 6% by weight of the premix.
Examples of useful polyols include, but are not limited to, glycerin,
diglycerin, propylene
glycol, ethylene glycol, butylene glycol, pentylene glycol, cyclohexane
dimethanol, hexane diol,
polyethylene glycol (200-600), sugar alcohols such as sorbitol, manitol,
lactitol and other mono- and
polyhydric low molecular weight alcohols (e.g., C2-C8 alcohols); mono di- and
oligo-saccharides
such as fructose, glucose, sucrose, maltose, lactose, and high fructose corn
syrup solids and ascorbic
acid. Examples of polycarboxylic acids include, but are not limited to citric
acid, maleic acid,
succinic acid, polyacrylic acid, and polymaleic acid. Examples of suitable
polyesters include, but
are not limited to, glycerol triacetate, acetylated-monoglyceride, diethyl
phthalate, triethyl citrate,
tributyl citrate, acetyl triethyl citrate, acetyl tributyl citrate. Examples
of suitable dimethicone
copolyols include, but are not limited to, PEG-12 dimethicone, PEG/PPG-18/18
dimethicone, and
PPG-12 dimethicone.
Other suitable platicizers of the present invention include, but are not
limited to, alkyl and
allyl phthalates; napthalates; lactates (e.g., sodium, ammonium and potassium
salts); sorbeth-30;
urea; lactic acid; sodium pyrrolidone carboxylic acid (PCA); sodium
hyraluronate or hyaluronic
acid; soluble collagen; modified protein; monosodium L-glutamate; alpha & beta
hydroxyl acids
such as glycolic acid, lactic acid, citric acid, maleic acid and salicylic
acid; glyceryl
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polymethacrylate; polymeric plasticizers such as polyquaterniums; proteins and
amino acids such
as glutamic acid, aspartic acid, and lysine; hydrogen starch hydrolysates;
other low molecular
weight esters (e.g., esters of C2-C10 alcohols and acids); and any other water
soluble plasticizer
known to one skilled in the art of the foods and plastics industries; and
mixtures thereof.
5 EP283165B1 discloses other suitable plasticizers, including glycerol
derivatives such as
propoxylated glycerol.
In one embodiment, the plasticizers include glycerin or propylene glycol and
combinations
thereof.
Surfactants and Emulsifiers
10 The surfactant component of the porous solid of the soluble solid
hair coloring article is used
as a processing aide in preparing a stable solid porous structure for the
porous solids described
herein.
Cationic Surfactants
The porous solid may comprise from about 2% to about 75% of a cationic
surfactant, by
15 weight of the soluble solid hair coloring article, such as the porous
solid. The cationic surfactant
may be present from about 0.1% to about 30% by weight of the premix used to
form the soluble
solid hair coloring article, such as the porous solid of cationic surfactants,
such as from about 1% to
about 25% by weight of the premix used to form the porous solid of cationic
surfactants.
Suitable cationic surfactants comprise an amino or quaternary ammonium
hydrophilic
20 moiety which is positively charged when dissolved.
Suitable quaternary ammonium cationic surfactants useful herein include, but
are not limited
to, those having the formula (I):
R1
\ / R4
N+ X-
R2/ \ q
25 R-
Formula (I)
in which R1, R2, R3, and R4 of formula (I) are each independently selected
from (a) an aliphatic
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group of from 1 to 22 carbon atoms, or (b) an aromatic, alkoxy,
polyoxyalkylene, alkylamido,
hydroxyalkyl, aryl or alkylaryl group having up to 22 carbon atoms; and X is a
salt-forming anion
such as those selected from halogen (e.g. chloride, bromide), acetate,
citrate, lactate, glycolate,
phosphate, nitrate, sulphate, and alkylsulphate radicals. In one embodiment,
the alkylsulphate
radical is methosulfate and/or ethosulfate.
The aliphatic groups can contain, in addition to carbon and hydrogen atoms,
ether linkages,
and other groups such as amino groups. The longer chain aliphatic groups,
e.g., those of about 12
carbons, or higher, can be saturated or unsaturated and branched or
unbranched. In one
embodiment, the class of cationic conditioner actives of general formula (I),
R1 and R2 are each
independently selected from C16 to C22 hydrocarbyl chains comprising at least
one ester linkage in
both R1 and R2, and R3 and R4 are each independently selected from CH3 and
CH2CH2OH. In
another embodiment, the class of cationic conditioner actives of general
formula (I), R1 and R2 are
each independently selected from C16 to C22 saturated or unsaturated, and R3
and R4 are each
independently selected from CH3, CH2CH2OH, and CH3. In yet another embodiment,
the class of
cationic conditioner actives of general formula (I), R1 is a C16 to C22 alkyl
chain and R2, R3 and R4
are each independently selected from CH3, CH2CH2OH, and CH3.
Suitable quaternary ammonium cationic conditioner actives of general formula
(I) can
include cetyltrimethylammonium chloride, behenyltrimethylammonium chloride
(BTAC),
stearyltrimethylammonium chloride, cetylpyridinium chloride,
octadecyltrimethylammonium
chloride, hexadecyltrimethylammonium chloride, octyldimethylbenzylammonium
chloride,
decyldimethylbenzylammonium chloride, stearyldimethylbenzylammonium
chloride,
didodecyldimethylammonium chloride, dioctadec yldimethyl ammonium
chloride,
distearyldimethylammonium chloride, tallowtrimethylammonium
chloride,
cocotrimethylammonium chloride, dipalmitoylethyldimethylammonium chloride, PEG-
2
oleylammonium chloride and salts of these, where the chloride is replaced by
halogen (e.g.,
bromide), acetate, citrate, lactate, glycolate, phosphate nitrate, sulphate,
or alkylsulphate.
In a particular embodiment, the quaternary ammonium cationic conditioner
actives for use in
the invention are cetyltrimethylammonium chloride, available commercially, for
example as
GENAMIN CTAC by Clariant and ARQUAD 16/29 supplied by Akzo Nobel,
behenyltrimethylammonium chloride (BTMAC) such as GENAMIN KDMP supplied by
Clariant,
and distearyldimethylammonium chloride such as GENAMIN DSAP supplied by
Clariant.
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Mixtures of any of the foregoing materials may also be suitable. In a
preferred embodiment, the
quaternary ammonium cationic conditioner active is behenyltrimethylammonium
chloride
(BTMAC).
Other suitable cationic surfactant conditioner actives can include salts of
primary, secondary,
and tertiary fatty amines. In one embodiment, the alkyl groups of such amines
have from about 12
to about 22 carbon atoms, and can be substituted or unsubstituted. These
amines are typically used
in combination with an acid to provide the cationic species.
Suitable alkyl amine salts useful herein include, but are not limited to,
those salts corresponding
to alkyl amines having the general formula (II):
R1¨C(0)¨N(H)¨R2¨N(R3)(R4)
Formula (II)
in which R1 of formula (II) is a fatty acid chain containing from 12 to 22
carbon atoms, R2 of
formula (II) is an alkylene group containing from one to four carbon atoms,
and R3 of formula (II)
and R4 of formula (II) are, independently, an alkyl group having from one to
four carbon atoms. R1
can be saturated or unsaturated and branched or unbranched.
Suitable materials of general formula (II) are stearamidopropyldimethylamine,
stearamidopropyldiethylamine, stearamidoethyldiethylamine,
stearamidoethyldimethylamine,
palmitamidopropyldimethylamine, palmitamidopropyldiethylamine,
palmitamidoethyldiethylamine,
palmitamidoethyldimethylamine,
behenamidopropyldimethylamine,
behenamidopropyldiethylamine, behenamidoethyldiethylamine,
behenamidoethyldimethylamine,
arachidamidopropyldimethylamine,
arachidamidopropyldiethylamine,
arachidamidoethyldiethylamine, arachidamidoethyldimethylamine,
and
diethylaminoethylstearamide.
Other suitable alkyl amine salts can include dimethylstearamine,
dimethylsoyamine, soyamine,
myristylamine, tridecylamine, ethylstearylamine, N-tallowpropane diamine,
ethoxylated (with 5
moles of ethylene oxide) stearylamine, dihydroxyethylstearylamine, and
arachidyl behenylamine. In
a preferred embodiment, the alkyl amine salt is stearamidopropyldimethylamine.
Mixtures of any of
the foregoing materials may also be suitable.
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Non-ionic surfactants
The porous solid may comprise from about 2% to about 75% of a nonionic
surfactant, by
weight of the soluble solid hair coloring article, such as the porous solid.
The porous solid may
comprise from about 0.1% to about 30% by weight of the premix used to form the
porous solid of
nonionic surfactants, such as from about 0.5% to about 10% by weight of the
premix used to form
the porous solid of nonionic surfactants.
In one embodiment nonionic surfactants are surfactants to be employed as a
process aid in
making the soluble porous solid. Suitable nonionic surfactants include, but
are not limited to, fatty
alcohols, polyoxyethylenated alkyl phenols, polyoxyethylenated alcohols,
polyoxyethylenated
polyoxypropylene glycols, glyceryl esters of alkanoic acids, polyglyceryl
esters of alkanoic acids,
propylene glycol esters of alkanoic acids, sorbitol esters of alkanoic acids,
polyoxyethylenated
sorbitor esters of alkanoic acids, polyoxyethylene glycol esters of alkanoic
acids,
polyoxyethylenated alkanoic acids, alkanolamides, N-alkylpyrrolidones, alkyl
glycosides, alkyl
polyglucosides, alkylamine oxides, and polyoxyethylenated silicones.
Representative fatty alcohols include decyl alcohol, lauryl alcohol, myristyl
alcohol, cetyl
alcohol, stearyl alcohol, oleyl alcohol and mixtures thereof.
Representative polyoxyethylenated alcohols include alkyl chains ranging in the
C9-C16 range
and having from about 1 to about 110 alkoxy groups including, but not limited
to, laureth-3, laureth-
23, ceteth-10, steareth-10, steareth-100, beheneth-10, and commercially
available from Shell
Chemicals, Houston, Texas under the trade names NEODOL 91, NEODOL 23, NEODOL
25,
NEODOL 45, NEODOL 135, NEODOL 67, NEODOL PC 100, NEODOL PC 200,
NEODOL PC 600, and mixtures thereof.
Also available commercially are the polyoxyethylene fatty ethers available
commercially
under the BRIJ trade name from Uniqema, Wilmington, Delaware, including, but
not limited to,
BRIJ 30, BRIJ 35, BRIJ 52, BRIJ 56, BRIJ 58, BRIJ 72, BRIJ 76,
BRIJ 78,
BRIJ 93, BRIJ 97, BRIJ 98, BRIJ 721 and mixtures thereof.
Suitable alkyl glycosides and alkyl polyglucosides can be represented by the
formula
(Sugar)n-O-R of formula (III) wherein (Sugar) of formula (III) is a sugar
moiety such as glucose,
fructose, mannose, galactose, and the like; n of formula (III) is an integer
of from about 1 to about
1000, and R of formula (III) is a C8-C30 alkyl group. Examples of long chain
alcohols from which
the alkyl group can be derived include decyl alcohol, lauryl alcohol, myristyl
alcohol, cetyl alcohol,
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stearyl alcohol, oleyl alcohol, and the like. Examples of these surfactants
include alkyl
polyglucosides wherein (Sugar) is a glucose moiety, R is a C8_20 alkyl group,
and n is an integer of
from about 1 to about 9. Commercially available examples of these surfactants
include decyl
polyglucoside and lauryl polyglucoside available under trade names APG@ 325
CS, APG@ 600 CS
and APG@ 625 CS) from Cognis, Ambler, PA. Also useful herein are sucrose ester
surfactants such
as sucrose cocoate and sucrose laurate and alkyl polyglucosides available
under trade names
TRITONTm BG-10 and TRITONTm CG-110 from The Dow Chemical Company, Houston, TX.
Other nonionic surfactants suitable for use in the present invention are
glyceryl esters and
polyglyceryl esters, including but not limited to, glyceryl monoesters,
glyceryl monoesters of C12_22
saturated, unsaturated and branched chain fatty acids such as glyceryl oleate,
glyceryl monostearate,
glyceryl monopalmitate, glyceryl monobehenate, and mixtures thereof, and
polyglyceryl esters of
C12_22 saturated, unsaturated and branched chain fatty acids, such as
polyglyceryl-4 isostearate,
polyglyceryl-3 oleate, polyglyceryl-2- sesquioleate, triglyceryl
diisostearate, diglyceryl monooleate,
tetraglyceryl monooleate, and mixtures thereof.
Also useful herein as nonionic surfactants are sorbitan esters. Sorbitan
esters of C12-22
saturated, unsaturated, and branched chain fatty acids are useful herein.
These sorbitan esters
usually comprise mixtures of mono-, di-, tri-, etc. esters. Representative
examples of suitable
sorbitan esters include sorbitan monolaurate (SPAN 20), sorbitan
monopalmitate (SPAN 40),
sorbitan monostearate (SPAN 60), sorbitan tristearate (SPAN 65), sorbitan
monooleate (SPAN
80), sorbitan trioleate (SPAN 85), and sorbitan isostearate.
Also suitable for use herein are alkoxylated derivatives of sorbitan esters
including, but not
limited to, polyoxyethylene (20) sorbitan monolaurate (TWEEN@ 20),
polyoxyethylene (20)
sorbitan monopalmitate (TWEEN@ 40), polyoxyethylene (20) sorbitan monostearate
(TWEEN@
60), polyoxyethylene (20) sorbitan monooleate (TWEEN@ 80), polyoxyethylene (4)
sorbitan
monolaurate (TWEEN@ 21), polyoxyethylene (4) sorbitan monostearate (TWEEN@
61),
polyoxyethylene (5) sorbitan monooleate (TWEEN@ 81), and mixtures thereof, all
available from
Uniqema.
Also suitable for use herein are alkylphenol ethoxylates including, but not
limited to,
nonylphenol ethoxylates (TERGITOLTm NP-4, NP-6, NP-7, NP-8, NP-9, NP-10, NP-
11, NP-12,
NP-13, NP-15, NP-30, NP-40, NP-50, NP-55, NP-70 available from The Dow
Chemical Company,
Houston, TX) and octylphenol ethoxylates (TRITONTm X-15, X-35, X-45, X-114, X-
100, X-102,
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X-165, X-305, X-405, X-705 available from The Dow Chemical Company, Houston,
TX).
Also suitable for use herein are alkanolamides including cocamide
monoethanolamine
(CMEA) and tertiary alkylamine oxides including lauramine oxide and cocamine
oxide.
In one embodiment a mixture of nonionic and cationic surfactant are present
from about 2%
5 to about 75% by weight of the soluble solid hair coloring article.
Amphoteric Surfactants
The porous solid may comprise from about 2% to about 75% of an amphoteric
surfactant, by
weight of the soluble solid hair coloring article, such as the porous solid.
The porous solid may
comprise from about 0.1% to about 30% by weight of the premix used to form the
porous solid of
10 amphoteric surfactants, such as from about 1% to about 25% by weight of
the premix used to form
the porous solid of amphoteric surfactants.
Amphoteric surfactants suitable for use in the soluble porous solid includes
those that are
broadly described as derivatives of aliphatic secondary and tertiary amines in
which the aliphatic
radical can be straight or branched chain and wherein one of the aliphatic
substituents contains from
15 about 8 to about 18 carbon atoms and one contains an anionic water
solubilizing group, e.g.,
carboxy, sulfonate, sulfate, phosphate, or phosphonate. Examples of compounds
falling within this
definition are sodium 3-dodecyl-aminopropionate, sodium 3-dodecylaminopropane
sulfonate,
sodium lauryl sarcosinate, N-alkyltaurines such as the one prepared by
reacting dodecylamine with
sodium isethionate according to the teaching of U.S. 2,658,072, N-higher alkyl
aspartic acids such
20 as those produced according to the teaching of U.S. 2,438,091, and the
products described in U.S.
2,528,378.
Zwitterionic surfactants suitable for use include those that are broadly
described as
derivatives of aliphatic quaternary ammonium, phosphonium, and sulfonium
compounds, in which
the aliphatic radicals can be straight or branched chain, and wherein one of
the aliphatic substituents
25 contains from about 8 to about 18 carbon atoms and one contains an
anionic group, e.g., carboxy,
sulfonate, sulfate, phosphate, or phosphonate. Zwitterionic surfactants
suitable for use include
betaines, including cocoamidopropyl betaine, alkylamphoacetates including
lauroamphoacetate and
cocoamphoacetate. Alkylamphoacetates can be comprised of monoacetates and
diacetates.
Emulsifiers
30 The premix for making the soluble solid hair coloring article, such as a
porous solid, may
comprise from about 1% to about 20% of an emulsifier, by weight of the soluble
solid hair coloring
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article, such as the porous solid. Examples of emulsifiers include mono- and
di-glycerides,
polyglycerol esters, propylene glycol esters, sorbitan esters and other
emulsifiers known or
otherwise commonly used to stabilize air interfaces.
Optional Ingredients
The soluble solid hair coloring article, such as a porous solid, may further
comprise other
optional ingredients that are known for use or otherwise useful in a hair
colorant composition,
provided that such optional materials are compatible with the selected
essential materials described
herein, or do not otherwise unduly impair product performance.
Such optional ingredients are most typically those materials approved for use
in cosmetics.
Non limiting examples of such optional ingredients include silicones,
including aminosilicones,
preservatives, thickeners, sensates, plant extracts, pH modifiers, anti-
microbial agents, co-solvents
or other additional solvents, and similar other materials.
Silicones
An optional ingredient may include silicones, such as polyalkyl siloxanes,
polyaryl
siloxanes, polyalkylaryl siloxanes, polyether siloxane copolymers, amino
substituted silicones,
quaternized silicones, and mixtures thereof. Preferred polyalkyl siloxanes
include, for example,
polydimethylsiloxane, polydiethylsiloxane, and polymethylphenylsiloxane.
Polydimethylsiloxane,
which is also known as dimethicone, is especially preferred. Suitable amino
substituted silicones
include terminally substituted or pendant substituted amino substituted
silicones.
Silicones may be present from about 0.5% to about 5% by weight of the premix
used to form
the soluble solid hair coloring article, such as a porous solid.
Suitable terminally substituted amino silicones conform to the general formula
(IV):
(Ri)aG3_a-Si-(-0SiG2).-(-0SiGb(R02-b)m-O-SiG3_a(Ri)a
Formula (IV)
wherein G of formula (IV) is hydrogen, phenyl, hydroxy, or C1-C8 alkyl,
preferably methyl; a of
formula (IV) is 0 or an integer having a value from 1 to 3, preferably 1; b of
formula (IV) is 0, 1 or
2, preferably 1; n of formula (IV) is a number from 0 to 1,999; m is an
integer from 0 to 1,999; the
sum of n and m is a number from 1 to 2,000; a and m are not both 0; R1 of
formula (IV) is a
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monovalent radical conforming to the general formula CqH2qL, wherein q is an
integer having a
value from 2 to 8 and L is selected from the following groups: -N(R2)CH2-CH2-
N(R2)2; -N(R2)2;
-N(R2)3A; -N(R2)CH2-CH2-NR2H2A ; wherein R2 is hydrogen, phenyl, benzyl, or a
saturated
hydrocarbon radical, preferably an alkyl radical from about C1 to about C20; A
is a halide ion.
Highly preferred amino silicones are those corresponding to formula (IV)
wherein m=0, a=1,
q=3, G=methyl, n is preferably from about 1500 to about 1700, more preferably
about 1600; and L
is ¨N(CH3)2 or ¨NH2, more preferably ¨NH2. Another highly preferred amino
silicones are those
corresponding to formula (IV) wherein m=0, a=1, q=3, G=methyl, n is preferably
from about 400 to
about 600, more preferably about 500; and L is ¨N(CH3)2 or ¨NH2, more
preferably ¨NH2. Such
highly preferred amino silicones can be called terminal aminosilicones, as one
or both ends of the
silicone chain are terminated by a nitrogen containing group.
Suitable pendant substituted amino silicones are discussed in US
2007/0039103A1 at
paragraphs [0027] ¨ [0031].
Other optional ingredients include organic solvents, especially water miscible
solvents and
co-solvents useful as solublizing agents for polymeric structurants and as
drying accelerators. Non-
limiting examples of suitable solvents include alcohols, esters, ketones,
aromatic hydrocarbons,
aliphatic hydrocarbons, ethers, and combinations thereof. In one embodiment
the alcohols are
monohydric.
In another embodiment monohydric alcohols are ethanol, iso-propanol, and n-
propanol. In
one embodiment esters are ethyl acetate and butyl acetate. Other non-limiting
examples of suitable
organic solvents are benzyl alcohol, amyl acetate, propyl acetate, acetone,
heptane, iso-butyl acetate,
iso-propyl acetate, toluene, methyl acetate, iso-butanol, n-amyl alcohol, n-
butyl alcohol, hexane, and
methyl ethyl ketone. methanol, ethanol, n-propanol, isopropanol, n-butanol,
isobutanol,
methylethylketone, acetone, and combinations thereof.
Other optional ingredients include latex or emulsion polymers, thickeners such
as water
soluble polymers, clays, silicas, waxes, ethylene glycol distearate,
deposition aids, including
coacervate forming components and quaternary amine compounds.
Product Form
The soluble porous solids can be produced in any of a variety of product
forms, including
soluble porous solids that can be used alone or in combination with direct
dyes and other optional
components. The soluble porous solids are in the form of one or more flat
sheets or pads of an
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adequate size to be able to be handled easily by the user. It may have a
square, rectangle or disc
shape or any other shape. The pads can also be in the form of a continuous
strip including delivered
on a tape-like roll dispenser with individual portions dispensed via
perforations and/or a cutting
mechanism. Alternatively, the soluble porous solids of the present invention
are in the form of one
or more cylindrical objects, spherical objects, tubular objects or any other
shaped object. The
soluble porous solids may have a thickness (caliper) of from about 0.5 mm to
about 10 mm, in one
embodiment from about 1 mm to about 7 mm, and in still another embodiment from
about 2 mm to
about 6 mm. In the case of cylindrical, spherical, or other objects with more
of a third dimension
versus a pad or strip, the thickness is taken as the maximum distance of the
shortest dimension, i.e.,
the diameter of a sphere or cylinder for instance.
The soluble porous solids may comprise one or more textured, dimpled or
otherwise
topographically patterned surfaces including letters, logos or figures. The
textured substrate can
result from the shape of the substrate, in that the outermost surface of the
substrate contains portions
that are raised with respect to other areas of the surface. The raised
portions can result from the
formed shape of the article, for example the article can be formed originally
in a dimpled or waffle
pattern. The raised portions can also be the result of creping processes,
imprinted coatings,
embossing patterns, laminating to other layers having raised portions, or the
result of the physical
form of the soluble porous solid substrate itself. The texturing can also be
the result of laminating a
first soluble porous solid to a second soluble porous solid that is textured.
In a particular embodiment, the soluble porous solids may be perforated with
holes or
channels penetrating into or through the porous solid. These perforations can
be formed during the
drying process via spikes extended from the surface of the underlying mould,
belt or other non-stick
surface. Alternatively, these perforations can be formed after the drying
process via poking or
sticking the porous solids with pins, needles or other sharp objects. In one
embodiment, these
perforations are great in number per surface area, but not so great in number
so as to sacrifice the
integrity or physical appearance of the porous solid. Without being limited by
a theory, it is
believed that perforations increase the dissolution rate of the porous solids
into water relative to un-
perforated porous solids.
The soluble porous solids can also be delivered via a water insoluble
implement or device.
For instance, they may be attached or glued by some mechanism to an applicator
to facilitate
application to hair, i.e., a comb, rag, wand, or any other conceivable water-
insoluble applicator.
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Additionally, the soluble porous solids may be adsorbed to the surfaces of a
separate high surface
area water-insoluble implement, i.e., a porous sponge, a puff, a flat sheet
etc. For the latter, the
soluble porous solid may be adsorbed as a thin film or layer or included
within a specific regional
space provided by the implement.
Method of Manufacture
The soluble solid hair coloring article comprises a soluble porous solid which
can be
prepared by the process comprising: (1) Preparing a processing mixture
comprising surfactant(s),
dissolved polymer structurant and other optional ingredients; (2) Aerating the
processing mixture by
introducing a gas into the mixture to form an aerated processing mixture; (3)
Forming the aerated
process mixture into one or more desired shapes to form a shaped aerated
processing mixture; and
(4) Drying the shaped aerated processing mixture to a desired final moisture
content (e.g., from
about 0.1 % to about 25%, in one embodiment from about 3% to about 25%, in
another embodiment
from about 5% to about 20% and in yet another embodiment from about 7% to
about 15%, by
addition of energy) to form the soluble porous solid.
Preparation of Processing Mixture (Pre-Mix)
The processing mixture or pre-mix is generally prepared by dissolving the
polymer
structurant in the presence of water, plasticizer and other optional
ingredients by heating followed
by optional cooling. In one embodiment, a direct dye is included in the
preparation step with the
surfactant(s), dissolving polymer structurant and plasticizer. The preparation
step is accomplished
by dissolving the desired components in any suitable heated batch agitation
system or via any
suitable continuous system involving either single screw or twin screw
extrusion or heat exchangers
together with either high shear or static mixing. The ingredients may be
included in a step-wise via
pre-mix portions or of any combination of ingredients or as a single batch.
The processing mixtures may comprise: from about 15% to about 50% solids, in
one
embodiment from about 20% to about 40% solids, and in another embodiment from
about 25% to
about 35% solids, by weight of the processing mixture before drying; and have
a viscosity of from
about 2,500 cps to about 75,000 cps, in one embodiment from about 5,000 cps to
about 75,000 cps,
in another embodiment from about 7,500 cps to about 75,000 cps, and in still
another embodiment
from about 10,000 cps to about 75,000 cps, in another embodiment from about
65,000 cps to about
70,000 cps.
The processing mixture viscosity values can be measured on a suitable
rheometer, such as a
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TA Instruments AR500 Rheometer with 4.0 cm diameter parallel plate and 1,200
micron gap at a
shear rate of 1.0 reciprocal seconds for a period of 30 seconds at 25 C
(available from TA
Instruments, New Castle, DE), or on a standard viscometer, such as a
Brookfield Model DV-1
PRIME Digital Viscometer with CP-41 and CP-42 spindles at a shear rate of 1.0
reciprocal seconds
5 for a period of 2 minutes at 25 C (available from Brookfield Engineering
Laboratories, Inc.,
Middleboro, MA).
The percent (%) solids content is the summation of the weight percentages by
weight of the
total processing mixture of all of the solid, semi-solid and liquid components
excluding water and
any obviously volatile materials such as low boiling alcohols.
10 Aeration of Processing Mixture
The aeration of the processing mixture is accomplished by introducing a gas
into the
mixture, in one embodiment by mechanical mixing energy but also may be
achieved via other
physical or chemical means. The aeration may be accomplished by any suitable
mechanical
processing means, including but not limited to: (i) Batch tank aeration via
mechanical mixing
15 including planetary mixers or other suitable mixing vessels, (ii) semi-
continuous or continuous
aerators utilized in the food industry (pressurized and non-pressurized),
(iii) gas injection, (iv) gas
evolution via a pressure drop, or (v) spray-drying the processing mixture in
order to form aerated
beads or particles that can be compressed such as in a mould with heat.
In a particular embodiment, it has been discovered that the soluble porous
solids of the
20 present invention can be prepared within semi-continuous and continuous
pressurized aerators that
are conventionally utilized within the foods industry in the production of
marshmallows. Suitable
pressurized aerators include the Morton whisk (Morton Machine Co., Motherwell,
Scotland), the
Oakes continuous automatic mixer (E.T. Oakes Corporation, Hauppauge, New
York), the Fedco
Continuous Mixer (The Peerless Group, Sidney, Ohio), and the Preswhip
(Hosokawa Micron Group,
25 Osaka, Japan).
Forming the Aerated Processing Mixture
The forming of the aerated processing mixture may be accomplished by any
suitable means
to form the aerated processing mixture in a desired shape or shapes including,
but not limited to (i)
depositing the aerated processing mixture to specially designed moulds
comprising a non-interacting
30 and non-stick surface including TEFLON , metal, HDPE, polycarbonate,
neoprene, rubber, LDPE,
glass and the like; (ii) depositing the aerated processing mixture into
cavities imprinted in dry
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granular starch contained in a shallow tray (starch moulding forming technique
widely utilized in
the confectionery industry); or (iii) depositing the aerated processing
mixture onto a continuous belt
or screen comprising any non-interacting or non-stick material such as TEFLON
, metal, HDPE,
polycarbonate, neoprene, rubber, LDPE, glass and the like to form a shaped
aerated processing
mixture. Optionally, stamping, cutting or embossment of the shaped aerated
processing mixture
may occur.
Drying the Shaped Aerated Processing Mixture
The drying of the shaped aerated processing mixture may be accomplished by any
suitable
means including, but not limited to: (i) drying room(s) including rooms with
controlled temperature
and pressure or atmospheric conditions; (ii) ovens including non-convection or
convection ovens
with controlled temperature and optionally humidity; (iii) Truck/Tray driers,
(iv) multi-stage inline
driers; (v) impingement ovens; (vi) rotary ovens/driers; (vii) inline
roasters; (viii) rapid high heat
transfer ovens and driers; (ix) dual plenum roasters, (x) conveyor driers,
(xi) microwave drying
technology, and combinations thereof. Any suitable drying means that does not
comprise freeze-
drying can be used to form the soluble porous solid. If continuous shaping
processes are used, the
resulting soluble porous solid may be stamped, cut, embossed and/or stored in
roll form.
Optional ingredients may be imparted during any of the above described four
processing
steps or even after the drying process.
The soluble porous solids of the present invention may also be prepared with
chemical
foaming agents by in-situ gas formation (via chemical reaction of one or more
ingredients, including
formation of CO2 by an effervescent system).
Performance and Physical Characteristics
Dissolution Rate
The soluble porous solid may have a Dissolution Rate that allows the porous
solid to rapidly
disintegrate during use with the application with water. The Dissolution Rate
of the soluble porous
solid component is determined in accordance with the methodology described
below.
Hand Dissolution Method: Approximately 0.5g of the soluble porous solid is
placed in the
palm of the hand while wearing nitrile gloves. 7.5 cm3 of luke warm tap water
(from about 30 C to
about 35 C) is quickly applied to the product via syringe. Using a circular
motion, palms of hands
are rubbed together 2 strokes at a time until dissolution occurs (up to 30
strokes). The hand
dissolution value is reported as the number of strokes it takes for complete
dissolution or as 30
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strokes as the maximum (in the case for where the solid is considered non-
dissolving).
The soluble porous solids of the present invention have a hand dissolution
value of from
about 1 to about 30 strokes, in one embodiment from about 2 to about 25
strokes, in another
embodiment from about 3 to about 20 strokes, and in still another embodiment
from about 4 to
about 15 strokes.
Thickness
In one embodiment the soluble porous solid may be a flat, flexible substrate
in the form of a
pad, a strip or tape and having a thickness of from about 0.5 mm to about 10
mm, in one
embodiment from about 1 mm to about 7 mm, and in another embodiment from about
2 mm to
about 6 mm, as measured by the below methodology. In the case of cylindrical,
spherical, or other
objects with more of a third dimension versus a pad or strip, the thickness is
taken as the maximum
distance of the shortest dimension, i.e., the diameter of a sphere or cylinder
for instance, and the
thickness ranges are the same as described above.
The thickness of the soluble porous solid (i.e., substrate or sample
substrate) is obtained
using a micrometer or thickness gage, such as the Mitutoyo Corporation Digital
Disk Stand
Micrometer Model Number IDS-1012E (Mitutoyo Corporation, 965 Corporate Blvd,
Aurora, IL,
USA 60504). The micrometer has a 1 inch diameter platen weighing about 32
grams, which
measures thickness at an application pressure of about 40.7 phi (6.32 gm/cm2).
The thickness of the soluble porous solid is measured by raising the platen,
placing a section
of the sample substrate on the stand beneath the platen, carefully lowering
the platen to contact the
sample substrate, releasing the platen, and measuring the thickness of the
sample substrate in
millimeters on the digital readout. The sample should be fully extended to all
edges of the platen to
make sure thickness is measured at the lowest possible surface pressure,
except for the case of more
rigid substrates which are not flat. For more rigid substrates which are not
completely flat, a flat
edge of the substrate is measured using only one portion of the platen
impinging on the flat portion
of the substrate.
Basis Weight
The soluble porous solid may have a basis weight of from about 125 grams/m2 to
about
3,000 grams/m2, in one embodiment from about 150 grams/m2 to about 1,200
grams/m2, in another
embodiment from about 200 grams/m2 to about 1,000 grams/m2, and in still
another embodiment
from about 300 grams/m2 to about 800 grams/m2.
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The basis weight of the soluble porous solid is calculated as the weight of
the soluble porous
solid component per area of the selected soluble porous solid (grams/m2). The
area is calculated as
the projected area onto a flat surface perpendicular to the outer edges of the
porous solid. For a flat
object, the area is thus computed based on the area enclosed within the outer
perimeter of the
sample. For a spherical object, the area is thus computed based on the average
diameter as 3.14 x
(diameter/2)2. For a cylindrical object, the area is thus computed based on
the average diameter and
average length as diameter x length. For an irregularly shaped three
dimensional object, the area is
computed based on the side with the largest outer dimensions projected onto a
flat surface oriented
perpendicularly to this side. This can be accomplished by carefully tracing
the outer dimensions of
the object onto a piece of graph paper with a pencil and then computing the
area by approximate
counting of the squares and multiplying by the known area of the squares or by
taking a picture of
the traced area (which can be shaded-in for contrast) including a scale and
using image analysis
techniques.
Density
The soluble porous solid is characterized in terms of a density determination.
The density of
the soluble porous solid is determined by the equation: Calculated Density =
Basis Weight of porous
solid / (Porous Solid Thickness x 1,000), wherein the porous solid has a
density of from about 0.03
g/cm3 to about 0.4 g/cm3, in one embodiment from about 0.05 g/cm3 to about 0.3
g/cm3, and in
another embodiment from about 0.075 g/cm3 to about 0.2 g/cm3. The Basis Weight
and Thickness
of the soluble porous solid are determined in accordance with the
methodologies described herein.
Figures 1-3 exemplify desired densities herein rather than higher densities
that can be
exemplified in comparative densities in Figures 4-5.
Cell Inter-connectivity
The soluble porous solid may have a high degree of cell inter-connectivity,
i.e., are
predominantly open-celled solid foams as opposed to being predominantly closed-
cell solid foams.
The cell inter-connectivity can be assessed by cutting a 2-3 mm wide sliver of
the solid in the z-
direction using scissors or a sharp blade, measured across the normal x-y
largest surface of the solid,
and turning the resulting sliver by 90 degrees to reveal the internal cellular
structure of the freshly
cut cross-sectional area. This cross-sectional area can be assessed by close
visual inspection or,
more accurately, by employing magnification under a stereo microscope such as
the SZX12 Stereo
microscope available from Olympus Olympus America Inc., Center Valley, PA. The
open-celled
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soluble porous solids can easily be identified by examining the inner portion
of the cross-sectional
area which will comprise a predominantly three dimensional network of struts
with open void
spaces surrounding the struts that are inter-connected to one another
including in the third dimension
through the depth of the cross-section. In contrast, the inner cross-section
of a closed-cell foam will
appear as discrete bubbles that are cut across and then only being inter-
connected at the cross-
sectional surface in two dimensions by virtue of the cutting process employed
to generate the
exposed cross-sectional area.
Solid Flexibility and Cohesiveness
The physical integrity of the soluble porous solids (or solid cohesiveness) is
assessed via a
qualitative rating system by two separate qualitative ratings (1 to 4 scale)
on brittleness/flexibility
(brittle is breakable) and cohesiveness (ease in removing from moulds):
Brittleness/Flexibity Qualitative Rating
Very brittle = 1 Somewhat brittle = Somewhat flexible = Very flexible =
4
2 3
Cohesiveness Qualitative Rating (Ease of removal from moulds)
Very difficult = 1 Somewhat difficult Somewhat easy = 3 Very easy= 4
=2
These ratings are assessed on three dimensional moulds and resulting flat
solids with z-dimension
thicknesses between 3 mm and 10 mm and extending in the x-y dimensions
encompassing surface
areas of between 10 cm2 and 60 cm2 (with any x-y shape including circles,
ovals, squares, rectangles
etc.). The examples herein were evaluated employing circular Teflon moulds and
resulting removed
soluble porous solids with 4.15 cm diameters and depths of 0.7 cm. The
brittleness/flexibility rating
is judged by bending the soluble porous solid in pad form in half and
assessing each pad on its
propensity for breakage/creasing versus the pads resiliency and ability to
return to the original
shape. The cohesiveness rating is judged by peeling a freshly dried (after at
least 20 hours at 40
degrees Celsius) soluble porous solid from the mould and noting the difficulty
of removal. Solids
with low cohesiveness ratings are difficult to remove from the moulds in one
piece with significant
adhesion to the mould surface and with significant solid remaining adhered to
the mould after the
solid removal process. Soluble porous solids with high cohesiveness ratings
are easy to peel from
the moulds in one piece and without significant solid remaining adhered to the
mould after the
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soluble porous solid removal process.
Methods of Use
The soluble solid hair coloring article may be used for treating hair. The
soluble solid hair
coloring article may be used for whole head hair coloring, partial head hair
coloring such as root
5 touch up, highlights and lowlights.
The present application further covers a method of coloring hair comprising
the steps of
taking a soluble solid hair coloring article as described herein, preferably
such that the weight ratio
of direct dye to hair is about 2:1 to 5:1, such as 3:1 to 5:1, such as 4:1 and
exposing the soluble solid
hair coloring article to a solvent such that the soluble solid hair coloring
article dissolves to form a
hair coloring solution and then applying the hair coloring solution to hair.
Hair color refreshing may
be done at a neutral pH (pH about 7.0) while longer lasting hair coloring may
be done at a pH of
from about 7 to about 11, such as 10.
The exposure of the soluble solid hair coloring article may be to a solvent
such as water, a
solution of water and hydrogen peroxide, or a solution of water, hydrogen
peroxide, and a source of
ammonium ions.
The treatment steps also may further comprise working the hair coloring
solution into the
10 hair by hand or by a tool for a few minutes to ensure uniform
application to all of the hair. The hair
coloring solution remains on the hair while the end hair color develops for a
time period of 5 to 45
minutes, such as 30 minutes. The consumer then rinses his/her hair thoroughly
with tap water and
allows it to dry and/or styles the hair.
Examples
15 The following examples further describe and demonstrate embodiments
within the scope of
the present invention. The examples are given solely for the purpose of
illustration and are not to be
construed as limitations of the present invention, as many variations thereof
are possible without
departing from the spirit and scope of the invention. All exemplified amounts
are concentrations by
weight of the total composition, i.e., wt/wt percentages, unless otherwise
specified.
Example 1: Soluble Porous Solid
The following polyvinyl alcohol premix compositions (PVA premix) were prepared
for use
during the preparation of the soluble porous solids:
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Table 1
Component lA 1B
Distilled water 79.94 74.95
Polyvinyl alcohola 20.06 25.05
Total 100.0 100.0
a 87-89% hydrolyzed, MW 85,000 to 124,000 ex. Celanese
Into an appropriately sized and cleaned vessel, the distilled water is added
with stifling at
100-300 rpm. The polyvinyl alcohol is weighed into a suitable container and
slowly added to the
main mixture in small increments using a spatula while continuing to stir
while avoiding the
formation of visible lumps. The mixing speed is adjusted to minimize foam
formation. The mixture
is slowly heated to 85 C while continuing to stir approximately 30 minutes
and then allowed to cool
to room temperature (20 C). The hazy mixture is allowed to sit overnight
resulting in an amber
colored clear solution.
Example 2: Retail liquid hair conditioner product (Matrix Biolage)
Table 2
Component 2A 2B 2C 2D
PVA premix lA 54.88 -- 59.9 --
PVA premix 1B -- 44.00 -- 59.9
Matrix Biolagel 29.60 30.84 18.6 18.6
Tween 60K 5.93 5.94 4.1 4.1
Glycerine 3.71 3.73 1.2 1.2
Direct dye(s) 5.88 1.50 -- --
Ammonium chloride -- 0.40 -- --
Water -- To 100 To 100 To 100
1A liquid hair conditioner was purchased for use during the preparation of the
soluble porous solids
of the present invention. The product was Matrix Biolage Detangling Solution,
33.8 Fl. Oz., which
was distributed by Matrix LLC, New York, NY. The product was purchased in
February 2008 with
a lot number GC048. The listed ingredients on the bottle were: water, cetearyl
alcohol,
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behentrimonium methosulfate, cetyl alcohol, cyclopentasiloxane, behentrimonium
chloride,
phenoxyethanol, methylparaben, amodimethicone, fragrance, dimethiconol,
stearamine oxide,
propylene glycol, C11-15 pareth-7, C12-16 pareth-9, glycerin, trideceth-12,
polysorbate 20, citric
acid, sunflower extract, bitter almond kernel oil, wheat germ extract, hops
extract, ext. violet 2,
pollen extract, blue 1.
Example 3: Concentrated Conditioner Mix/BTMAC premix
Concentrated Conditioner Premix
Table 3
Component 3A
Wt%
Water 56.66
Behenyl trimethyl ammonium 11.39
chloride
Cetyl alcohol 7.34
Stearyl alcohol 18.57
Dissolvine EDTA acid 0.51
Sodium hydroxide (1%) 5.44
BTMAC premix
Table 4
Component 3B
Wt%
Water 59.94
Behenyl trimethyl ammonium 40.06
chloride
Table 5
Component 3C 3D 3E 3F
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PVA premix 1B 43.23 42.24 43.23 42.24
Concentrated 12.04 11.77 12.04 11.77
Conditioner Premix
(3A)
BTMAC premix 9.58 9.37 9.58 9.37
(3B)
Tween 60K 3.85 3.77 3.85 3.77
glycerine 4.26 4.17 4.26 4.17
Amino silicone -- 2.29 -- 2.29
(TAS)
PEG-90M' 3.88 3.79 3.88 3.79
Direct dye(s) 11.54 11.29 -- --
water To 100 To 100 To 100 To 100
1
PEG-90M: a 90% water, 10% PEG-90M mixture; POLYOXTM WSR-301 ex Dow Personal
Care
The above examples are prepared by mixing via a SpeedMixerTm DAC 400 FV
available
from FlackTek, Inc., Landrum, South Carolina. "A" grams of the above
components indicated in
Table 6 below in the given amounts are added into a Max 300 SpeedMixerTm
plastic jar with all
components being at room temperature. The mixture is thoroughly mixed within
the SpeedMixerTm
which is run at a range of approximately 2,750 rounds per minute for a time
period of at least 30
seconds.
Approximately "B" grams of the above mixture (indicated in Table 6) is
transferred into a 5
quart stainless steel bowl of a KitchenAid Mixer Model K555 (available from
Hobart Corporation,
Troy, OH) and fitted with a flat beater attachment. The mixture is vigorously
aerated at high speed
for approximately "C" minutes (indicated in Table 6). An aliquot of the
resulting aerated mixture is
then spread evenly with a spatula into a 19.4 ml circular Teflon mould (using
rubber spatulas
straight edge to scrape off excess foam leaving a flat smooth surface level
with the top of the mould)
which is weighed before and after with the wet mixture weight of "D" grams
(indicated in Table 6)
indicating a wet foam density of approximately "E" grams/cm3 (indicated in
Table 6).
The remainder of the aerated mixture is spread evenly with a spatula into
aluminum moulds
(each with inner dimensions of 15.9 cm x 15.9 cm x 0.6 cm) bottom-lined with
Bytac General
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Purpose film (Saint-Gobain, Paris, France). Each mould is placed into a 75 C
convection oven for
30 minutes. The moulds were then placed into a 45 C convection oven overnight.
Table 6
A grams B grams C minutes D grams E
grams/cm3
Example 2A 220.50 215 10 5.50 0.28
Example 2B 205.71 247 6 4.79 0.25
Example 3C 204.50 197 8 3.11 0.16
Example 3D 204.50 137 16 4.63 0.24
Hair Coloring and Color Refreshing with the Soluble Solid Hair Coloring
Article
Direct dye(s) incorporated into Soluble Solid Hair Coloring Article
1.5 grams of Piedmont white hair was exposed to a soluble solid hair coloring
article made from
Example 2A under the conditions indicated. The direct dyes used in Example 2A
were selected as
blue (CAS #904316-43-4), magenta (CAS #904316-50-3), and yellow (CAS #953082-
11-6). These
direct dyes are presented in a 1:1:1 ratio (or present in Example 2A in 1.96
wt%).
Exp. 1: dyeing under neutral conditions (pH 7): 1/4 soluble solid hair
coloring article of Example 2A
(15.9 cm x 15.9 cm x 0.6 cm), was combined with (1) 6 mL of water and
separately (2) 6 mL of 3%
of aqueous H202. The dissolved hair coloring article forms a hair coloring
solution that was then
applied on hair for 30 min at 30 C. Hair switches were then shampooed, rinsed
and dried for color
reading.
Exp. 2: dyeing at pH 10: 1/4 solid hair coloring article of Example 2A (15.9
cm x 15.9 cm x 0.6 cm)
was combined with (1) 6 mL of water and separately (2) 6 mL of 3% of aqueous
H202. The
dissolved hair coloring article forms a hair coloring solution that was then
applied on hair for 30 min
at 30 C. Hair switches were then shampooed, rinsed and dried.
Direct dye(s) encompassed by Soluble Solid Hair Coloring Article
Two soluble porous solids made according to Example 2D (totaling 1.2 grams)
may be used
to encompass 0.6 grams of direct dye. Direct dyes resulting in the brown
color, blue color, yellow
color and red color are as follows:
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Table 7
Dye Brown Blue Red Yellow
Bluequat bromide (CAS #502453- 0.02g 0.06 -- --
61-4)
orangey red (CAS #946602-30-8) 0.02 g -- 0.06 --
Yellow (CASE #68259-00-7) 0.02 g -- -- 0.06
The soluble solid hair coloring article was then dissolved in 6.0 grams of
water or in 2.88 grams of
water, 3.00 grams of Clairoxide 20 volume and 0.12 grams of ammonium hydroxide
(30% active).
5 The dissolved hair coloring article forms a hair coloring solution and
applied on hair for 30 min at
30 C. Hair switches were then shampooed, rinsed and dried.
Comparative Example for Density
The following solid does not have the desired density of the present
application and is
10 included only for comparative purposes:
Table 8
Component Wt%
Distilled water QS 100
Glycerin 1.0
Polyvinyl alcohol' 7.3
Sodium Laureth-3 sulfate (28% activity) 35.7
Sodium Lauryl sulfate (29% activity) 20.7
Cetyl alcohol 0.9
Cocamide MEA 1.5
Tetrasodium EDTA 0.04
Sodium benzoate 0.08
Kathon CG2 0.01
1 ___________________________________________________________________
CELVOL 523 available from Celanese Corporation (Dallas, Texas)
2 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazoliin-3-one
available from Rohm and Haas (Philadelphia, PA).
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Add into an appropriately sized and cleaned vessel, the distilled water and
glycerin with
stifling at 100-300 rpm. Weigh the CELVOL 523 into a suitable container and
add slowly to the
main mixture in small increments using a spatula while continuing to stir
while avoiding the
formation of visible lumps. Adjust the mixing speed to minimize foam
formation. Heat the mixture
slowly to 75 C then add the sodium laureth-3 sulfate and sodium lauryl
sulfate. Heat the mixture to
75 C and add the cetyl alcohol and cocamide MEA. Heat the mixture to 85 C
while continuing to
stir and then allow to cool to room temperature (35 C). Adjust the final pH is
between 5.2 - 6.6 with
citric acid or diluted sodium hydroxide if necessary. The viscosity of the
mixture should be
approximately 65,000 to 75,000 cps at 1 s-1.
Transfer 250 grams of the above mixture into a 5 quart stainless steel bowl of
a
KITCHENAID Mixer Model K5SS (available from Hobart Corporation, Troy, OH) and
fitted with
a flat beater attachment. Vigorously aearate the mixture at high speed for 30
seconds. Spread a
portion of the resulting aerated mixture with a spatula into 12 circular
Teflon moulds with a 4.2 cm
diameter and a depth of 0.6 cm which are weighed indicating an average wet
foam density of
approximately 0.31 grams/cm3. Aerate the remaining mixture again for an
additional 30 seconds for
a total of 60 seconds. Spread a portion of the resulting aerated mixture with
a spatula into 12
circular TEFLON moulds with a 4.2 cm diameter and a depth of 0.6 cm which are
weighed
indicating an average wet foam density of approximately 0.21 grams/cm3. Aerate
the remaining
mixture again for an additional 30 seconds for a total of 90 seconds. Spread a
portion of the resulting
aerated mixture with a spatula into 12 circular Teflon moulds with a 4.2 cm
diameter and a depth of
0.6 cm which are weighed indicating an average wet foam density of
approximately 0.19 grams/cm3.
Place the segregated moulds into a 75 C convection oven for 30 minutes and
then place into
a 40 C convection oven for drying overnight. The following day, remove the
resulting porous solids
from the moulds with the aid of a thin spatula and tweezers. The approximate
average density and
basis weight are as indicated in Table 3. The estimated surfactant levels are
between 50 wt% and 69
wt% and the estimated polymer level is between 20% and 27%, assuming a
moisture content of
between 0 wt% and 10 wt%.
Table 9
seconds mixing 60 seconds mixing 90 seconds
mixing
Density 0.21 grams/cm3 0.16 grams/cm3
0.13 grams/cm3
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WO 2013/176666
PCT/US2012/039161
52
Basis Weight 1,260 grams/m2 960 grams/m2
780 grams/m2
A micro computed tomography system image of the comparative example can be
seen in Figures 4
and 5 showing the physical distinction in density between the comparative
example and the claimed
ranges of density for the present application (See Fig. 1-3).
The dimensions and values disclosed herein are not to be understood as being
strictly limited
to the exact numerical values recited. Instead, unless otherwise specified,
each such dimension is
intended to mean both the recited value and a functionally equivalent range
surrounding that value.
For example, a dimension disclosed as "40 mm" is intended to mean "about 40
mm."
Every document cited herein, including any cross referenced or related patent
or application,
is hereby incorporated herein by reference in its entirety unless expressly
excluded or otherwise
limited. The citation of any document is not an admission that it is prior art
with respect to any
invention disclosed or claimed herein or that it alone, or in any combination
with any other
reference or references, teaches, suggests or discloses any such invention.
Further, to the extent that
any meaning or definition of a term in this document conflicts with any
meaning or definition of the
same term in a document incorporated by reference, the meaning or definition
assigned to that term
in this document shall govern.
While particular embodiments of the present invention have been illustrated
and described, it
would be obvious to those skilled in the art that various other changes and
modifications can be
made without departing from the spirit and scope of the invention. It is
therefore intended to cover
in the appended claims all such changes and modifications that are within the
scope of this
invention.
