Note: Descriptions are shown in the official language in which they were submitted.
2043~0~
ARTICLE FOR CONDmONTNG FABRI(-~
BA('T<(~R()UNl~ OF THF TNVENTION
Fn~T.n OF l~lE INVENTION
The instant invention relates to conditioning of fabrics in tumble-dryer
automatic dryers and, more particularly, to an article in the form of a
flexible substrate carrying a fabric ~nnfiitifming composition.
RFT ~TED ART
Silicones have been applied to fabrics during manufacture of fabrics or
during the make up of articles of clothing. With respect to application of
silicones to fabrics during a laundry process, Great Britain Patent
Application 1,549,480; Burmeister et al., U.S. Patent 4,818,242; Konig
~ ~ 2~43~03
- 2 - C6123
et al., U.S. Patent 4,724,089; Konig et al., U.S. Patent
4,806,255; Dekker et al., ~.S. Patent 4,661,267 and Trinh
et al., ~.S. Patent 4,661,269 describe aqueous
dispersions or emulsions of certain silicones of limited
viscosity incorporated in liquid rinse-cycle fabric
softening compositlons. A fabric softening composition
containing emulsified silicone is also taught by Barrat
et al. in U.S. Patent 4,446,033. Coffindafer et al.,
U.S. Patent 4,800,026 discloses fabric care compositions
containing curable amine functional silicones.
The application of fabric softeners to fabrics in the
tumble dryer by use of a flexible substrate carrying the
fabric softeners is known in the art. The advantages of
dryer added fabric conditioning include a more convenient
time of addition in the laundry process and avoidance of
undesirable interaction of softening agents with
detergents.
Rudy et al., ~.S. Patent 3,972, 131 discloses ~ryer
sheets including a silicone oil as an ironing aid.
Kasprzak et al., U.S. Patent 4,767,548 discloses the use
of certain silicones in dryer sheet formulations.
Coffindafer et al., U.S. Patent 4,800,026 discloses
curable amine functional silicones in fabric care
compositions.
In the manufacture of the dryer added fabric conditioning
sheets described in the references mentioned above, when
silicones are mixed with fabric softeners, the resulting
mixtures are non-homogeneous and phase separation occurs
readily. The homogeneity of such mixtures is ensured
only by continuous vigorous agitation. An additional
problem associated with the use of a nonhomogeneous
mixture is the separation of actives at the point of
~ 2~43503
- 3 - C6123
application of the active mixture on the substrate
resulting in unevenly impregnated sheets.
The compositions disclosed in the art contain individual
particles of a silicone and individual particles of a
fabric softening agent.
In the present invention the dispersed particle is a
composite particle containing a mutually compatible
mixture of a silicone and a fabric softening component.
Compatible organosilicones described herein preferably
form mutually soluble mixtures with certain types of
commonly used fabric softening agents. Critically, the
organosilicones in the dispersed composite particles do
not separate from fabric softening agents during
processing, on standing, during coating or drying of the
dryer sheet. An additional advantage afforded by the
present invention is a simplified manufacture of fabric
softener compositions since the silicones need not be
dispersed separately and can be introduced into the
composition simultaneously with a fabric softener.
Another advantage of using compatible silicones is that
compatible silicones enhance the spreading of the fabric
softening agents on the fabric surface as compared to the
spreading of the fabric softening agents alone or in
combination with incompatible silicones. As a result of
the use of compatible silicones as described herein
greater, more complete surface coverage by a fabric
softening agent is achieved with a further advantage of
smaller dosage re~uirements. Additionally, even and
uniform distribution of the actives on the dryer sheet
can be attained, alleviating the problem of unevenly
impregnated sheets.
4 ~043~03
It is an object of the invention to provide an article which provides for
release of a fabric conditioning composition within an automatic laundry
dryer, the composition containing a compatible mixture of a fabric
softening component and a selected organosilicone.
SUMMARY OF TH~ INVE~T~ON
The present invention is based, in part, on the discovery that specific
silicones, defined herein as compatible, are capable of forming compatible
mixtures with certain conventional fabric softening agents.
It is important to differentiate between compatible and incompatible
silicones and between mutually soluble and insoluble mixtures of
silicones and fabric softeners. Compatibility as taught herein is critical and
is ascertained by the appearance of the mixture of a silicone and a fabric
softener. When a silicon and a fabric softener are heated and mixed
together, the resulting liquid mixtures are either transparent or opaque. In
the transparent mixtures, silicone and fabric softener are mutually soluble
and are, accordingly suitable for use in the present invention. In the
opaque mixtures, silicone and fabric softener are mutually insoluble and
the mixtures may or may not form mutually stable dispersions. A
mutually stable dispersion is also compatible and is formed if a mixture of
a silicone and a fabric softener does not separate into more than one phase
on storage at elevated temperatures and if the mixture does not form a
uniform solid or liquid on cooling. Thus, the class of compatible mixtures
as defined herein includes mutually soluble mixtures as well as mutually
stable dispersions. Compatibility of the mixture is critical and is det-
ermined by the silicone softener compatibility test (SSCT) described below.
~0~35~1~
~ -5 -
According to the invention there is provided an article for t-~n~ k~nin~
fabrics, which provides for release of a fabric c nnfli~ ning culll,uosiLiull
within an automatic laundry dryer at dryer operating ~lllpt:laLulc~, the
article comprising a flexible substrate carrying thereon discrete composite
particles consisting of a ~ull~alil,lc mixture, as dPtPrminP~I by the
silicone/softener compatibility test of:
a) at least 1% of a fabric softening 1.:~ UI~JUllt~ CUlll,uli~illg a
cationic quatemary All.llll~llilllll salt; and
b) an orgAnocili( /-nP having a %CH2 content from 25% to 90%
and having at least one unit of Formula A:
Rl - si ~ ~(~-m) /2
R~
wherein m is a number from 0 to 2, R is a mono valent
hydrocarbon radical and Rl is
(i) a unit of Formula A1
-(CH2)a-(N-CH2CH2)b 1
R2 R2
wherein a is a number of at least 1, b is a number from 0 to 10, R2 is
-CH-CH-R3, R3 is
R4 OH
C
CA 02043~03 1998-01-08
-5a-
a hydrocarbon radical having from 4 to 40 carbon atoms
and R4 is hydrogen or a hydrocarbon radical having from
1 to 40 carbon atoms; or
(ii) a unit of Formula A2
-R7 - N ~ R5
I
R6
wherein R5 and R6 are independently selected from
hydrogen or a hydrogen radical having from 1 to 45
carbon atoms and at least one of R5 and R6 is a hydrogen
radical having from 6 to 45 carbon atoms, R7 is
R8 - CH - CH2 - , wherein R8 is a divalent
I
OH
organic radical having from 1 to 12 carbon atoms, in
which the weight ratio of organosilicone (b) to the fabric
softening component (a) is from 100:2 to 1:100.
The fabric softening component employed herein for
liquid compositions may be any commonly used fabric softening
agent complying with the above conditions provided that
CA 02043~03 1997-12-11
- 6 - C6123
it must include at least a portion of cationic quaternary
ammonium salts either used singly or, optionally, in
admixture with other softening agents such as nonionic
softeners selected from the group of tertiary amines
having at least one C8 30 alkyl chain, esters of
polyhydric alcohols, fatty alcohols, ethoxylated fatty
alcohols, alkyl phenols, ethoxylated alkylphenols,
ethoxylated fatty amines, ethoxylated monoglycerides,
ethoxylated diglycerides, mineral oils, polyols,
carboxylic acids having at least 8 carbon atoms, and
mixtures thereof.
The fabric conditioning composition employed in articles
of the present invention contains (A) certain fabric
softening agents used singly or in admixture with each
other and (B) an organosilicone having specific
structural requirements and a specific ~CH2 content.
DETAILED DESCRIPTION OF THE INVENTION
The fabric conditioning composition includes a cationic quaternary
ammonium salt. The counterion is methyl sulfate or any halide.
Examples of cationic quaternary ammonium salts include,
but are not limited to: -
1. Acyclic quaternary ammonium salts having at leasttwo C8 to C30, preferably C12 to C22 alkyl chains, such
as: ditallowdimethyl ammonium chloride, di(hydrogenated
tallow)dimethyl ammonium chloride, distearyldimethyl
ammonium chloride, dicocodimethyl ammonium chloride and
the like;
- . . 204~03
.
_ 7 -- C6123
2. Cyclic guaternary ammonium salts of the
imidazolinium type such as di (hydrogenated
tallow) dimethyl imidazolinium methyl sulfate,
l-ethylene-bis(2-tallow-l-methyl) imidazolinium methyl
sul~ate and the like
.
3. Diamido quaternary ammonium salts such as:
methyl-bis(hydrogenated tallow ~ ethyl)-2-hydroethyl
ammonium methyl sulfate,
methyl-bis (tallowamidoethyl) -2-hy-lr oxy~ropyl ammonium
methyl sulfate and the like;
4. Biodegradable quaternary ammonium salts such as
N, N-di (ta1lowoyl-oxy-ethyl) -N, N, -dimethy1 ammonium
chloride, and N,N-dittallowoyl-oxy-propyl)-N,N-dimethyl
ammonium chloride and the like. When fabric
conditioning compositions employ biodegradable guaternary
arlmonium salts, the pH of the composition is preferably
adjusted to between about 2 and about 5. Biodegradable
guaternary ammonium salts are described, for example, in
U.S. Patents 4,767,547 and 4,789,491.
5. Mixtures of water- insoluble cationic fabric
softeners and polyalkoxylated ammonium salts as described
in U.S. Patent 4,422,949. Suchmixturesare
particularly suitable for incorporation in concentrated form
of the liquid compositions herein.
The fabric softening component may include other fabric
softeners in addition to the cationic guaternary ammonium
salts. Additional fabric softeners suitable for use
herein can be selected from the following classes of
compounds:
~ ~.
CA 02043~03 1997-12-11
- 8 - C6123
i. Tertiary fatty amines having at least one and
preferably two C8 to C30, preferably C12 to C22 alkyl
chains. Examples include hardened tallow amine and
cyclic amines such as l-(hydrogenated
tallow)amidoethyl-2-(hydrogenated tallow) imidazoline.
Cyclic amines which may be employed for the compositions
herein are described in U.S. Patent 4,806,255,
ii. Carboxylic acids having 8 to 30 carbon atoms and one
carboxylic group per molecule. The alkyl portion has 8
to 30, preferably 12 to 22 carbon atoms. The alkyl
portion may be linear or branched, saturated or
unsaturated, with linear saturated alkyl preferred.
Stearic and myristic acids are preferred fatty acids for
use in the composition herein. Examples of these
carboxylic acids are commercial grades of stearic acid
and the like which may contain small amounts of other
acids.
iii. Esters of polyhydric alcohols such as sorbitan
esters or glycerol stearate. Sorbitan esters are the
condensation products of sorbitol or iso-sorbitol with
fatty acids such as stearic acid. Preferred
sorbitanesters are monoalkyl. A common example of
sorbitan ester is SPAN*60(ICI) which is a mixture of
sorbitan and isosorbide stearates.
iv. Fatty alcohols, ethoxylated fatty alcohols,
alkylphenols, ethoxylated alkyl phenols, ethoxylated
fatty amines, ethoxylated monoglycerides and ethoxylated
diglycerides.
v. Mineral oils, and polyols such as polyethylene
glycol.
~denotes trade mark
CA 02043~03 1997-12-11
- g - C6123
vi. Condensation products of higher fatty acids with
polyamines, selected from the group consisting of
hydroxyalkyl alkylene diamines, dialkylene triamines and
mixtures thereof, as described in U.S. Patent 4,661,269.
Preferred fabric softeners for use herein are acyclic
quaternary ammonium salts, ditallowdimethyl ammonium
chloride being most preferred for fabric conditioning
compositions of this invention. Especially preferred are
mixtures of ditallowdimethyl ammonium chloride with fatty
acids, particularly stearic acid or myristic acid.
About 1% to about 40% of the fabric softening component
is used in the compositions of the invention. There must
be included at least a sufficient amount of quaternary
ammonium salt to achieve anti-static effect, for example,
about 1% to 3% in the dilute product and about 2% to
about 5% in the concentrated product. On the other hand,
the entire fabric softening component may be quaternary
ammonium salt. The diluted version of the product
contains about 1% to about 12%, preferably about 3% to
about 10% and most preferably about 4% to about 7% of the
fabric softening component. The concentrated version of
the product contains about 13% to about 40%, preferably
about 13% to 30% and most preferably about 13% to about
20% of the fabric softening component.
When the fabric softening composition is carried on a
flexible substrate according to the article of the
present invention the fabric softening agents (A) include
conventionally used cationic and nonionic fabric
softening agents such as those listed in (1) to (5) and
(i) to (vi) above.
~ . 2~43~03
- 10 - C6123
The amount of the fabric softening composition on the
sheet is subject to normal coating parameters such as,
for example, viscosity and melting point of the fabric
softening components and is typically about 0.5 grams to
about 5 grams, preferably about 1 gram to about 3.5
grams. The fabric softening composition employed in the
present invention contains about 0.1% to about 95% of the
fabric softening ' ~n~nt. Preferably from about 10% to
about 80% and most preferably from about 30% to about 70%
of the fabric softening component is employed herein to
obtain optimum softening at minimum cost. When the
fabric softening component includes a quaternary ammonium
salt, the salt is used in the amount of about 10% to
about 80%, preferably about 30% to about 70%.
Silicone
The second essential ingredient of the fabric softening
composition employed in the present invention is a
compatible organosilicone.
The organosilicones employed in the present invention
(also termed herein as compatible silicones) are capable
of forming compatible mixtures with the fabric softeners
listed above.
The organosilicones employed herein have a %CH2 content
of about 25% to about 90%. The % CH2 content is defined
as
%CH2 = number of methylene (CH2) qroups x 100%
number of methylene groups and methyl groups
20~35~3
~ C6123
The organosilicones included in the fabric conditioning
compositions of the invention contain at least one unit
of Formula A:
R1 _ SiO(3-m)/2
Rm
wherein m is a number from o to 2 and R is a mono valent
hydro~lbo-- radical.
The value of (3-m)/2 in Formula A means the ratio of
oxygen atoms to silicon atoms, i.e. siOl/2 means one
oxygen is shared between two silicon atoms.
Rl in Formula A is selected from the group consisting of:
(i) a unit of Formula A1
( 2)a (N-CH2CH2)b - N-R2
R2 R2
wherein a is a number of at least 1, preferably 3; b is a
number from O to 10, preferably 1; R2 is -CH-CH-R ,
R4 OH
R3 is a hydrocarbon radical having from 4 to 40 carbon
atoms preferably from 8 to 18 carbon atoms and may be
saturated, unsaturated, cyclic, acyclic, alkyl or
~C
4 ~
- 204~3
- 12 - C6123
aromatic; and R4 is hydrogen or a hydrocarbon radical
having from 1 to 40 carbon atoms, preferably hydrogen;
and
(ii) a unit of Formula A2
-R7 - N - R
R6
wherein R5 and R6 are independently selected from
hydrogen or a hydrocarbon radical having from 1 to 45
carbon atoms which may be saturated, unsaturated, cyclic,
acyclic, alkyl or aromatic and at least one of R5 and R6
is a hydrocarbon radical having from 6 to 45 carbon
atoms, R7 is
_R8 _ CH - CH2 - , wherein R8 is a divalent organic
OH
radical having from 1 to 12 carbon atoms which may be
saturated, unsaturated, cyclic, acyclic, alkyl or
aromatic, and preferably is -CH2CH2CH2-O-CH2.
Thus, organosilicones employed in the present invention
include alkylsilicones and alkylaminosilicones which
satisfy the structural parameters described above and
which have % methylene (%CH2) content of about 25% to
about 90%. Compatibility of the organosilicones herein
with fabric softening agents depends, in part, on the
%CH2 content of the organosilicones. The preferred range
of the %CH2 content for the silicones herein is from
about 40% to about 90%, more preferably from about 50% to
about 85%, and most preferably from about 50% to about
2~3~3
- 13 - C6123
75~ to increase the degree of compatibility of the
mixtures containing relatively large amounts of silicone.
The organosilicones included in the compositions herein
may be linear, branched, or partially crosslinked,
preferably linear, and may range from fluid, liquid or
viscous liquid, gum and solid.
. ,~_
An example of an alkylsilicone suitable for use herein
is:
~CH3 IH3 IH3 IH3
H3 sio ~io sio si CH3
CH3 CH3 100 C18H3~ 10 3
An example of a suitable alkylaminosilicone containing
the unit of Formula A1 is:
~ 2043~03
- 14 - C6123
~ ,
lCH3 IH3 IH3 IH3
CH3 slo sio 1iO si - CH3
CH3 CH3 190 13H6 10 3
NCH2-CH-(cH2)l5cH3
OH
12H4
N
[CH2-CH-(CH2)l~cH3]2
OH
An example of an alkyIaminosilicone containing the unit
of Formula A2 is:
CA 02043~03 1997-12-11
.
- 15 - C6123
CIH3 IH3 fH3 IH3
CH3 SiO sio sio si CH3
CH3 CH3 200 (CH2)3 10 3
'1
CH2
I
CH-OH
I
H2
N - (C12H25)2
Alkylsilicones employed in this invention may be produced
by reacting a hydrosiloxane co-polymer with a hydrocarbon
having 6 to 45 carbon atoms and having a terminal vinyl
functionality. Such reactions are described, for
example, in Chemistry and Technology of Silicones by
Walter Noll, Academic Press, N.Y. (1968), pages 49-51 and
219-226. Commercially available alkylsilicones suitable
for use~herein are, for example, Masil~ 264, Masil~ 265,
Masil~ 265 HV from Mazer International Corp. or ABIL - Wax~
9800/or ABIL -Wax~ 9801 from Th. Goldschmidt AG.
Alkylaminosilicones employed in this invention may be
produced by 1) treating silicones containing primary or
secondary amine functional groups with epoxides such as
ethylene oxide to form alkylaminosilicones having the
unit of Formula Al, or 2) by treating epoxysilicones with
primary or secondary amines such as dicocoamine to form
alkylaminosilicones having the unit of Formula A2.
~denotes trade mark
CA 02043~03 l997-l2-ll
- 16 - C6123
The modified alkylaminosilicones of the invention having
the unit of Formula A1 may be prepared by mixing epoxide
compounds with aminosilicones in a pressure reactor and
heating for about 24 hours, after which the unreacted
epoxide compound is vacuum stripped off. The amount of
epoxide to be used is calculated based upon the number of
amine functional groups on the alkylaminosilicone.
Preferably, two epoxides are reacted for every primary
amine and one epoxide for every secondary amine, in order
to convert them to tertiary amines. A stoichiometric
amount or up to 2S% excess if epoxide can be used. The
reaction is preferably conducted between 25~C and 150~C,
especially between 50~C and 100~C. The pressure is
preferably maintained from 50 psi to 300 psi,
particularly from 50 psi to 150 psi. Typical
aminosilicone starting compounds would include Dow
Corning Q2-8075. The art of making alkylaminosilicones
having the unit of Formula A1 is disclosed in Examples 1
and 2 herein and in U.S. Patent No. 4,994,593 of Lin et al. entitled
'Hydroxylhydrocarbyl Modified Aminoalkyl Silicones'.
The modified alkylaminosilicones having the unit of
Formula A2 may be prepared by mixing epoxysilicones,
secondary amines, and a solvent such as isopropanol or
toluene, and heating the mixture at reflux for about 24
hours, after which the solvent is removed by distillation
or vacuum stripping. The amount of amine to be used is
calculated based upon the number of epoxy functional
groups on the epoxysilicone. Preferably, one secondary
amine is reacted for every epoxy functional group in
order to convert the amine to tertiary amine. A
stoichiometric amount or up to 25% excess of amine can be
used. The reaction is preferably conducted between 50~C
~ 20435~3
.
- 17 - C6123
and lS0~C, especially between 75~C and 110~C. The
reaction is preferably conducted at atmospheric pressure,
but may be conducted in a pressure reactor with the
pressure being maintained from 50 psi to 300 psi.
The modified alkylaminosilicones employed in this
invention contain amine groups which may be ~uaternised
with, for example, alkyl halide or methyl sulfate, or may
be protonated with a Lewis acid such as hydrochloric
acid, acetic acid, citric acid, formic acid and the like
Alkylsilicones and alkylaminosilicones employed herein
may, in addition to the units of Formula A, contain
secondary units selected from the group consisting of a
unit of Formula B1 and a unit of Formula B2:
R - O(CH2cHO)cR - (sio)3y/2 Formula B1
R Ry
R1 - ~(CH2CH2CH2CH~)d ~ R (SlO)3z/2 Formula B2
wherein Rll is a hydrocarbon radical having from 1 to 40
carbon atoms, preferably is CH3; R9 is a hydrocarbon
radical having from 1 to 3 carbon atoms; R10 is oxygen or
alkylene having from 1 to 8 carbon atoms, preferably
propylene; c and d are numbers from 0 to 50, preferably 2
to 15; and y and z are numbers from 0 to 2.
Organosilicones preferred for use herein have a %CH2
content of about 40% to about 90% and are either
alkylaminosilicones having the unit of Formula A1 or
alkylsilicones.
2~4~
- 18 - C6123
The amount of organosilicone employed herein generally
ranges from about 0.1% to about 20%, and is preferably at
least about 0.5~ to about 2% to m~im;~e the spreading of
the fabric softeners on fabric surface, but could be
higher in concentrated liquids. Preferably when the
organosilicone is carried on a substrate, the amount
employed is from 0.1% to 20%, more preferably at least 3%
to 20%. The amount of the organosilicone is governed by
the ratio at which the mutually soluble mixture of the
fabric softening component and the organosilicone is
formed.
The weight ratio of the organosilicone to the fabric
softening component in the fabric conditioning
compositions employed herein is from about 100:2 to about
1:100, preferably from about 2:100 to about 20:100, but
must be such that a compatible mixture can be formed.
Silicone/Softener Compatibility Test (SSCT)
As described above, mixtures defined as compatible herein
include mutually soluble as well as mutually stable
dispersible mixtures. Compatibility of the fabric
conditioning mixtures herein depends on the structure and
the %CH2 content of the organosilicone and the particular
fabric softeners employed in the mixture. SSCT provides
a basis for selecting appropriate combinations of the
fabric softening component and the organosilicone.
The test may be used to determine the compatibility at a
particular weight ratio of interest or to ~t~m; n~ a
minimum concentration of the silicone at which a
compatible mixture of the silicone and the fabric
softening component is formed.
~ 20435~3
- 19 - C6123
SSCT is conducted as follows:
a 10 gram sample of the fabric softener or a combination
of fabric softeners i8 placed into a clear glass flask
equipped with a stirring ---~h~n;~, such as a magnetic
stirrer. If either the fabric softener or the silicone
is a solid at room temperature, it is melted before the
test is begun with the test taking place above the
melting point of the fabric softener or the silieone.
The silicone of interest is slowly introduced with,
conveniently, a Pasteur pipet into the flask, with
stirring. It is estimated that the weight of one drop
represents about 1% silicone concentration, so the
silicone is mixed with the fabric softener 1% at a time.
Thus, the lowest concentration of the silicone in the
mixture is about 1~.
If the resulting mixture of the fabric softening agent
and the silicone stays clear over the entire investigated
range of the silicone, this indicates that the components
of the mixture are mutually soluble over the investigated
concentration range and, accordingly, are compatible.
Clear mixtures are defined herein as mixtures having
about 90% transmittance when measured with a visible
light probe (one centimeter pathlength) against distilled
water background using Brinkman PC800 colormeter.
The mixture may also become cloudy indicating that the
silicone and the fabric softener are not mutually soluble
at that weight % of the silicone. In this case, if the
mixture became cloudy, the weight percent of the silicone
added to produce cloudiness is calculatea. This number,
termed compatibility ~, then represents the weight
percent of the silicone to produce a clouay mixture.
Cloudy samples are placed in an oven at 100~C for at
least two hours, then cooled to room temperature and
~ ~43~
- 20 - C6123
inspected. Samples which have completely separated into
distinct layers are incompatible and are not useful for
the invention. Samples which maintain a stable,
dispersed character are c~patible and, hence, useful in
the invention.
It is sufficient, for practical applications, to
investigate the silicone concentration range of up to
about 30%. However, the entire range up to 100% of the
silicone concentration may be investigated if desired.
When the entire range of the silicone concentration is to
be investigated, the silicone is added until the mixture
contains about 60% by weight of the silicone. Silicone
addition is then stopped, and the experiment is repeated
by adding the fabric softener to a 10 gram sample of the
silicone. In those samples that became cloudy, the
weight percent of the softener added to produce
cloudiness is calculated and subtracted from 100, the
resulting number is termed herein compatibility ~.
~ compatibility reflects compatibility of the mixtures
containing a fabric softener as a major component,
whereas ~ compatibility reflects compatibility of the
mixtures containing a silicone as a major component.
Minimal difference between ~ and ~ ) reflects degree
of compatibility of the mixture: more compatible mixtures
have a lower number for p-~.
Preferably, the silicone and the fabric softening
component are compatible at a silicone concentration of
at least about 2%.
Mutually soluble and clear mixtures of the silicone and
the fabric softening component indicate the highest
degree of compatibility and are preferred.
~ ' 2~3~a3
- 21 - C6123
Various additives may be used in combination with the
compatible mixture of the fabric softening component and
the compatible silicone. The additives are used in the
amounts that do not substantially affect the
compatibility of the mixture and include small amounts of
incompatible silicones, such as pr~;n~ntely linear
polydialkylsiloxanes, e.g. polydimethylsiloxanes; soil
release polymers such as block copolymers of polyethylene
oxide and terephthalate; fatty amines selected from the
group consisting of primary fatty amines, secondary fatty
amines, tertiary fatty amines and mixtures thereof;
amphoteric surfactants; smectite type inorganic clays;
anionic soaps, switterionic quaternary ammonium
compounds; and nonionic surfactants.
other optional ingredients include emulsifiers,
electrolytes, optical brighteners or fluorescent agents,
buffers~ perfumes, colourants, germicides and
bactericides.
The fabric conditioning compositions of the invention can
be used in the rinse cycle of a conventional home laundry
operation. Generally, rinse water has a temperature of
from about 5~C to about 70~C. The concentration of the
total active ingredients is generally from about 2 ppm to
about 1000 ppm, preferably from about 10 ppm to about 500
ppm, by weight of the aqueous rinsing bath. When
multiple rinses are used, the fabric conditioning
composition is preferably added to the final rinse.
Additionally, an article is disclosed for conditioning
fabrics in a tumble dryer. The article of the invention
comprises a flexible substrate which carries a fabric
conditioning amount of a conditioning composition and is
capable of releasing the conditioning composition at
~ 2~43~3
- 22 - C6123
dryer operating temperatures. The conditioning
composition in turn has a preferred melting (or
softening) point of about 25~C to about lSO~C.
The fabric conditioning composition employed in the
invention is coated onto a dispensing means which
effectively releases the fabric conditioning composition
in a tumble dryer. Such dispensing means can be~designed
for single usage or for multiple uses. One such article
comprises a sponge material releasably enclosing enough
of the conditioning composition to effectively impart
fabric softeness during several drying cycles. This
multi-use article can be made by filling a porous sponge
with the composition. In use, the composition melts and
leaches out through the pores of the sponge to soften and
condition fabrics. Such a filled sponge can be used to
treat several loads of fabrics in conventional dryers,
and has the advantage that it can remain in the dryer
after use and is not likely to be misplaced or lost.
Another article comprises a cloth or paper bag releasably
enclosing the composition and sealed with a hardened plug
of the mixture The action and heat of the dryer opens
the bag and releases the composition to perform its
softening.
A highly preferred article comprises the compositions
containing a softener and a compatible organosilicone
releasbly affixed to a flexible substrate such as a sheet
of paper or woven or nonwoven cloth substrate. When such
an article is placed in an automatic laundry dryer, the
heat, moisture, distribution forces and tumbling action
of the dryer removes the composition from the substrate
and deposits it on the fabrics.
~ 20~3~3
- 23 - C6123
The sheet conformation has several advantages. For
example, effective amounts of the compositions for use in
conventional dryers can be easily absorbed onto and into
the sheet substrate by a simple dipping or padding
process. Thus, the end user need not measure the amount
of the composition necessary to obtain fabric softness
and other benefits. Additionally, the flat configuration
of the sheet provides a large surface area which.results
in efficient release and distribution of the materials
onto fabrics by the tumbling action of the dryer.
The substrates used in the articles can have a dense, or
more preferably, open or porous structure. Examples of
suitable materials which can be used as substrates herein
include paper, woven cloth, and non-woven cloth. The
term 'cloth' herein means a woven or non-woven substrate
for the articles of manufacture, as distinguished from
the term 'fabric' which encompasses the clothing fabrics
being dried in an automatic dryer.
It is known that most substances are able to absorb a
liquid substance to some degree; however, the term
'absorbent', as used herein, is intended to mean a
substrate with a absorbent capacity (i.e., a parameter
representing a substrate's ability to take up and retain
a liquid) from 4 to 12, preferably 5 to 7 times its
weight of water.
If the substrate is a foamed plastics material, the
absorbent capacity is preferably in the range of 15 to
22, but some special foams can have an absorbent capacity
in the range from 4 to 12.
2B43503
_ Z4 _ C6123
Determination of absorbent capacity values is made by
using the capacity testing procedures described in U.S.
Federal Specification (UU-T-595b), modified as folIows:
1. tap water is used instead of distilled water;
2. the specimen is immersed for 30 seconds instead of 3
minutes; ~
3. draining time is 15 seconds instead of 1 minute; and
4. the specimen is immediately weighed on a torsion
balance having a pan with turned-up edges.
Absorbent capacity values are then calculated in
accordance with the formula given in said Specification.
Based on this test, one-ply, dense bleached paper (e.g.,
Kraft or bond having a basis weight of about 32 pounds
per 3,000 square feet) has an absorbent capacity of 3.5
to 4; commercially available household one-ply towel
paper has a value of 5 to 6; and commercially available
two-ply household towelling paper has a value of 7 to
about 9.5.
Suitable materials which can be used as a substrate in
the invention herein include, among others, sponges,
paper, and woven and non-woven cloth, all having the
necessary absorbency requirements defined above.
The preferred non-woven coth substrates can generally be
defined as adhesively bonded fibrous or filamentous
products having a web or carded fibre structure (where
the fibre strength is suitable to allow carding), or
comprising fibrous mats in which the fibres or filaments
are distributed hapha2ardly or in random array (i.e. an
~ 2~3503
- 2~ - C6123
array of fibres in a carded web wherein partial
orientation of the fibres is frequently present, as well
as a completely h~ph~rd distribution orientation), or
substantially aligned. The fibres or filaments can be
natural (e.g. wool, silk, jute, hemp, cotton, linen,
sisal, or ramie) or synthetic (e.g. rayon, celloluse
ester, polyvinyl derivatives, polyolefins, polyamides, or
polyesters).
The preferred absorbent properties are particularly easy
to obtain with non-woven cloths and are provided merely
by building up the thickness of the cloth, i.e., by
superimposing a plurality of carded webs or mats to a
thickness adequate to obtain the necessary absorbent
properties, or by allowing a sufficient thickness of the
fibres to deposit on the screen. Any diameter or denier
of the fibre (generally up to about 10 denier) can be
used, ;n~smu~h as it is the free space between each fibre
that makes the thickness of the cloth directly related to
the absorbent capacity of the cloth, and which, further,
makes the non-woven cloth especially suitable for
impregnation with a composition by means of
intersectional or capillary action. Thus, any thickness
necessary to obtain the required absorbent capacity can
be used.
When the substrate for the composition is a non-woven
cloth made from fibres deposited haphazardly or in random
array on the screen, the articles exhibit excellent
strength in all directions and are not prone to tear or
separate when used in the automatic clothes dryer.
Preferably, the non-woven cloth is water-laid or air-laid
and is made from cellulosic fibres, particularly from
regenerated cellulose or rayon. Such non-woven cloth can
~3~3
- 26 - C6123
be lubricated with any standard textile lubricant.
Preferably, the fibres are from 5mm to 50mm in length and
are from 1.5 to 5 denier. Preferably, the fibres are at
least partially orientated h~ph~rdly, and are
adhesively bonded together with a hydrophobic or
substantially hydrophobic binder-resin. Preferably, the
cloth comprises about 70% fibre and 30% binder resin
polymer by weight and has a basis weight of from~about 18
to 45g per square metre.
In applying the fabric conditioning composition to the
absorbent substrate, the amount impregnated into and/or
coated onto the absorbent substrate is conveniently in
the weight ratio range of from about 10:1 to 0.5:1 based
on the ratio of total conditioning composition to dry,
untreated substrate (fibre plus binder). Preferably, the
amount of the conditioning composition ranges from about
5:1 to about 1:1, most preferably from about 3:1 to 1:1,
by weight of the dry, untreated substrate.
According to one preferred embodiment of the invention,
the dryer sheet substrate is coated by being passed over
a rotogravure applicator roll. In its passage over this
roll, the sheet is coated with a thin, uniform layer of
molten fabric softening composition contained in a
rectangular pan at a level of about 15g/square yard.
Passage of the substrate over a cooling roll then
solidifies the molten softening composition to solid.
This type of applicator is used to obtain a uniform
homogeneous coating across the sheet.
Following application of the liquefied composition, the
articles are held at room temperature until the
composition substantially solidifies. The resulting dry
articles, prepared at the composition substrate ratios
2~3~03
- 27 - C6123
set forth above, remain flexible; the sheet articles are
suitable for packaging in rolls The sheet articles can
optionally be slitted or punched to provide a
non-blocking aspect at any convenient time if desired
during the manufacturing process.
The following Examples will more fully illustrate the
~ nts of this invention. All parts, percentages
and proportions referred to herein and in the appended
claims are by weight of the composition unless otherwise
indicated.
Examples 1-6 include organosilicones within the scope of
the present invention having formulas A, B, C and D:
Formula A
iSi(CH3)3
(cH3)3s io ~ osi ( CH3)3
(CH2)3
N-[CH2-C~H (CH2)5 CH3]2
OH
Formula B
ICH3 CH3 lCH3 FH3
CH3_ sio~sio)~___(sio) 8 SiCH3
H3 3 (1CH2)3 CH3
N - CH2- CH - (CH2)9 - CH3
! OH
(CH2)2
~_[CH2-CH~ CH2~-CH3]2
OH
209L3~3
~
- 28 - C6123
Formula C
ICH3 ICH3
(CH3)3 si-o - (sio) lso (sio) lo si (CH3)3
CH3 (1CH2)3
N~CH2 CH-(CH2)15 CH3
¦ OH
(CH2)2
N-[CH2--ICH--(CH2)I3--CH3]2
OH
Formula D
o - si (CH3)3
1 3 1 3
(CH3)3 - =~sio_(sio) lo 4 sio - si (CH3)3
3 3
(CH2)3
~-CH2 CH ~ CH2)9 CH3
¦ OH
(lCH2)2
N-[CH2 CH-(CH2)9 CH3]2
OH
2~43~3
- 29 - C6123
~X~MPLE 1
The silicone of Formula C is a reaction product of the
starting aminosilicone (where the nitrogen-containing
branch chain is -(CH2)3-NH-(CH2)2NH2) and 1,2
epoxyoctadecane. The compound was prepared by placing
the starting aminosilicone (61.16g), 1,2 epoxyoct~ nP
(38.84g) and 2-propanol (60.0g) in a reaction vessel and
heating to 80~C for 24 hours. The reaction vessel
consisted of a three neck round bottom flask containing a
stirrer, a reflux condenser and a th~ ter. ~he
2-propanol was then stripped off with a N2 sparge at
100~C as described in the Lin et al. application
mentioned above.
Formula C silicone has ~CH2 equal 56.62.
~ 2~35~3
- 30 - C6123
EXAMPJ,~ 2 _ _ _ . _
A 'T' structure modified alkylaminosilicone of Formula D,
having %CH2 equal 52.50 was prepared. In the starting
Am;n~Alkylsilicone, the nitrogen-containing branch chain
is -(CH2)3-NH-(CH2)2NH2. In the modified
aminoalkylsilicone hydrogens on nitrogens were replaced
with -CH2CH-(CH2)9CH2. ..
OH
In the process, 34.7g of the starting ~m~nnAlkylsilicone,
34.4g 1,2-epoxydodecane and 17.4g 2-propanol were charged
to the reaction vessel ~ollowing the procedures of
Example 1.
CA 02043~03 l997-l2-ll
- 31 - C6123
EXAMPLE 3
Effect of the %CH2 content of various silicones as
indicated in Table I on the compatibility with Adogen~442
(dihydrogenatedtallow dimethyl ammonium chloride from
Sherex Corp.) was investigated by mixing the silicones
with Adogen 442, following the SSCT procedure.
The results that were generated are summarised in Table
I. Samples 6 and 7 were synthesised in Examples 1 and 2
respectively.
Table I
# Silicone%CH2 Compatible
1. ~ 2001* 0 no
2. DC SSF2* o no
3. Formula A 56.69 yes
4. Formula B 57.61 yes
5. Formula B, protonated57. 61 yes
6. Formula C 56.62 yes
7. Formula D 52.50 yes
1Linear polydimethylsiloxane, supplied by Dow Corning,
viscosity = lOOOcst
Aminosilicone supplied by Dow Corning, amine neutral
equivalent = 2000, viscsity - 130cst.
Silicones of samples 3 - 7 were mutually soluble with
Adogen 442 at silicone concentration of 5% by weight of
the mixture. However, silicone 1 and 2, which are not
within the scope of the present invention, were not
compatible with Adogen 442 at 5% or even at 25% of
silicone.
~denotes trade mark
~ 204~3
- 32 - C6123
~xamples ~-6 _~
Con~aç~ A~qle ~A~llremen~s
Contact angle values reflect the spreading behaviour of a
liquid on a solid surface. Discussion of the
relationship between contact angle values and spreading
is provided, for example, in Chapter 6 of "Introduction
to Colloid and Surface Chemistry", Duncan J. Shaw,
Butterworth, 1985. A contact angle of a liquid on solid
surface is the angle between the tangent of the droplet
and the surface. A smaller contact angle indicates
better spreading on the surface. When it is desired to
measure the contact angle on fabrics, there is an
experimental problem of accurately measuring the true
contact angle: due to the surface roughness of the fabric
it is difficult to obtain an accurate baseline. Thus,
the true contact angle measurements were obtained using
cellulose paper.
Samples were prepared by mixing a fabric softener and a
silicone above the melting point. A droplet of the melt
liquid was applied to a piece of cellulose filter paper.
After the droplet cooled and solidified, an initial
contact angle was measured. The cellulose paper with the
droplet was then placed in a 70~C oven for 30 minutes in
order for the equilibrium contact angle to be achieved.
The paper was then removed from the oven and a final
contact angle was measured.
The contact angle was measured using a contact angle
goniometer (Rame'-Hart model 100). The cellulose with
the drop of active was placed on the stage and viewed
with a microscope. With the light source on, the drop
appeared as a silhouette against a soft, green
~ 20435~3
_ 33 - ~ C6123
background. The drop/cellulose interface was aligned
with the horizontal crosshair, and the contact angle was
determined by rotating the read-out crosshair to tangency
with the drop right pro~ile. The contact angle value was
then read directly on the graduated goniometer scale.
This procedure was repeated to read the contact angle on
the left side_ Both sides should give the fiame reading
otherwise the sample was not levelled correctly and the
stage height should be readjusted.
~ 2~43~03
- 34 - C6123
~Y~nle 4
Effect o~ various silicones as indicated in Table II on
the spreading of Adogen 442 was investigated. The true
contact angle (initial and final) of the mixtures of
silicones and Adogen 442 prepared in Example 3 was
measured on cellulose paper as described above.
Additionally, spreading of the mixtures on cotton fabric
was evaluated qualitatively, using a score of 1 to 4: l =
best spreading, 2 = moderate spreading, 3 = droplet
starting to wet the surface, 4 = no spreading, droplet
beading up. Sample l contained only Adogen 442 without
any silicone and ~as used as a control.
The results that were generated are summarised in Table
II.
TABLE II
Sample Silicone Cotton Cellulose
No. Initial Final
.
1 none 4 110 112
2 DC200 4 110 147-
3 DCSSF 4 95 132
4 Formula A 1 70 18
Formula B 2-3 72 59
6 Formula B,
protonated 2 59 21
7 Formula C 2-3 86 57
8 Formula D 1 47 60
Initial and final contact angles for samples 4-8
containing compatible silicones within the scope of the
invention were lower than contact angles for samples 1-3.
~ . 2~43~3
_ 3~ _ C6123
Silicones of samples 4-8 were shown to form mutually
soluble mixtures with Adogen 442 in Example 3.
Samples 1-3 contained either no silicone or silicones
which are not within the scope of the invention. ~he
results established that, in mutually soluble mixtures of
compatible silicones and fabric softener as taught by the
present invention, compatible silicones improve-~he
spreading of the fabric softener on a cellulose surface.
Qualitative evaluation of spreading on cotton showed the
same pattern of improved spreading when compatible
silicones within the scope of the invention were used.
~ 2043503
- 36 - C6123
ExamPle 5
The concentration effect of various silicones as
indicated in Table III on the spreading of Adogen 442
fabric softener was investigated by measuring the contact
angle on a celIulose surface using the procedure
described above.
.
TABLE III ~: ~
Sample Silicone Final Contact Angle at % Silicone of
No. 1.5% 3.5% 7.5%
1 DC200 147 147 147
2 Formula B118 55
3 Formula B,
protonated48 20 20
4 Formula D 42 - 55
Formula D,
protonated98 78 5
This example demonstrates that in Samples 2-5 containing
organosilicones within the scope of the invention as
little as about 2% by weight of the mixture is needed to
reduce the contact angle to improve the spreading on the
surface.
Further increase in silicone concentration in Samples 2-5
further reduced the contact angle, indicating even better
spreading on the surface.
Silicone of sample l which is not suitable for the
present invention did not reduce the contact angle of the
fabric softener regardless of the amount of the silicone
used.
CA 02043~03 l997-l2-ll
- 37 - C6123
EXAMPLE 6
Mixtures of various silicones as indicated in Table IV
with nonionic fabric softeners, such as mineral oil were
investigated. The spreading of the mixtures on cotton
and polycotton fabrics was investigated by measuring the
fabric area (centimetres2) per gram of mineral oil spread
on the fabrics.
All sampples contained 5% by weight of the mixture of a
silicone. The mineral oil used was Semtol~ 350 from Witco
Corp.
TABLE IV
Sample Silicone Viscosity Surface Tension Fabric Area
No. (cst) (dyne/cm) Cotton Polycotton
none 105 32.0 303 371
2 Formula B 295 22.9 227 224
3 Formula D 182 22.2 326 552
Formula B silicone was only partially soluble in mineral
oil, while Formula D silicone formed a mutually soluble
mixture with mineral oil, demonstrating that the mutual
solubility of the silicones and fabric softeners depend
on the particular fabric softener as well as the %CH2 of
the silicone.
"denotes trade mark
2~435a3
~ '
- 38 - ~ C~123
Silicones B and D both reduced the surface tension of
mineral oil as observed in the absence of silicones in
sample l. However, fabric area coverage was increased
only in sample 3 where a mutually soluble mixture was
formed.
2~3503
~
_ 39 - C6123
EXAMPLES 7-8
Examples 7-8 include organosilicones within the scope of
the invention having formulas E, F and G.
Formula E
IH3 IH3 iH3 F 3
CH3- sio sio sio - si - CH3
CH3 3 100 (I 2)7 CH3
~ 3 ~10
Formula F
~ , ~
CIH3 CIH3 CIH3 ~CH3
CH - sio sio Isio *i CH
CH3 ~CH3~200 ~(1CH2)3~20 3
- CH2
CH - OH
'H2
~ _ (C12H25)2
Formula G
~ , ~
,CH3 CIH3 C~H3 CIH3
CH - sio sio - sio si - CH3
CH3 CH3 100 (CIH2)17 CH3
CH3 5
CA 02043~03 l997-l2-ll
_ 40 - C6123
EXAMPLE 7
The mutual solubility of organosilicones with mixtures of
fabric softening agents was investigated in the following
formulations:
Formulation Fabric Softening
No. Component Mixture .
10% varisoft 4751
10% Mineral Oil
II 10% Adogen 442
1% Myristic Acid
III 11.7% Varisoft~ 4452
3.5% Stearic Acid
1 Varisoft~ 475 = Methyl-l-tallowamidoethyl-2-tallOW
imidazolinium methyl sulfate
2 Varisoft~ 44S = Methyl-1-hydrogenated
tallowamidoethyl-2-tallow imidazolinium
methyl sulfate
The fabric softening mixtures of Formulations I, II and
III above were heated and melted at approximately 80~C.
Various silicones as indicated in Table V were added,
with stirring, until the resulting mixture became hazy.
At this point, the % silicone added was recorded as
solubility of the silicone in the formulation. The
results that were generated are summarised in Table V.
~denotes trade mark
~ 20~3503
~
- 41 - C6123
ABLE V
Formulation Silicone Solubility (%)
No. PDMS Silicone E Silicone F
I 0.26 1.28 4.70
II : 0.34 0 ~9 ~ 3_10
III 0.39 1.69 15.58
1PDMS - Polydimethylsiloxane, viscosity = 10,000 cst
Silicones E and F were significantly more soluble in
Formulations I, II and IrI than PDMS.
CA 02043503 1997-12-11
- 42 - C6123
Example 8
Various silicones within the scope of the invention as
indicated in Table VI were incorporated into liquid
fabric conditioning compositions. Fabric softening
agents and silicones were mixed together at 80~C (above
the melting point) and then dispersed into water at
60~C-80~C to form liquid compositions containing.
composite particles of the fabric softening component and
the silicone.
The resulting compositions are summarised in Table VI.
TABLE VI
Ingredients Sample A B C D E F G H
Adogen 442 7.37.3 - - - 13.3
Varisoft 475 - - 10 10 10 - - -
Varisoft 445 - - - - - - 11.7 11.7
Neodol* 23l 0.940.94 -
Siponic~ L7-90 0.940.94 -
Mineral Oil - - 10 10 10
Myristic acid - - - - - 1.25
Stearic acid - - - - - - 3.5 3.5
Silicone E 0.119 - 0.2 - - 0.131 0.213 -
Silicone G - 0.1 - 0.2
Silicone F - - - - 0.2 - - 1.9
Water 90.7 90.7 79.8 79.8 79.8 85.3 84.6
82.9
Neodol 23 = Lauryl alcohol
H25 (OCH2CH2)12OH, from Alcolac
~denotes trade mark
~ 2~3~03
_ 43 _ C6123
Samples C, D, E, G and H were further tested for their
softening properties. Terry cloths were prewashed with a
solution of Neodol 25-9 (alcohol ethoxylate from Shell
Corp.) and Na2C03 to remove textile finishes on the
surface, rinsed with the samples in a Tergometer and then
line-dried. The cloth load was 20g per litre and the
active concentration was O.lg per litre of rinse liquid.
The control was rinsed with only water. Using paired
comparison, a panel of 20 judges assessed the softness of
the treated cloth vs. control. All panelists preferred
the treated cloths over the control in all tests.
2Q4~3
- 44 - C6123
E~AMPLES 9-11
The compatibility of various fabric softening agents with
various silicones was det~rmin~d by the SSCT. The entire
concentration range up to 100% of the silicones was
investigated. Samples that ~. ;n~d clear over the
entire range of silicone concentration were labelled
'completely soluble'. For samples that became cloudy
stability of the dispersions was ascertained and ~ and
compatibility values were ~t~rm; n~d by the SSCT.
The silicones that were investigated are listed in Table
II. In the silicone formulas of Table II.
M = Me3SiO0 5,
D = Me2Si-O, D* = Me-Si-R' and R' is as indicated in
Table II.
Table II
Code Formula R' %CH2
AA Polydimethylsiloxane
( = 1000 cst) - o
BB MDlOOD*5M C8H17 14
CC* MDlOOD*5M C18H37 28
DD MD300D*20M 18 37 28
EE ~DlOOD*lOM C18H37 43
FF ~ :MD95D*24M C12H25 57
*Code CC, Formula MDlOOD*5M is equivalent to Formula G of
Example 8.
CA 02043~03 1997-12-11
- 45 - C6123
Example 9
In this example, mixtures of the silicones listed in
Table II with mineral oil were investigated using the
SSCT. The mineral oil used was Fished Light~ Mineral oil.
The results that were generated are summarised in Table
III.
Table III
Compatibility with Mineral oi 1
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATIBILITY (YEs/No)
AA 1 95 NO
BB 4 80 NO
CCCOMPLETELY SOLUBLE YES
EECOMPLETELY SOLUBLE YES
FFCOMPLETELY SOLUBLE YES
As determined by the SSCT, silicones CC, EE and FF having
the structural requirements and %CH2 recited by the
present invention form compatible mixtures with mineral
oil.
~denotes trade mark
2043503
'
- 46 - C6123
F~ le 10
In this example, mixtures of the silicones listed in
Table II with various cationic quaternary fabric
softening agents were investigated using the SSCT.
The results that were generated are summarlsed in Tables
IV, V and VI. ._
TABLE IV
Compatibility with Varisoft 137
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATIBILITY (YES/NO)
AA 2 97 NO
BB 2 98 NO
CC 2 9 6 NO
EE 7 9 3 YES
FF ~ 7 ~O YES
1Varisoft 137 = di(hydrogenated)tallow dimethyl ammonium
methylsulfate ~rom Sherex.
2043~3
- 47 - C6123
TABLE V _
Compatibility with Varisoft 4451
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATIBILITY (YES/NO)
AA 2 97 NO
EE ~ 10 97 YES
FF - 97 YES
~7arisoft 445 = di(hydrogenated)tallow imidazolinium
methylsulfate from Sherex.
TABLE V
Compatibility with Varisoft 110
SILICONE ~ ~ COMPATIBLE
CONPATIBILITY COMPATIBILITY (YES/NO)
AA 1 98 NO
EE ~ 5 90 YES
FF 5 90 YES
Varisoft 110 ~ methyl bis-(hydrogenated tallow
amidoethyl)
2-hydroxyethyl ammonium methylsulfate from Sherex
20435~3
S '
- 48 - C6123
ExamPle 11
In this example, mixtures of the silicones listed in
Table II with various nonionic fabric softening agents
were investigated using the SSCT.
Results that were generated are summarised in Table VII,
VIII, IX and X.
Table VII
Compatibility with Neodol 45_71
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATIBILITY (YES/NO)
AA 1 99 NO
BB 1 99 NO
DD 2 99 NO
FF 5 93 YES
1Neodol 45-7 = ethoxylated fatty alcohol from Shell.
2~43~a3
_ 49 - C6123
Table VIII
Compatibility with Adogen 345Dl
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATIBILITY (YES/NO)
A 2 60 NO
BCOMPLETELY SOLUBLE YES
DCONPLETELY SOLUBLE YES
ECOMPLETELY SOLUBLE YES
FCOMPLETELY SOLUBLE YES
1Adogen 345D = di(hydrogenated)tallow dimethyl amine from
Sherex.
Table IX
Compatibility with PEG 600
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATIBILITY (YES/NO)
AA 2 99 NO
BB 2 98 NO
DD 4 95 NO
EE 4 95 YES
FF 4 95 YES
1PEG 600 = Polyethylene Glycol
~ . 2~43503
- 50 - C6123
Table X
Compatibility with isostearic acid
SILICONE ~ ~ COMPATIBLE
COMPATIBILITY COMPATI8ILITY (YES/NO)
AA 3 95 NO
FF 3 ~ : 96 ~ YES
Examples 3-6 demonstrate that mutual compatibility
between the fabric softening component and
organosilicones may be easily ~f~r~;n~d by the SSCT and
that the compatibility depends on the structure and %CH2
content of the silicone as well as the particular fabric
softening component employed in the mixture. Although
silicone C was highly compatible (mutually soluble) with
mineral oil in Example 3 and with Adogen 345D in Example
6, it was less compatible with Varisoft 137 of Example 4,
i.e. a cloudy mixture was formed at 2~ of silicone.
However, silicone C was more compatible with Varisoft 137
in Example 4 than polydimethylsioxane, since ~
compatibility was lower for silicone C than for
polydimethylsiloxane. Results in Table VIII indicate
that amines have the highest degree compatibility with
organosilicones, since silicone B, which has the %CH2
content of 14% and is not within the scope of this
invention is still compatible with di(hydrogenated)tallow
dimethyl amine. Silicones E and F, having a high %CH2
content (43% and 57% respectively) were the most
compatible with all softeners tested.
~3~3
. ,
- 51 - C6123
EXAMPLE 12
Two fabric softening sheets, A and B were prepared as
follows:
The ingredients of a fabric conditioning composition as
listed below were mixed in the melt. 500g of the
prepared fabric conditioning mixture was placed in the
pan of a two-roll coating machine and coated onto a
spun-bonded polyester non-woven material. The fabric
softening articles thus manufactured contained about 1.6g
of solidified softening composition. The articles of
manufacture were then placed into a tumble dryer machine
which already contained 2.2 kg of prewashed clothing,
including terry towelling softness monitors. The fabrics
were then tumble dried with the fabric softening article
until dry and the softening benefit was evaluated by a 20
member panel.
Fabric Conditioning formulation for sheet A:
a. 10% of a silicone note suitable for use in the
present invention (silicone B from Table II)
b. 70% di(hydrogenated)tallow dimethyl ammonium
methylsulfate
c. 20% stearic acid.
Fabric Conditioning formulation for sheet B:
a. 7% of a silicone within the scope of this invention
(silicone FF from Table II)
b. 70% di(hydrogenated tallow dimethyl ammonium
methylsulfate
c. 23% stearlc acid.
~ ~ 2~43~3
- 52 - C6123
Observationq ;~n~l resl-lt5: . .
Sheet A - Due to the incompatible nature of the silicone,
the silicone separated from the softening component
during the coating process. The articles thus contained
unknown amounts of the silicone.
Sheet B - The compatible silicone of the invention and
the softening c , ~-~t formed a compatible mixture which
remained homogeneous during the coating process as it was
transferred to the substrate indicating that the
substrate was uniformly and evenly coated.
A 20 member panel judged the towelling monitors for both
sheet A and sheet B to have superior softness vs. towels
prepared in an identical fashion but dried without
softener.
This invention has been described with respect to certain
preferred embodiments and various modifications thereof
will occur to persons skilled in the art in the light of
the instant specification and are to be included within
the spirit and purview of this application and the scope
of the appended claims.
