Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
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FABRIC SOFTENER COMPOSITIONS
Field of the invention
The present invention relates to fabric softening compositions showing
excellent stability upon storage. More particularly, it relates to liquid fabricsoftening compositions.
Background of the invention
Fabric softening compositions, in particular fabric softening compositions to
be used in the rinse cycle of laundry washing processes, are well-known to
the consumer to provide fabrics with a soft and agreeable feeling. Such
compositions are provided in two forms: concentrated compositions
comprising more than 10% by weight of fabric softening agents and diluted
compositions comprising less than 10% by weight of fabric softening
agents.
Nevertheless, consumer acceptance of such compositions is determined not
only by the performance achieved with these products but also by the
aesthetics associated therewith. Viscosity of the product is therefore an
important aspect of the successful formulation of such commercial
products; stable medium to medium-high viscosities being highly preferred
by consumer. By medium-high viscosities, it is meant viscosities of 50cps
to 150cps when the fabric softening composition is in a diluted form and
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viscosities of 30cps to 90cps when the fabric softening composition is in a
concentrated form.
However, a problem encountered with diluted compositions is that, contrary
to concentrated compositions which exhibit a "self-building viscosity" due
to their high amount of active, diluted compositions show a phase
instability as well as a viscosity problem. Such a problem can be
encountered either with an already-made diiuted product or with a
concentrated product as it is diluted.
To this end, thickeners such as compounds of the polyacrylamide,
polysacharide or polyurethanes type have been widely used in such
compositions. Disclosure of such compounds may be found in EP
0,422,179 and EP 0,309,052. However, a problem encountered with such
thickeners is the necessity for them to be present at high levels to provide
effective thickening effect. Whilst the use of such high levels would
provide a good remedy to the problem, this would increase the formulation
cost.
Compounds of the associative polymeric type or cross-linked cationic
polymeric type are effective as thickeners, even at low levels. Disclosure of
such compounds may be found in EP 0,385,789 and EP 0,422,179.
However, the use of such compounds has been found to be detrimental to
the phase stability and viscosity performance of the product upon storage
and thus to the fabric softening performance of the product.
Not to be bound by theory, it is believed that such compounds are provided
with anionic charges which destabilise the formulation equilibrium.
The potential for such a problem is enhanced when the softening
composition comprises electrolytes.
The Applicant has now found that the addition of a component capable ofsequestering metal ions, preferably in specific amounts, overcomes the
problem.
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By thickener is meant a component which has thickening properties, that is
a compound which, when incorporated in a fabric softening composition,
produces compositions with a higher viscosity in the presence of the
polymer than in the absence of the polymer. Not included within the scope
of this term are components having soil release properties such as those
defined in US 4,702,857.
It is therefore an advantage of the invention to provide compositions with
good phase stability and viscosity.
It is another advantage of the invention to provide softening compositions
with an effective softness performance.
It is a further advantage of the invention to provide softening compositions
which allow the use of electrolytes without being detrimental to the
formulation equilibrate.
Summarv of the invention
The present invention relates to a liquid fabric softening composition
comprising:
a) from 0.01% to 10% by weight of a fabric softener component,
b) at least 0.001% of a thickening agent selected from the group
consisting of:
i~ associative polymers having a hydrophilic backbone and at least two
hydrophobic groups per molecule attached to the hydrophilic
backbone,
ii) cross-linked cationic polymers that are derivable from a water-
soluble cationic ethylenically unsaturated monomer or blend of
monomers which is cross-linked by 5 to 45ppm of a cross-linking
agent comprising polyethylenic functions, and
iii) mixtures thereof,
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c) a component capable of sequestering metal ions and selected from the
group consisting of:
i) chelating components selected from the group consisting of amino
carboxylic acid, organo aminophosphonic acid components, and
mixtures thereof,
ii) polycarboxylic building components, other than those defined under
i) as chelating components, comprising at least two carboxylic
radicals separated from each other by not more than two carbon
atoms, and,
iii) mixtures thereof .
Detailed descri~tion of the invention
Fabric softeners
An essential component of the invention is a fabric softener component.The fabric softening materials may be selected from the group consisting of
cationic, nonionic, amphoteric or anionic fabric softening material.
The fabric softener components herein are present at levels of from 0.01%
to 10% by weight, with a preferred level of fabric softening components
from 1% to 5% by weight of the composition.
Typically, such compositions contain a water-insoluble quaternary-
ammonium fabric softening active, the most commonly used having been di-
long alkyl chain ammonium chloride.
In recent years, the need has arisen for more environmentally-friendly
materials, and rapidly biodegradable quaternary ammonium compounds have
been presented as alternatives to the traditionally used di-long chain
ammonium chlorides. Such quaternary ammonium compounds contain long
chain alk(en)yl groups interrupted by functional groups such as carboxy
groups. Said materials and fabric softening compositions containing them
are disclosed in numerous publications such as EPA 040 562, and EPA 239
-91 O.
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The quaternary ammoniurn compounds and amine precursors herein have
the formula (I) or (Il), below:
R3~ R3
\ / + N -(CH,)n-CH ~ X -
-(C ~ ~-Q--T 1 X 13 Q Q
Rl Tl T'
or
(I) (Il)
Q is selected from the group consisting of -O-C(O)-, -C(O)-O-, -O-C(O)-O-, -
NR4-C(o)-, -C(o)-NR4-;
R 1 is (CH2)n-Q-T2 or T3;
R2 is (CH2)m-Q-T4 or T5 or R3;
R3 is C1-C4 alkyl or C1-C4 hydroxyalkyl or H;
R4 is H or C1-C4 alkyl or C1-C4 hydroxyalkyl;
T1, T2, T3, T4, T5 are independentlY C1 1-c22 alkyl or alkenyl;
n and m are integers from 1 to 4; and
X~ is a softener-compatible anion.
Non-limiting examples of softener-compatible anions include chloride ormethyl sulfate.
The alkyl, or alkenyl, chain T1, T2, T3, T4, T5 must contain at least 11
carbon atoms, preferably at least 16 carbon atoms. The chain may be
straight or branched.
Tallow is a convenient and inexpensive source of long chain alkyl and
alkenyl material. The compounds wherein T1, T2, T3, T4, T5 represents
the mixture of long chain materials typical for tallow are particularly
preferred .
Specific examples of quaternary ammonium compounds suitable for use in
the aqueous fabric softening compositions herein include:
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1) N,N-di(tallowyl-oxy-ethyl~-N,N-dimethyl ammonium chloride;
2) N,N-di(tallowyl-oxy-ethyl)-N-methyl, N-(2-hydroxyethyl) ammonium
chloride;
3) N,N-di(2-tallowyl-oxy-2-oxo-ethyl)-N,N-dimethyl ammonium chloride;
4) N,N-di(2-tallowyl-oxy-ethylcarbonyloxyethyl)-N,N-dimethyl ammonium
chloride;
5) N-(2-tallowyl-oxy-2-ethyl)-N-(2-tallowyloxy-2-oxo-ethyl)-N,N-dimethyl
ammonium chloride;
6) N,N,N-tri(tallowyl-oxy-ethyl)-N-methyl ammonium chloride;
7) N-(2-tallowyl-oxy-2-oxoethyl)-N-(tallowyl-N,N-dimethyl-ammonium
chloride); and
8) 1,2-ditallowyl-oxy-3-trimethylammoniopropane chloride; and mixtures of
any of the above materials.
Of these, compounds 1-7 are examples of compounds of Formula (I);
compound 8 is a compound of Formula (Il).
Particularly preferred is N,N-di(tallowyl-oxy-ethyl)-N,N-dimethyl ammonium
chloride, where the tallow chains are at least partially unsaturated.
The level of unsaturation of the tallow chain can be measured by the lodine
Value (IV) of the corresponding fatty acid, which in the present case should
preferably be in the range of from 5 to 100 with two categories of
compounds being distinguished, having a IV below or above 25.
Indeed, for compounds of Formula (I) made from tallow fatty acids having a
IV of from 5 to 25, preferably 15 to 20, it has been found that a cis/trans
isomer weight ratio greater than 30/70, preferably greater than 50/50 and
more preferably greater than 70/30 provides optimal concentrability.
For compounds of Formula (I) made from tallow fatty acids having a IV of
above 25, the ratio of cis to trans isomers has been found to be less critical
unless very high concentrations are needed.
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Other examples of suitable quaternary ammoniums of Formula (I) and (Il) are
obtained by, e.g.:
- replacing "tallow" in the above compounds with, for example, coco,
palm, lauryl, oleyl, ricinoleyl, stearyl, palmityl, or the like, said fatty acylchains being either fully saturated, or preferably at least partly
unsaturated;
- replacing "methyl" in the above compounds with ethyl, ethoxy, propyl,
propoxy, isopropyl, but,vl, isobutyl or t-butyl;
- replacing "chloride" in the above compounds with bromide, methylsulfate,
formate, sulfate, nitrate, and the like.
In fact, the anion is merely present as a counterion of the positively charged
quaternary ammonium compounds. The nature of the counterion is not
critical at all to the practice of the present invention. The scope of this
invention is not considered limited to any particular anion.
By "amine precursors thereof" is meant the secondary or tertiary amines
corresponding to the above quaternary ammonium compounds, said amines
being substantially protonated in the present compositions due to the
claimed pH values.
For the preceding biodegradable fabric softening agents, the pH of the
compositions herein is an essential parameter of the present invention.
Indeed, it influences the stability of the quaternary ammonium or amine
precursors compounds, especially in prolonged storage conditions.
The pH, as defined in the present context, is measured in the neat
compositions at 20 ~ C . For optimum hydrolytic stability of these
compositions, the neat pH, measured in the above-mentioned conditions,
must be in the range of from 2.0 to 4.5. Preferably, where the liquid fabric
softening compositions of the invention are in a diluted form, the pH of the
neat composition is in the range of 2.0 to 3Ø The pH of these
compositions herein can be regulated by the addition of a Bronsted acid.
Examples of suitable acids include the inorganic mineral acids, carboxylic
acids, in particular the low molecular weight (C1-Cs~ carboxylic acids, and
alkylsulfonic acids. Suitable inorganic acids include HCI, H2S04, HN03 and
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H3PO4. Suitable organic acids include formic, acetic, citric, methylsulfonic
and ethylsulfonic acid. Preferred acids are citric, hydrochloric, phosphoric,
formic, methylsulfonic acid, and benzoic acids.
Other fabric softening materials may be used in addition or alternatively to
the biodegradable fabric softener. These may be selected from the group
consisting of cationic fabric softening materials such as di-long alkyl chain
ammonium chloride, nonionic, amphoteric or anionic fabric softening
materials. Disclosure of such materials may be found in US 4,327,133;
4,421,792; 4,426,299; 4,460,485; 3,644,203 and 4,661,269.
Typically, such nonionic fabric softener materials have an HLB of from about
2 to about 9, more typically from about 3 to about 7. Such nonionic fabric
softener materials tend to be readily dispersed either by themselves, or
when combined with other materials such as single-long-chain alkyl cationic
surfactant described in detail hereinafter. Dispersibility can be improved by
using more single-long-chain alkyl cationic surfactant, mixture with other
materials as set forth hereinafter, use of hotter water, and/or more agitation.
In general, the materials selected should be relatively crystalline, higher
melting, (e.g. > 40 ~ C~ and relatively water-insoluble.
Preferred nonionic softeners are fatty acid partial esters of polyhydric
alcohols, or anhydrides thereof, wherein the alcohol, or anhydride, contains
from 2 to 18, preferably from 2 to 8, carbon atoms, and each fatty acid
moiety contains from 12 to 30, preferably from 16 to 20, carbon atoms.
Typically, such softeners contain from one to 3, preferably 2 fatty acid
groups per molecule.
The polyhydric alcohol portion of the ester can be ethylene glycol, glycerol,
poly (e.g., di-, tri-, tetra, penta-, and/or hexa-) glycerol, xylitol, sucrose,
erythritol, pentaerythritol, sorbitol or sorbitan. Sorbitan esters and
polyglycerol monostearate are particularly preferred.
The fatty acid portion of the ester is normally derived from fatty acids
~having from 12 to 30, preferably from 16 to 20, carbon atoms, typical
examples of said fatty acids being lauric acid, myristic acid, palmitic acid,
stearic acid and behenic acid.
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Highly preferred optional nonionic softening agents for use in the present
invention are the sorbitan esters, which are esterified dehydration products
of sorbitol, and the glycerol esters.
Commercial sorbitan monostearate is a suitable material. Mixtures of
sorbitan stearate and sorbitan palmitate having stearate/palmitate weight
ratios varying between about 10:1 and about 1:10, and 1,5-sorbitan esters
are also useful.
Glycerol and polyglycerol esters, especialiy glycerol, diglycerol, triglycerol,
and polyglycerol mono- and/or di-esters, preferably mono-, are preferred
herein (e.g. polyglycerol monostearate with a trade name of Radiasurf
7248).
Useful glycerol and polyglycerol esters include mono-esters with stearic,
oleic, palmitic, lauric, isostearic, myristic, and/or behenic acids and the
diesters of stearic, oleic, palmitic, lauric, isostearic, behenic, and/or myristic
acids. It is understood that the typical mono-ester contains some di- and tri-
ester, etc.
The "glycerol esters" also include the polyglycerol, e.g., diglycerol through
octaglycerol esters. The polyglycerol polyols are formed by condensing
glycerin or epichlorohydrin together to link the glycerol moieties via ether
linkages. The mono- and/or diesters of the polyglycerol polyols are
preferred, the fatty acyl groups typically being those described hereinbefore
for the sorbitan and glycerol esters.
Thickening agent
The second essential component of the invention is a thickening agent.
Typical ievels of such a thickener is of at least 0.001%, preferably from
0.001 to 3%, more preferably from 0.01% to 1% and most preferably from
0.1% to 0.5% by weight of the composition.
Suitable thickening agents are selected from the group consisting of
associative polymers having a hydrophilic backbone and at least two
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hydrophobic groups per moiecule attached to the hydrophilic backbone,
cross-linked cationic polymers that are derivable from a water-soluble
cationic ethylenically unsaturated monomer or blend of monomers which is
cross-linked by 5 to 45ppm of a cross-linking agent comprising
polyethylenic functions, and mixtures thereof.
Associative Polymers havinq a hvdroPhilic backbone and at least two
hvdrophobic qrouPs Per molecule attached to the hYdroPhilic backbone
It is believed that for associative polymers only polymeric molecules having
at least two hydrophobic moieties contribute to the thickening effect.
However, for practical purposes, generally, a reaction mixture of polymeric
molecules will be used, in that case it is not necessary that in such a
mixture the molecules contain on average two hydrophobic moieties;
satisfactory results can also be obtained when the average is less than two,
provided that a significant part of the molecules comprise two or more
hydrophobic moieties. It is however preferred that polymeric reaction
mixtures are used which comprise on average two or more hydrophobic
moieties per molecule.
The polymeric thickeners for use in fabric softener compositions according
to the invention preferably have a nonionic or cationic hydrophilic backbone.
Preferably the polymeric thickeners are hydrophobically modified nonionic
polymers.
Preferred hydrophobically modified nonionic polymers are based on
polyoxyalkylene or polyvinylalcohol hydrophilic backbones, to which a small
number of alkyl groups have been attached. Examples of these materials
are:
(i) copolymers of ethylene oxide and/or propylene oxide with small amounts
of Cg-C24 side chains, for instance having the basic formula:
[R4](4-x)-c-[cH2o-(cH(R5)-cH2o)y-cH(R6)-cH(R7)oH]x
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1 1
wherein each R4, independently, is a C 1 -C4 alkyl group, preferably a C2
alkyl group;
wherein each Rs, independently, is hydrogen or a methyl group;
wherein each R6, R7, independently, is selected from the group consisting
of H, a Cg-C24 alkyl group and a a Cg-C24 alkyl containing group,
preferably a C1 6 alkyl group or a C16 alkyl containing group; with the
proviso that for each chain, one of R6 or R7 is H and the other R6 or R7 is
a Cg-C24 alkyl group and a a Cg-C24 alkyl containing group, preferably a
C16 alkyl group or a C1 6 alkyl containing group.
wherein y is an integer Iying in the range of from 20 to 1000, preferably in
the range of from 50 to 500, more preferably in the range of from 200 to
400;
wherein x is an integer Iying in the range from 2 to 4 and preferably has the
value of 3.
Preferably, the above associative thickener has hydrophobic groups
constituting less than 10% by weight, preferably less than 6% by weight of
the polymeric material.
The associative thickeners of formula i) can be prepared by first reacting
ethylene oxide or propylene oxide and generally one lower alkylene oxide
with at least one active hydrogen-containing compound containing at least
one active hydrogen and subsequently or simultaneously reacting therewith
at least one long chain aliphatic alpha-olefin oxide or glycidyl ether. Said
long chain oxide or glycidyl ether has a carbon chain length of 8 to 24
aliphatic carbon atoms, preferably 12 to 18 carbon atoms. The proportion
of said alpha-olefin oxide or glycidyl ether present in the polyether thickener
is 1 to 20% by weight, based upon the total weight of the thickener.
Suitable active hydrogen-containing compound containing at least one
active hydrogen include monohydric and polyhydric alcohol initiators. Useful
polyhydric alcohol initiators are selected from the alkane polyols, alkene
polyols, alkyne polyols, aromatic polyols, and oxyalkylene polyols.
Monohydric alcohol initiators which are useful include aliphatic monohydric
alcohols and alkyl phenols containing 12 to 18 carbon atoms in the aliphatic
or alkyl group. In addition, aliphatic mercaptans having 12 to 18 carbon
atoms are useful initiators.
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12
A preferred example of thickener is the associative polymer of formula i),
whereby said thickener is a polymer with a central part made of
polyalkylene oxide chains ~80% ethylene oxide and 15% propylene oxide)
on which 5% hydrophobic chains (1,2-epoxyhexadecane) are branched.
Most preferably, the thickener of formula i~ is mixed with an ethoxylated
surfactant. In this case, the ethoxylated alcohols can vary in chainlength
and degree of ethoxylation or any mixtures thereof. A preferred example of
ethoxylated surfactant is Lutensol T08TM, a C1 3 ethoxylated alcohol with an
average ethoxylation grade of 8, available from BASF. The thickener of
formula i) and the ethoxylated surfactant are preferably present in a ratio of
polymer to Lutensol T08TM of 25:75.
A preferred example for preparing said thickener is as follows:
A liquid copolymer contaning 80 % by weight of the residue of ethylene
oxide, 15% by weight of the residue of 1,2-propylene oxide and 5% by
weight of the residue of an alpha-olefin oxide having an aliphatic carbon
chain length of 15 to 18 carbon atoms was prepared according to the
following procedure. A polyether derived from ethylene oxide and 1,2-
propylene oxide in the weight ratio of 75% ethylene oxide and 25% 1,2-
propylene oxide was prepared by reaction with trimethylolpropane in two
stages in a stainless steel auto clave. A first intermediate product was
prepared by reacting a mixture of trimethyiol, potassium hydroxide, 1,2-
propylene oxide, and ethylene oxide for a period of 18 hours at 1 20~C. The
final product was prepared in a second stage by reacting the previously
prepared intermediate with a mixture of 1,2-propylene oxide and ethylene
oxide under a nitrogent atmosphere of 115~ for 22 hours. The product had
a molecular weight of 23,000.
A glass flask was charged with 1410 grams of the final polyether product
prepared above and heated to 1 05~C while maintaining a nitrogen
-atmosphere. There was then added with stirring 10.2 grams of sodium and
the mixture reacted for a period of 24 hours. The intermediate product
obtained thereby was cooled to room temperature prior to further use.
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Thereafter, a 250ml centrifuge bottle was charged with 100grams of thisintermediate product together with 3.3 grams of 1,2-propylene oxide and
19 grams of ethylene oxide. The contents of the bottle were mixed at room
temperature and after the bottie was stoppered with a rubber stopper, the
bottle was placed in a steam b'ath for 24 hours. This product was cooled to
room temperature before further use. To the centrifuge bottle containing
this product, there was added 2.5 grams of an alpha-olefin oxide having an
aliphatic carbon chain length of 15 to 18 carbon atoms together with 3.3
grams of 1,2-propylene oxide and 19 grams of ethylene oxide. The
contents of the bottle were further mixed and the bottle was stoppered and
placed in a steam bath for 21 hours after which a viscous product was
obtained .
(ii) copolymers of ethylene oxide and/or propylene oxide with small amounts
of Cg-C24 side chains, for instance having the basic formula:
H0 - ( CH2CH20 ) n ( CpH2pcH2o ) m - CHCH20H
R2
wherein the group - (CH2CH20) n (CpH2pCH20 ) m - is substituted by a
minimum of two R1 groups which can be substituted at any CH2 group
along the polymer backbone;
(iii) Hydrophobically modified poly ~ethylene oxide and/or propylene
oxide/urethanes) for instance of the following formula:
rllo ~
R1 - N - C - ( CH2CH20 ) n ( CpH2pcH2o ) m - C - N - R1
wherein the group - (CH2CH20) n (CpH2pCH20 ) m - is substituted by a
minimum of two R 1 groups which can be substituted at any CH2 group
along the polymer baclcbone; and
(iv) alkyl substituted poly (vinyl~ alcohols, for instance of the following
formula:
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CH
HO - CH2 - ( CH2CH ) n - CH CH2 OH
I
R2
wherein the group - ( CH2CHOH) n - is substituted by a minimum of two
R1 groups which can be substituted at any CH2 group along the polymer
backbone; and
Wherein for formula (ii) to (iv):
n = greater than 10
p = 1 to 4 preferably 1 or 2
n + m = greater than 10
m = if p is greater than 1, m is such that the group involved constitutes
less than 50 mole %, preferably less than 25 mole % of the polymer.
R1 = a Cg-C24 linear or branched alkyl or alkenyl
R2 = hydrogen or a Cg-C24 linear or branched alkyl or alkenyl
R3 = a minimum of two R1 groups which can be substituted at any CH2
group along the polymer backbone.
Hydrophobically modified poly (ethylene oxide and/or propylene
oxide/urethanes) according to formula (iii) are marketed by UNION CARBIDE
under the UCAR SCT trademark for the thickening of latex systems and
generally have a molecular weight in the region of 40.000.
Preferably for the compounds of formula (ii) to (iv) the number of
hydrophobic groups attached to the hydrophilic backbone is relatively small.
Preferably, the hydrophobic groups constitute less than 5 % by weight of
the polymer, more preferably between 0. 5 and 2 % by weight of the
polymer. Preferred hydrophobic groups are linear or branched alkyl or
alkenyl groups, preferably having a chain length of less than 40, more
preferably between 8 and 24 carbon atoms.
Other preferred hydrophobically modified nonionic polymers based on
polyoxyalkylene hydrophilic backbones, to which a small number of alkyl
groups have been attached are the hydrophobically modified polyacrylic acid
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polymers such as the polyalkyl acrylic acid sold under the tradenames
Viscalex, Rheovis CRX, Rheovis CR, Rheovis CR2 available from Allied
Colloid, Acusol 810, Acusol 820, Acusol 823, Acusol 830, Acusol 842
available from Rohm & Haas.
The preferred molecular weight of the above mentionned thickener materials
to be used is preferably above 10 000 more preferred from 10 000 to 1
000 000 more preferred from 15 000 to 100 000, especially preferred from
20 000 to 70 000.
Cross-linked cationic polymers that are derivable from a water-soluble
cationic
ethvlenically unsaturated monomer or blend of monomers which is cross-
linked bv 5 to 45PPm of a cross-linkinq agent comPrising polvethvlenic
functions
The cross-linked, cationic polymers, (hereafter "CP"), are formed from
monoethylenically unsaturated monomer that is either a water soluble
cationic monomer or is a cationic blend of monomers that may consist of
cationic monomers alone or may consist of a mixture of cationic and non-
ionic monomers in the presence of a cross-linking agent. If a blend of
monomers is being used, then part of the blend may have a low water
solubility, providing the blend is water soluble. The monomers can be allyl
monomers but are generally vinyl, preferably acrylic.
Suitably, the cationic polymers are derivable from cationic monomers
comprising one or more of (a) dialkylaminoalkyl-acrylates or methacrylates,
~b) dialkylaminoalkyl-acrylamides or methacrylamides and (c) the quaternary
or acid salts of (a) or (b), for instance methacrylamidopropyl tremethyl
ammonium chloride and Mannich products such as quaternised
dialkylaminomethylacrylamides. Alkyl groups are generally C1 4 alkyl.
Suitable non-ionic monomers are acrylamide, methacrylamide, N-vinyl
pyrrolidone, and lower alkyl water insoluble acrylic (or other ethylenically
~ unsaturated) monomers such as methyl methacrylate, styrene or
acryloniltrile which may be included in sufficiently small amounts so that
the blend is soluble.
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Blends of 5-90%, preferably 5-60%, acrylamide with dialkylaminoalkyl-
acrylate or, preferably -methacrylate as acid addition or quaternary addition
salts, or, cationic homopolymers (containing no acrylyamide groups) are
preferred .
The monomers can contain hydrophobic groups, e.g. as described in EP-A-0,172,723, for instance on page 10 of that specification. If the monomer is
to impart insolubility to the polymer, ethoxy chains, if any, should be short
or absent, i.e., n=0. The allyl ether monomers are especially preferred.
The cationic polymer must be added while in the form of particles below 10
micrometers in size, and preferably below 2 micrometers in size. These can
be made by comminuting a cross-linked polymer gel but preferably the
particles are formed initially in the cross-linked state. The particles may be
added to the aqueous solution as disintegratable aggregates or pellets, but
preferably are added as dispersion in a liquid, generally a non-aqueous lic~uid
such as a hydrocarbon. This dispersion may be made by dispersing
preformed particles in the liquid but is preferably made by reverse phase
polymerisation of the monomer or monomer blend in the presence of the
cross linker.
The monoethylenically unsaturated starting material may be contaminatedwith a small amount of crosslinking agent and the amount of additional
cross-linking agent that is added will therefore be selected having regard to
this. Preferably the monoethylenically unsaturated material is as free of
cross-linking agent as is commercially possible, for instance containing
cross-linking agent in an amount that gives cross-linking or chain branching
less than is given by e.g. 1 ppm of a cross-linking agent comprising
polyethylenic functions used in the present invention. By the term
"polyethylenic functions" as used herein and throughout the specification is
meant cross-linking agents which have two or more ethylenically
unsaturated groups per molecule of the agent. Thus, an example of such an
agent is methylene bisacrylamide (hereafter "MBA"). The amount of cross-
linking agent with polyethylenic functions e.g. MBA that is added is at least
5 ppm and upto 45 ppm (based on monomer), generally from 10 to 40
ppm. The precise amount will depend upon the polymerisation and other
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processing conditions. Instead of using MBA, cross-linking may be equaily
achieved by using effective amounts of other diethylenically unsaturated
compounds such as ethylene glycol di-acrylate, diacrylamide,
cyanomethylacrylate, vinyloxyethylacrylate or methacrylate and other
means of cross linking, e.g. formaldehyde or glyoxal or metal salt addition.
Preferably a water-soluble cross-linking agent is used.
The degree of non-linearity can additionally be controlled by the inclusion of
chain transfer agents in the polymerisation mixture. Their use, in
combination with cross-linking agent, will tend to promote chain branching
rather than cross linking. Amounts may vary widely. For instance 1000 to
5000 ppm ~based on monomer) of a moderate chain transfer agent such as
isopropyl alcohol may be suitable whilst much lower amounts, typically 100
to 500 ppm, of more effective chain branching agents such as
mercaptoethanol are useful. Often, however, adequate results are obtained
by conducting polymerisation under conventional conditions without
deliberate addition of chain transfer agents using commercially pure
monoethylenically unsaturated monomer together with the specified amount
of MBA or other cross-linking agent.
Preferred CP's are often formed with up to 40% w/w acrylamide and 100
to 60% w/w dialkylaminoethyl methacrylate quaternary salt (for instance
20% acrylamide 80% dimethylaminoethyl methacrylate quaternary salt)
cross linked with 10 to 40 ppm, preferably 10-30 ppm of MBA or other
cross linker. All parts and percentages are by weight. The precise optimum
for any particular composition can be determined by observing the
properties of the composition when thickened with the chosen amount of a
range of CP's differing from one another solely by differing the amounts of
MBA from 5 to 45 ppm.
The polymerisation conditions are preferably such that the polymer has, if
uncross-linked, a notional high molecular weight of 5 million to 30 million
and an intrinsic viscosity (hereafter IV) of above 4, preferably above 6, e.g.,
up to 10 or 15 dl/g. If the polymer is cross linked (CP) it is preferably
polymerised such that it would have such molecular weight if it had been
made in the absence of cross linking agent. However, cross linking will
.. . .
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reduce the IV but the shearing may then cause the IV to increase, as
explained below.
The particle size in the emulsion of reverse phase polymerisation mixture
may be controlled by the degree of shear applied to the monomers and by
the possible presence of emulsifying agent. Emulsion polymerisation may
be utilised when polymerising, for instance, water insoluble monomers such
as acrylic esters or water insoluble but acid soluble monomers such as
amines (the resultant CP being distributed into acidic aqueous composition)
but generally reverse phase emulsion or suspension polymerisation is
utilised when the monomer or monomer blend is soluble in water. The
aqueous monomer is emulsified into a suitable non-aqueous liquid, generally
in the presence of a water in oil emulsifier, generally in an amount below
the critical micelle concentration. Emulsifiers, stabilisers, non-aqueous
liquids and other reverse phase polymerisation materials and process details
are described in, for instance, EP-A-0,126,528. The CP particles may be
dehydrated, for instance by subjecting the dispersion to azeotropic
distillation.
The liquid product from the reverse phase polymerisation or emulsion
polymerisation is generally used as such, without separation of the polymer
particles from it, but if desired dried polymer particles may be separated
from the dispersion in known manner. Because these dry particles will be
very dusty they should preferably be formed into pellets that will
disintegrate upon addition to water.
The polymer-in-oil emulsion that results from reverse phase polymerisation
may be added to the composition to be thickened in the presence of oil-in-
water emulsifier in conventional manner.
When the polymeric material is cross linked and cationic, and in particular
when it is a copolymer of acrylamide with at least 5%, and preferably at
least 10%, by weight dialkylamino alkyl acrylate (generally as acid addition
or quaternary ammonium salt) the degree of non-linearity is preferably such
that the CP has an ionic regain (IR) of at least 15%. IR is calculated as (x-
y/x)100 where x is the ionicity measured after applying standard shear and
y is the ionicity of the polymer before applying standard shear.
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These values are best determined by forming a 1% composition of the CP in
deionised water, allowing this to age for 2 hours and then further diluting it
to 0.1 % active CP. The ionicity of the CP, y, is measured by Colloid
Titration as described by Koch-Light Laboratories Limited in their publication
4/77 KLCD-1.
(Alternatively the method described in GB-A-1,579,007 could possibly beused to determine y). The ionicity after shear, x, is determined by
measuring by the same technique the ionicity of this solution after
subjecting it to standard shear.
The shear is best applied to 200ml of the solution in a substantially
cylindrical pot having a diameter of about 8cm and provided in its base with
a rotatable blade about 6cm in diameter, one arm of the blade pointing
upwards by about 45 degrees and the other downwards by about 45
degrees. The blade is about 1mm thick and is rotated at 16,500 rpm in the
base of the pot for 10 minutes. These conditions are best provided by the
use of a Moulinex homogeniser but other satisfactory conditions can be
provided using kitchen blenders such as Kenwood, Hamilton Beach, lona or
Osterizer blenders of a Waring Blender.
In practice, the precise conditions of shear are relatively unimportant since,
provided the degree of shear is of the same order of magnitude as specified,
it will be found that IR is not greatly affected by quite large changes in the
amount, for instance the duration of shear, whereas at lower amounts of
shear (for instance 1 minute at 16,500 rpm) IR is greatly affected by small
changes in shear. Conveniently therefore the value of x is determined at the
time when, with a high speed blade, further shear provides little or no
further change in ionicity. This generally requires shearing for 10 minutes,
but sometimes longer periods, e.g., up to 30 minutes with cooling, may be
desired .
The CP's used in the invention preferably have IR above 30%, often in the
range 35 to 45%. iR may increase from zero at zero cross linker up to peak
or plateau at a level around, for instance 10 to 25 ppm, cross linker and
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preferably IR is at or near this peak or plateau, generally at as low a level ofcross linking as is consistent with the high IR value.
A preferred example of a cross-linked polymer is as follows:
A reversed phase dispersion was formed by dispersing into a conventional
reverse phase non-aqueous liquid containing emulsifying agent and
amphiphatic stabiliser an aqueous monomer blend consisting of 80% by
weight dimethylaminoethyl methacrylate methyl chloride quaternary salt and
20% acrylamide and 15ppm methylene bis acrylamide. The mixture was
degassed and initiated in the conventional manner and polymerisation was
aliowed to go to completion. The mixture was then subjected to azeotropic
distillation to provide a substantially anhydrous dispersion of polymer
particles less than 2 micrometers in size dispersed in mineral oil (50%w/w)
which was Shell oil 60 Solvent Pale.
A preferred commercially representative of a cross-linked cationic polymer is
BP 7050TM ex BP Chemicals.
ComPonent caPable of sequestering metal ions
A third essential component of the invention is a component capable of
sequestering properties, that is a component which acts to sequester
~chelate) metal ions. Such compound may be selected from the group
consisting of a chelating component, a polycarboxylic building component
and mixtures thereof.
A. Chelating components
Chelating components are present at a level of at least 0.001% (lOppm),preferably in amount from 0.001% (10ppm) to 0.5%, more preferably from
0.005% to 0.25%, most preferably from 0.01% to 0.1% by weight of the
composition.
Suitable chelating components for use in the present invention are selected
from the group consisting of amino carboxylic acid, organo
aminophosphonic acid compounds, and mixture thereof.
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Chelating components, which are acidic in nature, having for example
phosphonic acid or carboxylic acid functionalities, may be present either in
their acid form or as a complex/salt with a suitable counter cation such as
an alkali or alkaline metal ion, ammonium, or substituted ammonium ion, or
any mixtures thereof. Preferably any salts/complexes are water soluble.
The molar ratio of said counter cation to the chelating component is
preferably at least 1:1.
Suitable chelating components for use herein include the amino carboxylic
acids such as ethylenediamine-N,N'-disuccinic acid (EDDS), ethylenediamine
tetraacetic acid (EDTA), N-hydroxyethylenediamine triacetic acid,
nitrilotriacetic acid (NTA), ethylene diamine tetrapropionic acid,
ethylenediamine-N,N'-diglutamic acid, 2-hydroxypropylenediamine-N,N'-
disuccinic acid, triethylenetetraamine hexacetic acid, diethylenetriamine
pentaacetic acid (DETPA), trans 1,2 diaminocyclohexane-N,N,N',N'-
tetraacetic acid or ethanoldiglycine.
Other suitable chelating components for use herein include the organo
aminophosphonic acids such as ethylenediamine tetrakis
(methylenephosphonic acid), diethylene triamine-N,N,N',N",N"-pentakis
(methylene phosphonic acid) (DETMP), 1-hydroxyethane 1,1-diphosphonic
acid (HEDP) or hydroxyethane dimethylenephosphonic acid.
Mixture of any of the herein before described chelating components can
also be used.
Especially preferred is ethylenediamine-N,N'-disuccinic acid (EDDS), most
preferably present in the form of its S,S isomer, which is preferred for its
biodegradability profile.
B Polycarboxylic building components
Polycarboxylic building components are present at a level of at least 0.01%
(10ppm), typically at a level of at least 0.045% (450ppm), preferably at a
level of from 0.045% to 0.5%, more preferably from 0.09% to 0.25%,
most preferably from 0.1% to 0.2% by weight of the composition.
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Suitable polycarboxylic buifding components for use herein can be
monomeric or oligomeric in type although monomeric polycarboxylates are
generally preferred for reasons of cost and performance.
Polycarboxylic acids containing two carboxy groups include succinic acid,
malonic acid, (ethylenedioxy) diacetic acid, maleic acid, diglycolic acid,
tartaric acid, tartronic acid and fumaric acid, as well as the ether carboxylic
acid and the sulfinyl carboxylic acids. Polycarboxylic acids containing three
carboxy groups include, in particular, citric acid, aconitric and citraconic as
well as succinic derivatives such as the carboxymethyloxysuccinic described
in British Patent No. 1,379,241, lactoxysuccinic described in British Patent
No. 1,389,732, and aminosuccinic described in Netherlands Application
7205873, and the oxypolycarboxylic materials such as 2-oxa-1,1,3-propane
tricarboxylic described in British Patent No. 1,387,447.
Polycarboxylic containing four carboxy groups include oxydisuccinic
disclosed in British Patent No. 1,261,829, 1,1,2,2-ethane tetracarboxylic,
1,1,3,3-propane tetracarboxylic and 1,1,2,3-propane tetracarboxylic.
Polycarboxylic containing sulfo substituents include the sulfosuccinate
derivatives disclosed in British Patent Nos. 1,398,421 and 1,398,422 and
in U.S. Patent No. 3,936,448, and the sulfonated pyrolysed citric described
in British Patent No.1,439,000.
Alicyclic and heterocyclic polycarboxylic include cyclopentane-cis,cis,cis-
tetracarboxylic, cyclopentadienide pentacarboxylic, 2,3,4,5-tetrahydrofuran
- cis, cis, cis-tetracarboxylic, 2,5-tetrahydrofuran - cis - dicarboxylic,
2,2,5,5-tetrahydrofuran - tetracarboxylic, 1,2,3,4,5,6-hexane
hexacarboxylic and carboxymethyl derivatives of polyhydric alcohols such
as sorbitol, mannitol and xylitol. Aromatic polycarboxylic include mellitic
acid, pyromellitic acid and the phthalic acid derivatives disclosed in British
Patent No. 1,425,343. Although suitable for use, citric acid is less
preferred for the purpose of the invention.
Of the above, the preferred polycarboxylic are carboxylic containing up to
three carboxy groups per molecule, more particularly maleic acid.
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Another ingredient of the invention is a liquid carrier. Suitable liquid carriers
for the present invention are selected from the group consisting of water,
organic solvents and mixtures thereof. The liquid carrier employed in the
instant compositions is preferably at least primarily water due to its low cost
relative availability, safety, and environmental compatibility. The level of
~ water in the liquid carrier is preferably at least 50%, most preferably at least
60%, by weight of the carrier. Mixtures of water and low molecular weight,
e.g., <200, organic solvent, e.g., lower alcohol such as ethanol, propanol,
isopropanol or butanol are useful as the carrier liquid. ~ow molecular weight
alcohols include monohydric, dihydric (glycol, etc.) trihydric (glycerol, etc.),and higher polyhydric (polyols) alcohols.
Octional comDonents
Surfactant concentration aids
Surfactant concentration aids may also optionally be used. Surfactant
concentration aids are typically selected from the group consisting of single
long chain alkyl cationic surfactants, nonionic surfactants, amine oxides,
fatty acids, and mixtures thereof, typically used at a level of from 0 to 15%
of the composition.
Single long chain alkyl cationic surfactants
Such mono-long-chain-alkyl cationic surfactants useful in the present
invention are, preferably, quaternary ammonium salts of the general formula
[R2N + R3] X~
wherein the R2 group is C10-C22 hydrocarbon group, preferably C12-C18
alkyl group of the corresponding ester linkage interrupted group with a short
alkylene (C1-C4) group between the ester linkage and the N, and having a
similar hydrocarbon group, e.g., a fatty acid ester of choline, preferably
C12-C14 (coco) choline ester and/or C16-C18 tallow choline ester at from
0.1% to 20% by weight of the softener active. Each R is a C1-C4 alkyl or
substituted (e.g., hydroxy) alkyl, or hydrogen, preferably methyl, and the
....
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counterion X~ is a softener compatible anion, for example, chloride, bromide,
methyl sulfate, etc.
Other cationic materials with ring structures such as alkyl imidazoline,
imidazolinium, pyridine, and pyridinium salts having a single C12-C30 alkyl
chain can also be used. Very low pH is required to stabilize, e.g.,
imidazoline ring structures.
Some alkyl imidazolinium salts and their imidazoline precursors useful in the
present invention have the general formula:
~C' \ X
I a
wherein y2 is -C(O)-O-,-O-(O)C-, -C(o)-N(R5)-, or-N(R5)-C(O)- in which R5
is hydrogen or a C1-C4 alkyl radical; R6 is a C1-C4 alkyl radical or H (for
imidazoline precursors); R7 and R8 are each independently selected from the
group consisting of R and R2 as defined hereinbefore for the single-long-
chain cationic surfactant with only one being R2.
Some alkyl pyridinium salts useful in the present invention have the general
formula:
R - N ~ X
wherein R2 and X- are as defined above. A typical material of this type is
cetyl pyridinium chloride.
Nonionic Surfactant (Alkoxylated Materials)
Suitable nonionic surfactants for use herein include addition products of
ethylene oxide and, optionally, propylene oxide, with fatty alcohols, fatty
acids, fatty amines, etc.
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Suitable compounds are substantially water-soluble surfactants of the
general formula:
R2 y - (C2H40)z - C2H4~H
wherein R2 is selected from the group consisting of primary, secondary and
branched chain alkyl and/or acyl hydrocarbyl groups; primary, secondary and
branched chain alkenyl hydrocarbyl groups; and primary, secondary and
branched chain alkyl- and alkenyl-substituted phenolic hydrocarbyl groups;
said hydrocarbyl groups having a hydrocarbyl chain length of from 8 to 20,
preferably from 1 0 to 1 8 carbon atoms.
Y is typically -O-, -C~O)O-, -C(O~N(R)-, or -C~O)N(R)R-, in which R2 and R,
when present, have the meanings given hereinbefore, and/or R can be
hydrogen, and z is at least 8, preferably at least 10-1 1.
The nonionic surfactants herein are characterized by an HLB (hydrophilic-
lipophilic balance) of from 7 to 20, preferably from 8 to 15.
Examples of particularly suitable nonionic surfactants include
- Straight-Chain, Primary Alcohol Alkoxylates such as tallow alcohol-
EO(11), tallow alcohol-EO(18), and tallow alcohol-EO(25);
- Straight-Chain, Secondary Alcohol Alkoxylates such as 2-C16EO(11); 2-
C2oEO(11); and 2-C16EO(14);
- Alkyl Phenol Alkoxylates, such as p-tridecylphenol EO(11 ) and p-
pentadecylphenol EO(18), as well as
- Olefinic Alkoxylates, and Branched Chain Alkoxylates such as branched
chain primary and secondary alcohols which are available from the well-
known "OXO" process.
Amine Oxides
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Suitable amine oxides include those with one alkyl or hydroxyalkyl moiety of
8 to 28 carbon atoms, preferably from 8 to 16 carbon atoms, and two alkyl
moieties selected from the group consisting of alkyl groups and hydroxyalkyl
groups with 1 to 3 carbon atoms.
Examples include dimethyloctylamine oxide, diethyldecylamine oxide, bis-(2-
hydroxyethyl)dodecylamine oxide, dimethyldodecyl-amine oxide,
dipropyltetradecylamine oxide, methylethylhexadecylamine oxide, dimethyl-
2-hydroxyoctadecylamine oxide, and coconut fatty alkyl dimethylamine
oxide.
Fatty Acids
Suitable fatty acids include those containing from 12 to 25, preferably from
16 to 20 total carbon a~oms, with the fatty moiety containing from 10 to
22, preferably from 15 to 17 (mid cut), carbon atoms.
Electrolvte Concentration Aids
The composition of the invention may also optionally comprise one or more
electrolytes. It has been found that where electrolytes concentration aids
were added to diluted softening compositions comprising thickeners but no
sequestering component, the problem of phase and viscosity instability upon
storage was increased. Surprisingly, compositions according to the
invention allow the use of electrolytes concentration aids and still exhibit
excellent phase and viscosity stability upon storage.
Electrolyte concentration aids, e.g. inorganic viscosity control agents, which
can also act like or augment the effect of the surfactant concentration aids,
include water-soluble, ionizable salts. These inorganic viscosity control
agents can also optionally be incorporated into the compositions of the
present invention. Incorporation of these components to the composition
must be processed at a very slow rate. A wide variety of ionizable salts can
be used. Examples of suitable salts are the halides of the Group IA and IIA
metals of the Periodic Table of the Elements, e.g., potassium chloride,
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calcium chloride, magnesium chloride, sodium chloride, potassium bromide,
and lithium chloride. The ionizable salts are particularly useful during the
process of mixing the ingredients to make the compositions herein, and later
to obtain the desired viscosity. The amount of ionizable salts used depends
on the amount of active ingredients used in the compositions and can be
adjusted according to the desires of the formulator. Typical levels of salts
used to control the composition viscosity are from 20 to 20,000 parts per
million (ppm), preferably from 20 to 11,000 ppm, by weight of the
composition.
Alkylene polyammonium salts can be incorporated into the composition togive viscosity control in addition to or in place of the water-soluble, ionizable
salts above. In addition, these agents can act as scavengers, forming ion
pairs with anionic detergent carried over from the main wash, in the rinse,
and on the fabrics, and may improve softness performance. These agents
may stabilise the viscosity over a broader range of temperature, especially at
low temperatures, compared to the inorganic electrolytes.
Specific examples of alkylene polyammonium salts include l-lysine
monohydrochloride and 1,5-diammonium 2-methyl pentane dihydrochloride.
Still other optional ingredients are stabilisers, such as well-known
antioxidants and reductive agents, Soil Release Polymers, emulsifiers,
bacteriocides, colorants, perfumes, preservatives, optical brighteners, anti
ionisation agents, antifoam agents and enzymes.
Optionally, sensitive ingredients such as perfumes or enzymes can be
isolated from their hostile environment by reversibly absorbing said
compounds into a porous hydrophobic material. In this way, the porous
hydrophobic material serves as a "cage" wherein the sensitive ingredient is
enclosed. Subsequently, the pores of the filled hydrophobic porous
material are sealed by dispersing said porous material into a hydrophobic
liquid.
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By sealing the pores of the hydrophobic material, the hydrophobic liquid
acts as a "shell", thereby protecting the sensitive ingredient from its
environment, reducing the loss of activity which could be encountered in
hostile environment and without reducing the ability of the sensitive
ingredient to perform its normal function. Exemplary disclosure of this
"shell and cage" system can be found in EP-A-0,~83,512.
The invention is illustrated in the following non-limiting examples, in which
all percentages are on a weight basis unless otherwise stated.
ExamDle 1
The following prior art fabric softening compositions 1 and 2 were prepared
Composition 1 Composition 2
DEQA (1) 20 18
Hydrochloric acid 0.02 0.02
Fatty acid (2) - 1.0
Perfume 1.0
Electrolyte (3~ 0.20 0.06
Silicon antifoam 0.01 0.01
Dye 0-005
Polyethylene Glycol 4000 1.0 0.60
Water and minors to balance to 100
( 1 ) Di-(tallowyloxyethyl~ dimethyl ammonium chloride
(2) Stearic acid IV=0
(3) Calcium chloride
These compositions were made according to a known process for preparingfabric softener compositions, e.g by injection into the hot water seat (60~-
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70~) containing minors the molten DEQA, followed by slowly adding the
electrolyte to the desired viscosity and thereafter the perfume before leaving
the product to cool.
The product of composition 1 was thereafter diluted 4 times and a thickener
as defined below under (5) was added while the product of composition 2
was diluted 2 times and the thickener BP7050TM ex BP Chemicals was
added. The resulting diluted fabric softener composition exhibited excellent
viscosity and phase stability on a freshly made product as well as upon
storage.
The diluted formulations were as follows:
Composition 3 Composition 4
Composition 1 25 50
Hydrochloric acid - -
maleic acid 1 200ppm
DETMP (4) - 750ppm
thickener (5) 0.25
BP7050TM (6) - 0 8
Dye - 7. 5ppm
perfume - 2.0
Water up to 100 up to 100
(4) diethylene triamine-N,N,N',N",N"-pentakis (methylene phosphonic
acid)
(5) copolymers of ethylene oxide and/or propylene oxide with small
amounts of Cg-C24 side chains as defined herein before with a central
part made of polyalkylene oxide chains t80% ethylene oxide and 15%
propylene oxide) on which 5% hydrophobic chains (1,2-
epoxyhexadecane) are branched, said copolymer being mixed with
Lutensol T08TM in a ratio of copolymer to Lutensol T08TM of 25:75.
(6) BP7050T~ ex BP Chemicals
