Technical Field
[0001] The present invention relates to a softening-through-the wash composition (STW-composition).
Background to the Invention
[0002] STW-compositions simultaneously clean and soften fabric during the washing stage
of the laundering process, negating the need to add a separate fabric-conditioning
composition to the rinse stage and/or drying stage of the laundering process. Therefore,
STW-compositions provide the consumer with an efficient and easy way to clean and
soften fabric during the laundering process.
[0003] Fabric-softening quaternary-ammonium di-ester compounds (di-ester-quats) are a known
means of softening fabric during the rinse stage and/or drying stage of the laundering
process. For example, rinse added and/or drier added compositions comprising di-ester-quats
are described in EP704522, EP720645, US4840738 and US6037315. In addition, US6093336
relates to a process for making a composition comprising a di-ester-quat and a fatty
acid. US6093336 discloses a process, which is said to produce compositions comprising
low amounts of impurities, and that are storage stable and non-caking. Also, WO94/07978
relates to compositions comprising a di-ester-quat and a hydroxy compound. The compositions
described WO94/07978 are said to have improved cold water dissolution and/or dispersability.
WO97/43367 relates to a detergent composition comprising a hard acid cationic component
and a hard base polymeric component. EP 240 727 and EP 309 052 relate to fabric softening
compositions.
[0004] However, prior to the present invention, detergent manufacturers were not able to
incorporate fabric-softening compounds such as di-ester-quats, in STW-compositions,
especially solid STW-compositions, without adversely affecting the fabric-cleaning
performance. Di-ester-quats, although capable of providing extremely good fabric-softening
properties during the rinsing and/or drying stage of the laundering process, cannot
be successfully incorporated into detergent compositions as they cause residues to
deposit on fabric during the laundering process and also reduce the soil removal performance
of the STW-composition. Thus, there is still a need to produce improved STW-compositions
having both a good fabric-softening performance and a good fabric-cleaning performance.
[0005] The inventors have surprisingly found that specific di-ester-quats, when used in
combination with a specific source of acid and clay, can be successfully incorporated
in STW-compositions. These specific di-ester-quats, when used in combination with
the specific source of acid and clay, greatly improve the fabric-softening performance
of the STW-composition without adversely affecting the fabric-cleaning performance.
Thus, the STW-compositions of the present invention have a surprisingly improved fabric-cleaning
and fabric-softening performance.
Summary of the Invention
[0006] In a first embodiment of the present invention, there is provided a softening-through-the-wash
composition comprising: (i) a fabric-softening quaternary ammonium di-ester compound
comprising a cationic quaternary ammonium component having the formula:

wherein, each R is independently selected from C
12-C
22 alkyl groups; and (ii) a source of acid selected from the group consisting of C
12-C
22 fatty acids, mono-alkyl esters of a C
12-C
22 alkyl sulphuric acids, C
11-C
13 alkyl benzene sulphonic acids, anionic derivatives thereof, salts thereof, and combinations
thereof; and (iii) clay; and (iv) one or more adjunct components.
[0007] In a preferred embodiment of the present invention, the composition is a solid softening-through-the-wash
detergent composition and the source of acid is selected from C
12-C
22 fatty acids, anionic derivatives thereof, and combinations thereof.
[0008] In a second embodiment of the present invention, there is provided a softening-through-the-wash
composition comprising: (a) a particle comprising: (i) a fabric-softening quaternary
ammonium di-ester compound comprising a cationic quaternary ammonium component having
the formula:

wherein, each R is independently selected from C
12-C
22 alkyl groups; and (ii) a source of acid selected from the group consisting of C
12-C
22 fatty acids, mono-alkyl esters of a C
12-C
22 alkyl sulphuric acids, C
11-C
13 alkyl benzene sulphonic acids, anionic derivatives thereof, salts thereof, and combinations
thereof; and (iii) optionally clay; and (iv) optionally one or more adjunct components;
and (b) one or more adjunct components, wherein the composition comprises clay.
[0009] In a third embodiment of the present invention, there is provided the use of the
above compositions to reduce creasing of fabric, and/or to soften fabric, and/or to
confer an ease of ironing benefit to fabric, and/or to confer an anti-static benefit
to fabric, and/or to reduce the fading of colour from fabric, and/or to confer a skin
moisturising benefit to fabric, and/or to removal soil from fabric, and/or to confer
a stain release benefit to fabric, and/or to soften fabric without hydrophobizing
the fabric.
Detailed Description of the Invention
Fabric-Softening Quaternary Ammonium Ester Compound
[0010] The STW-composition comprises a di-ester-quat. Preferably, the STW-composition comprises
(by weight of the composition) from 0.1% to 3 0%, preferably from 0.5%, or from 1%,
or from 1.5%, and preferably to 20%, or to 15%, or to 10%, or to 5%, or to 3% di-ester-quat.
The STW-composition may comprise (by weight of the composition) less than 5% di-ester
quat, or even less than 4%, or less than 3% di-ester quat.
[0011] Without wishing to be bound by theory, the inventors believe that the di-ester-quat
deposits on the fabric surface during the washing stage of the laundering process,
whereupon it lubricates the fabric fibres at or near the fabric surface, thus, softening
the fabric. In addition, the inventors believe that the di-ester quat interacts with
the source of acid and clay, such that the source of acid and clay are also deposited
on the fabric surface, the di-ester-quat may even act as a means to enhance the deposition
of the source of acid, and possibly the clay, on the fabric surface. The Inventors
believe that the deposition of the source of acid and clay on the fabric surface provides
some enhancement of the fabric-softening performance of the STW-composition. Furthermore,
the di-ester-quat, when present in combination with the source of acid and clay, is
surprisingly compatible with the adjunct component(s) of the STW-composition.
[0012] The di-ester-quat comprising a cationc quaternary ammonium component that is represented
by the formula:

wherein, each R is independently selected from C
12-C
22 alkyl groups. Preferably, each R is independently selected from C
13, or from C
14, or from C
15, or from C
16, and preferably to C
20, or to C
19, or to C
18, or to C
17 alkyl groups. Alternatively, it may be preferred that each R is independently selected
from C
12-C
15 alkyl groups. R may be a saturated alkyl group. Alternatively, R may be an unsaturated
alkyl group. R may be an unsaturated alkyl group having an iodine value of from 18-25.
A highly preferred di-ester-quat is dimethyl bis(steroyl oxyethyl) ammonium chloride.
[0013] The cationic quaternary ammonium component can optionally be in the form of a complex
with a counter-anion. Thus, the complex can represented by the formula:

wherein, each R is independently selected from C
12-C
22 alkyl groups as defined above, and X
- is a counter-anion. X
- may be any conventional counter ion. X
- is preferably an anion selected from the group consisting of halide, sulphate, sulphonate,
nitrate, carboxylate, carbonate, phosphate, phosphonate, borate, derivatives thereof,
and combinations thereof. Preferred halides and derivatives thereof are selected from
the group consisting of chloride, bromide, iodide, fluoride, and combinations thereof.
Preferred carboxylates and derivatives thereof are selected from the group consisting
of methanoate, ethanoate, propanoate, 2-hydroxypropane-1,2,3-tricarboxylate (citrate),
butanedicarboxylate (adipate), benzoate, and combinations thereof. A preferred sulphate
and derivative thereof is methyl sulphate. A preferred phosphate and derivative thereof
is hexafluorophosphate. A preferred phosphonate and derivative thereof is di-methyl
phosphonate. Preferably, X
- is an anion selected from the group consisting of chloride, bromide, methanoate,
ethanoate, sulphate, sulphonate, phosphate, phosphonate, and combinations thereof.
Most preferably, X
- is an anion selected from the group consisting of chloride, bromide, and combinations
thereof.
[0014] The di-ester-quat may be obtained by any conventional process. A preferred process
for obtaining a di-ester-quat, comprises the steps of: (i) reacting a di-alcohol secondary
and/or tertiary amine with a source of acid, wherein the source of acid is a C
12-C
22 fatty acid or an anionic derivative thereof, to form a di-ester secondary and/or
tertiary amine; and (ii) quaternising the di-ester secondary and/or tertiary amine
to form a di-ester-quat. Preferably, a catalyst is present during step (i) above.
Preferably, an excess of source of acid is present in step (i). Preferably a quaternising
agent is present in step (ii) above. A preferred quaternising agent is selected from
methyl chloride, methyl sulphate, methyl bromide, methyl iodide and combinations thereof.
A preferred quaternising agent is methyl chloride and/or methyl sulphate. Preferably
the quaternising agent is in the form of a gas. If the quatel-nising agent is methyl
chloride, then it may be preferred that an excess of quaternising agent is present
in step (ii). Optionally, an antioxidant is used in step (i) and/or step (ii). Typically,
step (i) and/or step (ii) are carried out at a high temperature. Typically, a high
temperature is a temperature above 95°C.
[0015] Optionally, a solvent is present in step (i) and/or step (ii). Preferred solvents
are selected from C
1-5 alcohols and isomers thereof. A preferred solvent is ethanol and/or isopropanol.
Preferably, the molar ratio of the di-alcohol secondary and/or tertiary amine to source
of acid is at least 2:1, more preferably at least 3:1.
Source of Acid
[0016] The STW-composition comprises a source of acid. Preferably, the STW-composition comprises
(by weight of the composition) from 0.1 % to 30%, preferably from 0.5%, and preferably
to 20%, or to 10%, or to 5% source of acid. Without wishing to be bound by theory,
the inventors believe that the source of acid, when in combination with the di-ester-quat
and clay, protects the di-ester-quat from interactions with the adjunct component(s)
of the STW-composition. In addition, the inventors believe that the source of acid,
especially when the source of acid is a C
12-C
22 fatty acid or even an anionic derivative of a C
12-C
22 fatty acid, deposits on the surface of the fabric, whereupon it lubricates the fabric
fibres at or near the fabric surface, thus, softening the fabric.
[0017] The source of acid is selected from the group consisting of: C
12-C
22 fatty acids, mono-alkyl esters of a C
12-C
22 alkyl sulphuric acids, C
11-C
13 alkyl benzene sulphonic acids, anionic derivatives thereof, salts thereof, and combinations
thereof. The term "anionic derivative" is typically intended to include dissociated
acids.
[0018] Preferably, the source of acid is selected from the group consisting of C
12-C
22 fatty acids, anionic derivatives thereof, salts thereof, and combinations thereof.
More preferably, the source of acid is selected from C
12-C
22 fatty acids, anionic derivatives thereof, and combinations thereof. Most preferably,
the source of acid is selected from C
12-C
22 fatty acids.
[0019] C
12-C
22 fatty acids can be represented by the formula:
R
1-COOH,
wherein, R
1 is a C
11-C
21 alkyl group. Salts of fatty acids can be represented by the formula:
R
1-COO
-M
+,
wherein, M+ is an alkali metal ion, preferably Na
+ and/or K
+, and R
1 is a C
11-C
21 alkyl group. Anionic derivatives of fatty acids can be represented by the formula
R
1-COO
-,
wherein, R
1 is a C
11-C
21 alkyl group.
[0020] Preferred sources of C
12-C
22 fatty acids are selected from the group consisting of: lauric acid, tridecylic acid,
myristic acid, pentadecylic acid, palmitic acid, margaric acid, stearic acid, arachidic
acid, phytanic acid, behenic acid, anionic derivatives thereof, salts thereof, and
combinations thereof. Most preferably, the source of acid is stearic acid.
[0021] Preferred sources of acid are C
12-C
22 fatty acids comprising a saturated alkyl group. Other preferred sources of acids
are C
12-C
22 fatty acids comprising an unsaturated group, typically having an iodine value of
from 15 to 25, preferably from 18 to 22.
[0022] The source of acid may be selected from the group consisting of palmitoleic acid,
oleic acid, elaidic acid, vaccenic acid, linoleic acid, cis-eleostearic acid, trans-eleostearic
acid, linolenic acid, arachidonic acid, anionic derivatives thereof, salts thereof,
and combinations thereof.
[0023] Preferred sources of fatty acids are selected from the group consisting of coconut,
soybean, tallow, palm, palm kernel, rapeseed, lard, sunflower, corn, safflower, canola,
olive, peanut, and combinations thereof. A highly preferred source of fatty acid is
tallow. Preferred fatty acids have a cis:trans isomer ratio of from 1:1 to 200:1,
preferably from 10:1 to 200:1. A preferred source of acid is hard tallow fatty acid
and/or partially hydrogenated tallow fatty acid.
[0024] The source of acid may be a C
11-C
13 alkyl benzene sulphonic acid. The source of acid may be an anionic derivative or
a salt of a C
11-C
13 alkyl benzene sulphonic acid.
[0025] The source of acid may be a mono-alkyl ester of a C
12-C
22 alkyl sulphuric acid. The acid source may be an anionic derivative or a salt of a
mono-alkyl ester of a C
12-C
22 alkyl sulphuric acid. A preferred source of a mono-alkyl ester of a C
12-C
22 alkyl sulphuric acid is tallow alkyl sulphate.
Cationic-Anionic Ion Pair Complex
[0026] If the source of acid is an anionic derivative of an acid selected from the group
consisting C
12-C
22 fatty acid, mono-alkyl ester of a C
12-C
22 alkyl sulphuric acid, C
11-C
13 alkyl benzene sulphonic acid, and combinations thereof, then it may be preferred
that the cationic quaternary ammonium component and source of acid are in the form
of a cationic-anionic ion-pair complex. The cationic-anionic ion pair complex can
be represented by the formula:

wherein, each R is independently selected from C
12-C
22 alkyl groups, and X
1- is an anionic derivative of an acid selected from the group consisting C
12-C
22 fatty acids, mono-alkyl esters of a C
12-C
22 alkyl sulphuric acids, C
11-C
13 alkyl benzene sulphonic acids, and combinations thereof.
[0027] Preferably, X
1- is represented by the formula:
R
1-COO
- or R
1-OSO
3-,
wherein, R
1 is a C
11-C
21 alkyl group. Most preferably, X
1- is represented by the formula:
R
1-COO
-,
wherein, R
1 is a C
11-C
21 alkyl group.
[0028] The cationic-anionic complex can be obtained by any conventional process. A typical
process involves the following four steps. 1. Esterification of an appropriate aminoalcohol
with fatty acid to give an esteramine. 2. Quaternization of the esteramine with a
suitable quaternizing agent in an alcoholic solvent. 3. Treatment of the alcoholic
quaternary solution with a fatty acid salt. 4. Removal of the resultant insoluble
inorganic salt.
[0029] Typically, the cationic-anionic complex is obtainable, preferably obtained, by a
process comprising the step of esterifying a quaternary ammonium compound having a
structure represented by the formula:

in the presence of an oxo acid of phosphorous and/or an alkali metal salt thereof
and/or an alkaline earth metal salt thereof, in the presence of a C
11-C
21 fatty acid, while removing at least part of the water that is produced by the esterification
reaction from the resulting mixture of esterification reaction products.
[0030] Typically, the molar ratio of C
11-C
21 fatty acid to quaternary ammonium compound is at least 1.5:1, and is preferably from
4:1 to 20:1, most preferably at least 15:1, and typically less than 100:1. Preferably,
the reaction is carried out at a temperature of at least 100°C, more preferably from
130°C to 220°C, or from 150°C to 170°C.
[0031] Preferably, at least 50% of the water, or even substantially all of the water present
after the esterification reaction, is removed from the resulting mixture of esterification
reaction products. The withdrawal of water from the resulting mixture of esterification
reaction products is typically achieved by using a vacuum and/or an appropriate water
trap, and results in an increase in the conversion efficiency of the esterification
reaction. Preferably, the process is performed in a vacuum, such as at a pressure
of 2x10
4Nm
-2 or less. Typically, the esterification reaction is carried out in a container having
a means for separating water, preferably having a water trap.
[0032] Preferred oxo acids of phosphorous are selected from group consisting of di-phosphoric
acid, metaphosphoric acid, polyphosphoric acid, phosphorous acid, phosphoric acid,
hypophosphorous acid, and combinations thereof. Preferred salts of oxo acids of phosphorous
are selected from the group consisting of: mono-sodium di-hydrogen hypophosphite,
sodium hypophosphite monohydrate, and combinations thereof. The oxo acid of phosphorous
and/or salt thereof may be in the form of a solution, preferably an aqueous solution.
The cationic-anionic complex can be obtained by the process described in US6093336
and US6166232.
[0033] The cationic-anionic complex may also be obtainable, preferably obtained, by a process
comprises the steps of: (i) obtaining a mixture comprising a solvent, a di-ester-quat
and a source of acid, wherein the di-ester-quat is in the form of a complex with a
counter-anion, and wherein the source of acid is a salt of one or more acids selected
from the group consisting of: C
12-C
22 fatty acid, mono-alkyl ester of a C
12-C
22 alkyl sulphuric acid, C
11-C
13 alkyl benzene sulphonic acid, and combinations thereof; and (ii) desalting the mixture
to form a cationic-anionic complex.
[0034] Preferred solvents are C
1-5 alcohols and isomers. Other preferred solvents are heptane and/or hexane. A highly
preferred solvent selected from methanol, ethanol, isopropanol, and combinations thereof.
Preferred processes for obtaining a mixture comprising a di-ester-quat and a source
of acid that can be used to obtain the mixture in step (i), are described in more
detail below. A preferred desalting means is selected from filtration, decanting,
sedimentation, extraction, centrifugation, and combinations thereof.
Clay
[0035] The STW-composition comprises clay. Preferably, the STW-composition comprises (by
weight of the composition) from 0.1% to 30%, preferably from 1%, or from 5%, and preferably
to 20%, or to 15%, or to 10%, or to 7% clay. The STW-composition may comprise (by
weight of the composition) less than 7% clay. The STW-composition may comprise (by
weight of the composition) 5% clay, or even greater than 5% clay. If the STW-composition
is a solid STW-composition, then preferably the STW-composition composition comprises
a detergent particle that comprises clay and an adjunct component selected from the
group consisting of wax, glycerol, flocculant, and combinations thereof. In another
preferred embodiment of the present invention, the STW-composition comprises a detergent
particle comprising clay or part thereof, the di-ester quat or part thereof, and the
source of acid or part thereof, and optionally other adjunct component(s) preferably
selected from the group consisting of flocculant, wax, glycerol, and combinations
thereof.
[0036] Preferably, the weight ratio of clay to di-ester quat is from 0.5:1 to 20:1, preferably
from 1:1 to 20:1, or from 1:1 to 10:1, or preferably greater than 1:1, or even greater
than 2:1. Preferably, the weight ratio of clay to the source of acid is from 1:1 to
50:1, preferably from 5:1 to 50:1, or preferably greater than 5:1. Preferably, the
weight ratio of clay to the combined weight of the di-ester quat and source of acid
is from 0.1:1 to 10:1, preferably from 1:1 to 5:1, or preferably greater than 1:1.
[0037] If the particulate solid STW-composition comprises a flocculant, then preferably
the weight ratio of clay to flocculant is from 5:1 to 100:1. In addition, preferably
the flocculant, or part thereof, and the clay, or part thereof, are comprised by the
same particle. Optionally, the particle comprises additional adjunct components, preferably
glycerol and wax.
[0038] Typically, the clay is selected from the group consisting of: allophane clays; chlorite
clays, preferred chlorite clays are amesite clays, baileychlore clays, chamosite clays,
clinochlore clays, cookeite clays, corundophite clays, daphnite clays, delessite clays,
gonyerite clays, nimite clays, odinite clays, orthochamosite clays, pannantite clays,
penninite clays, rhipidolite clays, sudoite clays and thuringite clays; illite clays;
inter-stratified clays; iron oxyhydroxide clays, preferred iron oxyhydoxide clays
are hematite clays, goethite clays, lepidocrite clays and ferrihydrite clays; kaolin
clays, preferred kaolin clays are kaolinite clays, halloysite clays, dickite clays,
nacrite clays and hisingerite clays; smectite clays; vermiculite clays; and mixtures
thereof.
[0039] Preferably, the clay is a smectite clay. Preferred smectite clays are beidellite
clays, hectorite clays, laponite clays, montmorillonite clays, nontonite clays, saponite
clays and mixtures thereof. Preferably, the smectite clay may be a dioctahedral smectite
clay. A preferred dioctahedral smectite clay is montmorillonite clay. The montmorillonite
clay may be low-charge montmorillonte clay (also known as sodium montmorillonite clay
or Wyoming-type montmorillonite clay). Typically, low-charge montmorillonite clay
can be represented by the formula:
Na
xAl
2-xMg
xSi
4O
10(OH)
2,
wherein, x is a number from 0.1 to 0.5, preferably from 0.2, and preferably to 0.4.
The montmorillonite clay may also be a high-charge montmorillonite clay (also known
as a calcium montmorillonite clay or Cheto-type montmorillonite clay). Typically,
high-charge montmorillonite clays can be represented by the formula:
Ca
xAl
2-xMg
xSi
4O
10(OH)
2,
wherein, x is a number from 0.1 to 0.5, preferably from 0.2, and preferably to 0.4.
[0040] Preferably, the smectite clay is a trioctahedral smectite clay. A preferred trioctahedral
smectite clay is hectorite clay. Typically, hectorite clay can be represented by the
following formula:
[(Mg
3-xLi
x)Si
4-yMe
III yO
10(OH
2-zF
z)]
-(x+y)((x+y)/n)M
n+,
wherein: y=0 to 0.4, if y=>0 then Me
III is AL, Fe or B, preferably y=0; and n is 1 or 2; and M
n+ is a monovalent (n=1) or a divalent (n=2) metal ion, preferably M
n+ is selected from the group Na, K, Mg, Ca and Sr; and x is a number from 0.1 to 0.5,
preferably from 0.2, or from 0.25, and preferably to 0.4, or to 0.35; and z is a number
form 0 to 2; and the value of x+y is the layer charge of the hectorite clay, preferably
the value of x+y is from 0.1 to 0.5, preferably from 0.2, or from 0.25, and preferably
to 0.4 or to 0.35.
[0041] Preferred hectorite clays have a cationic exchange capacity of at least 90meq/100g.
Typically, the cationic capacity of clays are measured by the method described in
Grimshaw, The Chemistry and Physics of Clays, 1971, Interscience Publishers Inc.,
pages 264-265. Especially preferred Hectorite clays are supplied by Rheox, and sold
under the tradenames "Hectorite U" and "Hectorite R".
[0042] The clay may be a light coloured crystalline clay mineral, preferably having a reflectance
of at least 60, more preferably at least 70, or at least 80 at a wavelength of 460nm.
Typically, the average particle size of the light coloured crystalline clay mineral
particles should not exceed 2µm, especially preferably not exceeding 1µm. The average
particle size of the light coloured crystalline clay mineral particles is typically
measured using a Malvern Zetasizer™, using a dispersion of the light coloured crystalline
clay at 0.1 g/l in deionised water, the clay being dispersed by vigorous agitation
for 1 minute. Preferred light coloured crystalline clay minerals are china clays,
halloysite clays, dioctahedral clays such as kaolinte, trioctahedral clays such as
antigorite and amesite, smectite and hormite clays such as bentonite (montmorillonite),
beidilite, nontronite, hectorite, attapulgite, pimelite, mica, muscovite and vermiculite
clays, as well as pyrophyllite/talc, willemseite and minnesotaite clays. Preferred
light coloured crystalline clay minerals are described in GB2357523A and WO01/44425.
[0043] The clay, in combination with the di-ester-quat and source of fatty acids, gives
a surprising fabric-softening performance, ease of ironing benefit, reduces creasing
of fabric, confers an ease of ironing benefit to fabric, confers an anti-static benefit
to fabric, reduces the fading of colour from fabric, confers a skin moisturising benefit
to fabric and improves the soil removal performance of the STW-composition.
Adjunct Components
[0044] The STW-composition comprises one or more adjunct components. Typically, the detergent
composition comprises from 10% to 99.7%, preferably from 25%, or from 50%, or from
75%, and preferably to 95% adjunct components. Preferred adjunct components are selected
from the group consisting of: anti-redeposition agents, bleaching agents, brighteners,
builders, chelants, dye-transfer inhibitors, enzymes, fabric-integrity agents, fillers,
flocculants, perfumes, soil release agents, surfactants, soil-suspension agents, and
combinations thereof.
[0045] A highly preferred adjunct component is a surfactant. Preferably, the STW-composition
comprises one or more surfactants. Typically, the STW-composition comprises (by weight
of the composition) from 0% to 50%, preferably from 5% and preferably to 40%, or to
30%, or to 20% one or more surfactants. Preferred surfactants are anionic surfactants,
non-ionic surfactants, cationc surfactants, zwitterionic surfactants, amphoteric surfactants,
catanionic surfactants and mixtures thereof.
[0046] Preferred anionic surfactants comprise one or more moieties selected from the group
consisting of carbonate, phosphate, sulphate, sulphonate and mixtures thereof. Preferred
anionic surfactants are C
8-18 alkyl sulphates and C
8-18 alkyl sulphonates. The C
8-18 alkyl sulphates and/or C
8-18 alkyl sulphonates may optionally be condensed with from 1 to 9 moles of C
1-4 alkylene oxide per mole of C
8-18 alkyl sulphate and/or C
8-18 alkyl sulphonate. The alkyl chain of the C
8-18 alkyl sulphates and/or C
8-18 alkyl sulphonates may be linear or branched, preferred branched alkyl chains comprise
one or more branched moieties that are C
1-6 alkyl groups. Other preferred anionic surfactants are C
8-18 alkyl benzene sulphates and/or C
8-18 alkyl benzene sulphonates. The alkyl chain of the C
8-18 alkyl benzene sulphates and/or C
8-18 alkyl benzene sulphonates may be linear or branched, preferred branched alkyl chains
comprise one or more branched moieties that are C
1-6 alkyl groups. Other preferred anionic surfactants are selected from the group consisting
of: C
8-18 alkenyl sulphates, C
8-18 alkenyl sulphonates, C
8-18 alkenyl benzene sulphates, C
8-18 alkenyl benzene sulphonates, C
8-18 alkyl di-methyl benzene sulphate, C
8-18 alkyl di-methyl benzene sulphonate, fatty acid ester sulphonates, di-alkyl sulphosuccinates,
and combinations thereof. The anionic surfactants may be present in the salt form.
For example, the anionic surfactant may be an alkali metal salt of one or more of
the compounds selected from the group consisting of: C
8-18 alkyl sulphate, C
8-18 alkyl sulphonate, C
8-18 alkyl benzene sulphate, C
8-C
18 alkyl benzene sulphonate, and combinations thereof. Preferred alkali metals are sodium,
potassium and mixtures thereof. Typically, the STW-composition comprises from 0% to
50% anionic surfactant.
[0047] Preferred non-ionic surfactants are selected from the group consisting of: C
8-18 alcohols condensed with from 1 to 9 of C
1-C
4 alkylene oxide per mole of C
8-18 alcohol, C
8-18 alkyl N-C
1-4 alkyl glucamides, C
8-18 amido C
1-4 dimethyl amines, C
8-18 alkyl polyglycosides, glycerol monoethers, polyhydroxyamides, and combinations thereof.
[0048] Preferred cationic surfactants are quaternary ammonium compounds. Preferred quaternary
ammonium compounds comprise a mixture of long and short hydrocarbon chains, typically
alkyl and/or hydroxyalkyl and/or alkoxylated alkyl chains. Typically, long hydrocarbon
chains are C
8-18 alkyl chains and/or C
8-18 hydroxyalkyl chains and/or C
8-18 alkoxylated alkyl chains. Typically, short hydrocarbon chains are C
1-4 alky chains and/or C
1-4 hydroxyalkyl chains and/or C
1-4 alkoxylated alkyl chains. Typically, the STW-composition comprises (by weight of
the composition) from 0% to 20% cationic surfactant.
[0049] Preferred zwitterionic surfactants comprise one or more quaternized nitrogen atoms
and one or more moieties selected from the group consisting of: carbonate, phosphate,
sulphate, sulphonate, and combinations thereof. Preferred zwitterionic surfactants
are alkyl betaines. Other preferred zwitterionic surfactants are alkyl amine oxides.
[0050] Typically, catanionic surfactants are complexes comprising a cationic surfactant
and an anionic surfactant. Typically, the molar ratio of the cationic surfactant to
anionic surfactant in the complex is greater than 1:1, so that the complex has a net
positive charge.
[0051] A preferred adjunct component is a builder. Preferably, the STW-composition comprises
(by weight of the composition and on an anhydrous basis) from 5% to 50% builder. Preferred
builders are selected from the group consisting of: inorganic phosphates and salts
thereof, preferably orthophosphate, pyrophosphate, tri-poly-phosphate, alkali metal
salts thereof, and combinations thereof; polycarboxylic acids and salts thereof, preferably
citric acid, alkali metal salts of thereof, and combinations thereof; aluminosilicates,
salts thereof, and combinations thereof, preferably amorphous aluminosilicates, crystalline
aluminosilicates, mixed amorphous/crystalline aluminosilicates, alkali metal salts
thereof, and combinations thereof, most preferably zeolite A, zeolite P, zeolite MAP,
salts thereof, and combinations thereof; layered silicates, salts thereof, and combinations
thereof, preferably sodium layered silicate; and combinations thereof.
[0052] A preferred adjunct component is a bleaching agent. Preferably, the STW-composition
comprises one or more bleaching agents. Typically, the STW-composition comprises (by
weight of the composition) from 1% to 50% of one or more bleaching agent. Preferred
bleaching agents are selected from the group consisting of sources of peroxide, sources
of peracid, bleach boosters, bleach catalysts, photo-bleaches, and combinations thereof.
Preferred sources of peroxide are selected from the group consisting of: perborate
monohydrate, perborate tetra-hydrate, percarbonate, salts thereof, and combinations
thereof. Preferred sources ofperacid are selected from the group consisting of: bleach
activators, preformed peracids, and combinations thereof. Preferred bleach activators
are selected from the group consisting of: oxy-benzene-sulphonate bleach activators,
lactam bleach activators, imide bleach activators, and combinations thereof. A preferred
source of peracid is tetra-acetyl ethylene diamine (TAED). Preferred oxy-benzene-sulphonate
bleach activators are selected from the group consisting of: nonanoyl-oxy-benzene-sulponate,
6-nonamido-caproyl-oxy-benzene-sulphonate, salts thereof, and combinations thereof.
Preferred lactam bleach activators are acyl-caprolactams and/or acyl-valerolactams.
A preferred imide bleach activator is N-nonanoyl-N-methyl-acetamide. Preferred preformed
peracids are selected from the group consisting of N,N-pthaloyl-amino-peroxycaproic
acid, nonyl-amido-peroxyadipic acid, salts thereof, and combinations thereof. Preferably,
the STW-composition comprises one or more sources of peroxide and one or more sources
of peracid. Preferred bleach catalysts comprise one or more transition metal ions.
Other preferred bleaching agents are di-acyl peroxides. Preferred bleach boosters
are selected from the group consisting of: zwitterionic imines, anionic imine polyions,
quaternary oxaziridinium salts, and combinations thereof. Highly preferred bleach
boosters are selected from the group consisting of: aryliminium zwitterions, aryliminium
polyions, and combinations thereof. Suitable bleach boosters are described in US360568,
US5360569 and US5370826.
[0053] A preferred adjunct component is an anti-redeposition agent. Preferably, the STW-composition
comprises one or more anti-redeposition agents. Preferred anti-redeposition agents
are cellulosic polymeric components, most preferably carboxymethyl celluloses.
[0054] A preferred adjunct component is a chelant. Preferably, the STW-composition comprises
one or more chelants. Preferably, the STW-composition comprises (by weight of the
composition) from 0.01 % to 10% chelant. Preferred chelants are selected from the
group consisting of: hydroxyethane-dimethylene-phosphonic acid, ethylene diamine tetra(methylene
phosphonic) acid, diethylene triamine pentacetate, ethylene diamine tetraacetate,
diethylene triamine penta(methyl phosphonic) acid, ethylene diamine disuccinic acid,
and combinations thereof.
[0055] A preferred adjunct component is a dye transfer inhibitor. Preferably, the STW-composition
comprises one or more dye transfer inhibitors. Typically, dye transfer inhibitors
are polymeric components that trap dye molecules and retain the dye molecules by suspending
them in the wash liquor. Preferred dye transfer inhibitors are selected from the group
consisting of: polyvinylpyrrolidones, polyvinylpyridine N-oxides, polyvinylpyrrolidone-polyvinylimidazole
copolymers, and combinations thereof.
[0056] A preferred adjunct component is an enzyme. Preferably, the STW-composition comprises
one or more enzymes. Preferred enzymes are selected from then group consisting of:
amylases, arabinosidases, carbohydrases, cellulases, chondroitinases, cutinases, dextranases,
esterases, β-glucanases, gluco-amylases, hyaluronidases, keratanases, laccases, ligninases,
lipases, lipoxygenases, malanases, mannanases, oxidases, pectinases, pentosanases,
peroxidases, phenoloxidases, phospholipases, proteases, pullulanases, reductases,
tannases, transferases, xylanases, xyloglucanases, and combinations thereof. Preferred
enzymes are selected from the group consisting of: amylases, carbohydrases, cellulases,
lipases, proteases, and combinations thereof.
[0057] A preferred adjunct component is a fabric integrity agent. Preferably, the STW-composition
comprises one or more fabric integrity agents. Typically, fabric integrity agents
are polymeric components that deposit on the fabric surface and prevent fabric damage
during the laundering process. Preferred fabric integrity agents are hydrophobically
modified celluloses. These hydrophobically modified celluloses reduce fabric abrasion,
enhance fibre-fibre interactions and reduce dye loss from the fabric. A preferred
hydrophobically modified cellulose is described in WO99/14245. Other preferred fabric
integrity agents are polymeric components and/or oligomeric components that are obtainable,
preferably obtained, by a process comprising the step of condensing imidazole and
epichlorhydrin.
[0058] A highly preferred adjunct component is a flocculant. Preferably, the STW-composition
comprises (by weight of the composition) from 0.01 % to 25%, preferably from 0.5%,
and preferably to 20%, or to 15%, or to 10%, or to 5% one or more flocculants. Preferred
flocculants are polymeric components, typically having a weight average molecular
weight of at least 100kDa, preferably at least 200kDa. Preferred flocculants are polymeric
components derived from monomeric units selected from the group consisting of: ethylene
oxide, acrylamide, acrylic acid, dimethylamino ethyl methacrylate, vinyl alcohol,
vinyl pyrrolidone, ethylene imine, and combinations thereof. Other preferred flocculants
are gums, especially guar gums. A highly preferred flocculant is polyethylene oxide,
preferably having a weight average molecular weight of at least 100kDa, preferably
at least 200kDa. Preferred flocculants are described in WO95/27036.
[0059] A preferred adjunct component is a salt. Preferably, the STW-composition comprises
one or more salts. The salts can act as alkalinity agents, buffers, builders, co-builders,
encrustation inhibitors, fillers, pH regulators, stability agents, and combinations
thereof. Typically, the STW-composition comprises (by weight of the composition) from
5% to 60% salt. Preferred salts are alkali metal salts of aluminate, carbonate, chloride,
bicarbonate, nitrate, phosphate, silicate, sulphate, and combinations thereof. Other
preferred salts are alkaline earth metal salts of aluminate, carbonate, chloride,
bicarbonate, nitrate, phosphate, silicate, sulphate, and combinations thereof. Especially
preferred salts are sodium sulphate, sodium carbonate, sodium bicarbonate, sodium
silicate, sodium sulphate, and combinations thereof. Optionally, the alkali metal
salts and/or alkaline earth metal salts may be anhydrous.
[0060] A preferred adjunct component is a soil release agent. Preferably, the STW-composition
comprises one or more soil release agents. Typically, soil release agents are polymeric
compounds that modify the fabric surface and prevent the redeposition of soil on the
fabric. Preferred soil release agents are copolymers, preferably block copolymers,
comprising one or more terephthalate unit. Preferred soil release agents are copolymers
that are synthesised from dimethylterephthalate, 1,2-propyl glycol and methyl capped
polyethyleneglycol. Other preferred soil release agents are anionically end capped
polyesters.
[0061] A preferred adjunct component is a soil suspension agent. Preferably, the STW-composition
comprises one or more soil suspension agents. Preferred soil suspension agents are
polymeric polycarboxylates. Especially preferred are polymers derived from acrylic
acid, polymers derived from maleic acid, and co-polymers derived from maleic acid
and acrylic acid. In addition to their soil suspension properties, polymeric polycarboxylates
are also useful co-builders for laundry detergents. Other preferred soil suspension
agents are alkoxylated polyalkylene imines. Especially preferred alkoxylated polyalkylene
imines are ethoxylated polyethylene imines, or ethoxylated-propoxylated polyethylene
imine. Other preferred soil suspension agents are represented by the formula:
bis((C
2H
5O)(C
2H
4O)
n(CH
3)-N
+-C
xH
2x-N
+-(CH
3)-bis((C
2H
4O)
n(C
2H
5O)),
wherein, n=from 10 to 50 and x=from 1 to 20. Optionally, the soil suspension agents
represented by the above formula can be sulphated and/or sulphonated.
Softening-Through-the-Wash Detergent Composition
[0062] The STW-composition is typically a fully formulated laundry detergent composition
or may be an additive for use in the washing stage of a laundering process. Preferably,
however, the STW-compasition is a fully formulated detergent composition. The STW-compostion
is typically a softening-through-the-wash laundry detergent composition. The STW-composition
comprises a di-ester-quat, a source of acid, clay and one or more adjunct components.
[0063] The STW composition can be used to reduce creasing of fabric, and/or to soften fabric,
and/or to confer an ease of ironing benefit to fabric, and/or to confer an anti-static
benefit to fabric, and/or to reduce the fading of colour from fabric, and/or to confer
a skin moisturising benefit to fabric, and/or to removal soil from fabric, and/or
to confer a stain release benefit to fabric, and/or to soften fabric without hydrophobising
the fabric. After laundering with the STW composition, the fabric surfaces retain
their hydrophilicity. This is a highly noticeable consumer benefit as many softeners
generate a hydrophobic fabric surface so that for example, towel drying is less effective.
[0064] In addition it is believed, without wishing to be bound by theory, that the fabric-softening
cationic quaternary ammonium di-ester compound and possibly the source of acid and
also possibly the clay are deposited onto the fabric surface during the laundering
process and form a layer on the fabric surface. If the fabric becomes stained after
the laundering process, it is believed, that the stains, or at least part of or some
of the stains, contact this fabric-softening cationic quaternary ammonium di-ester
compound layer present on the fabric surface. Also, in a subsequent laundering process,
this layer, or part thereof, is stripped from the fabric and a new layer is deposited
on the fabric surface. During this stripping step, any stain in contact with the fabric-softening
cationic quaternary ammonium di-ester compound layer is more easily removed from the
fabric compared to stains directly contacted to the fabric. It is also believed, without
wishing to be bound by theory, that clay improves the stripping of the fabric-softening
cationic quaternary ammonium di-ester compound layer, and that when present, the clay
further improves the stain removal benefit of the STW composition.
[0065] The STW-composition may be in the form of a solid composition. Solid compositions
include powders, granules, noodles, flakes, bars, tablets, and combinations thereof.
The STW-composition may be in the form of a liquid composition. The STW-composition
may also be in the form of a paste, gel, suspension, or any combination thereof. The
STW-composition may be at least partially enclosed, preferably completely enclosed,
by a film or laminate such as a water-soluble and/or water-dispersible material. Preferred
water-soluble and/or water-dispersible materials are polyvinyl alcohols and/or carboxymethyl
celluloses. Preferably, the STW-composition is in the form of a solid composition,
most preferably a particulate solid composition. Typically, the STW-composition has
a bulk density of from 300g/l to 1500g/l, preferably from 600g/l to 900g/l. Preferably,
the STW-composition has a size average particle size of from 200µm to 2000µm, preferably
from 350µm to 600µm.
[0066] Typically, the STW-composition is obtainable, preferably obtained, by a process comprising
a step selected from the group consisting of spray-drying, agglomeration, extrusion,
spheronisation, and combinations thereof. Typically, the STW-composition comprises
spray-dried particles, agglomerates, extrudates, and combinations thereof. The STW-composition
may comprise particles that have been spheronised, for example marumerised particles.
[0067] Preferably the STW-composition comprises a particle that comprises a di-ester quat,
a source of acid, optionally clay and optionally other adjunct components, preferably
less than 90%, or less than 50%, or less than 10%, or even less than 5%, or even less
than 1% adjunct components. Preferably, the size average particle size of the STW-composition
is 200µm or larger, preferably 350µm or larger, and, wherein further, the size average
particle size of the particle comprising the di-ester-quat and the source of acid
is 120µm or smaller, preferably 75µm or smaller.
[0068] Preferably, the particle comprising the di-ester-quat and source of acid is a spray-dried
particle, an agglomerate, or an extrudate. Preferably the particle is a spray-dried
particle. If the particle is a spray-dried particle, then preferable the particle
comprises less than 5%, preferably less than 1% clay. Most preferably, the spray-dried
particle is substantially free of clay. Preferably, no clay is added to the spray-dried
particle. The spray-dried particle preferably has a size average particle size of
200µm or less, preferably 100µm or less, or even 75µm or less, and preferably from
25µm to 150µm. The spray-dried particle, which comprises a di-ester quat and a source
of acid, may be agglomerated with clay, and optionally other adjunct components, preferably
one or more flocculants, to form a particle comprising a di-ester quat, a source of
acid, clay and optionally one or more adjunct components, preferably one or more flocculants.
[0069] The di-ester-quat and source of acid may be incorporated in the STW-composition separately.
However, preferably, the di-ester-quat and source of acid are contacted together to
form a mixture, prior to the di-ester quat and/or the source of acid contacting the
clay and/or adjunct component(s).
[0070] The mixture comprising the di-ester-quat and source of acid can be obtained by any
conventional process. Typically, the mixture comprising the di-ester-quat and source
of acid is obtainable, preferably obtained, by a process comprising the steps of:
(i) obtaining a di-ester quat by quaternising a secondary and/or tertiary di-ester
amine in a substantially water-free solvent, to obtain a first mixture comprising
a di-ester-quat and a substantially water-free solvent, and (ii) contacting a source
of acid to the first mixture to obtain a second mixture comprising a di-ester-quat,
a substantially water-free solvent, and a source of acid, and (iii) removing at least
part, preferably all of the substantially water-free solvent from the second mixture
to obtain a mixture comprising a di-ester-quat and a source of acid. Preferably, the
mixture is solidified to form a solid mixture comprising a di-ester-quat and a source
of acid.
[0071] The substantially water-free solvent is preferably a polar solvent, more preferably
a C
1-5 alcohol, or an isomer thereof, or any combination thereof. Preferred substantially
water-free solvents are selected from the group consisting of: ethanol, isopropanol,
methanol, and combinations thereof. Typically, the term "substantially water-free"
means that the solvent comprises less than 5wt% water, preferably it means that the
substantially water-free solvent comprises no free water. The substantially water-free
solvent is removed from the second mixture by a means selected from the group consisting
of: distillation, sparging, vacuum stripping, evaporation, and combinations thereof.
[0072] Typically, a quaternising agent is used in step (i) of the above process. A preferred
quaternising agent is methyl chloride or methyl sulphate. Most preferably, an excess
of quaternising agent is used in step (i) of the above process.
[0073] A mixture of a di-ester-quat and a source of acid may also be obtainable, preferably
obtained, by a process comprising the steps of: (i) reacting a di-alcohol secondary
and/or tertiary amine with a source of acid optionally in the presence of a solvent,
wherein the source of acid is a C
12-22 fatty acid and/or an anionic derivative thereof, to obtain a first mixture comprising
a di-ester secondary and/or tertiary amine, a source of acid and optionally a solvent;
and (ii) optionally, removing at least part, preferably substantially all of the solvent
from the first mixture, and, optionally, adding an additional source of acid to the
first mixture, to obtain a mixture comprising a di-ester secondary and/or tertiary
amine and a source of acid, and (iii) quaternising the di-ester secondary and/or tertiary
amine to form a mixture comprising a di-ester-quat, a source of acid and optionally
a solvent; and (iv) optionally, removing at least part, preferably substantially all,
of the solvent to obtain a mixture comprising a di-ester-quat and a source of acid.
[0074] Preferably, the mixture is solidified to form a solid mixture comprising a di-ester-quat
and a source of acid. Preferably, in step (i) the molar ratio of the source of acid
to the di-alcohol secondary and/or tertiary amine is at least 2:1, preferably at least
3:1. Optionally, an additional source of acid can be added during step (ii). This
additional source of acid may be a different type of source of acid than the source
of acid that is present during step (i). Optionally, clay is added to the mixture,
the clay can be added between steps (iii) and (iv).
[0075] It may be preferred to remove at least part, preferably all, of the solvent from
the reaction mixture during step (ii). However, if the solvent is substantially all
removed during step (ii), then preferably an additional source of acid is added to
the reaction mixture during step (ii).
[0076] Preferably, step (i) is carried out in the presence of an oxo acid of phosphorous
and/or an alkali metal salt thereof and/or an alkaline earth metal salt thereof. Preferred
oxo acids of phosphorous are selected from group consisting of di-phosphoric acid,
metaphosphoric acid, polyphosphoric acid, phosphorous acid, phosphoric acid, hypophosphorous
acid, and combinations thereof. Preferred salts of oxo acids of phosphorous are selected
from the group consisting of: mono-sodium di-hydrogen hypophosphite, sodium hypophosphite
monohydrate, and combinations thereof.
[0077] Preferred solvents are selected from C
1-5 alcohols and isomers thereof. A preferred solvent is ethanol and/or isopropanol.
[0078] Preferably, the level of free amine impurity in the mixture comprising the di-ester-quat
and source of acid is 5 % by weight of the mixture or less, preferably 3% by weight
of the mixture or less.
[0079] The mixture comprising the di-ester-quat and source of acid may be atomised and sprayed
into a bed of finely ground clay and optionally other adjunct component(s), to obtain
particles comprising a di-ester-quat and source of acid, which are at least partially
enclosed, preferably completely enclosed, by a coating, wherein the coating comprises
clay. Alternatively, the mixture comprising the di-ester-quat and source of acid may
be atomised and sprayed into a bed of finely ground clay and optionally other adjunct
component(s), to obtain particles comprising clay and optionally other adjunct component(s),
which are at least partially enclosed, preferably completely enclosed, by a coating,
wherein the coating comprises a di-ester quat and source of acid.
[0080] Optionally, clay and optionally adjunct component(s) can be dispersed in the mixture
comprising the di-ester-quat and source of acid, to obtain a particle comprising a
di-ester-quat, source of acid, clay and optionally adjunct component(s). Preferably,
clay in the form of ground fines is dispersed in the mixture. Preferably the clay
and optionally adjunct component(s) are dispersed in a molten mixture comprising the
di-ester-quat and source of acid, and preferably the molten mixture is subsequently
cooled, to obtain a particle comprising a di-ester-quat, source of acid, clay and
optionally adjunct component(s).
[0081] Optionally, the STW-composition is obtainable, preferably obtained by a process comprising
the step of adding the di-ester quat or part thereof, the source of acid or part thereof,
optionally the clay or part thereof, and optionally one or more adjunct components,
optionally one or more surfactant, and/or optionally one or more flocculants, to a
crutcher and spray-drying the above components to obtain a spray-dried particle. The
spray-dried particle comprising the di-ester-quat and source of acid may be at least
partially enclosed, preferably completely enclosed by a coating. Preferably, the coating
comprises clay.
[0082] Optionally, the STW-composition is obtainable, preferably obtained, by a process
comprising the step of agglomerating a di-ester quat, a source of acid, optionally
clay, and optionally one or more adjunct component, preferably one or more flocculants,
to obtain an agglomerate. Optionally, the STW-composition is obtained by a process
comprising the steps of: (i) obtaining a first mixture comprising a di-ester-quat
and a source of acid; and (ii) contacting the first mixture to clay to form a second
mixture; and (iii) mixing the second mixture in a high shear mixer to form a third
mixture; and (iv) contacting one or more adjunct components to either the first mixture
and/or second mixture and/or the third mixture to form a STW-composition.
Examples
Example 1: Diester of N-methyl Diethanolamine (DEEMA)
[0083] Fatty acid (1580 g, 5.770 moles) was placed in a glass flask and degassed with nitrogen
at 58°. N-methyldiethanolamine (366.7 g, 3.077 moles) and a 50% solution of hypophosphorous
acid (0.83 g) were added to the flask. The contents of the flask were heated to approximately
195°C, following which the flask was placed under reduced pressure (28-29" Hg) and
held under these conditions for four hours. During the four hours some water vaporized
which was collected and removed from the reaction flask. The material was then cooled
and used for subsequent reactions.
Example 2: Quaternization of DEEMA with Methyl Chloride (DEQ)
[0084] DEEMA (800.0 g, 1.299 moles) and enough ethanol to make an 85% solution were placed
in an autoclave. The contents of the reactor were heated to 95°C and methyl chloride
(85.3 g, 1.689 moles) was added. The reaction was allowed to proceed for seven hours
before the excess methyl chloride was vented and the contents of the reactor sparged
with nitrogen.
Example 3: Ion Pair of DEQ
[0085] The reaction product from the above reaction (328.5 g, 0.436 mole) was placed in
a reaction flask along with an additional 500g of ethanol. The solution was stirred
at 60°C under N2 and tallow alcohol sulfate1 (160.4 g 0.436 mole) was added. A precipitate
formed. Ethanol was distilled (309 g of at 58°/17" vacuum) and replaced with 600 mL
of a 50/50 heptane/hexane mixture. Perlite filter aid (5.0 g) was added and the reaction
mixture filtered at 50°C to give a solution of the ion pair, which solidified on standing.
The hydrocarbon solvent was removed under reduced pressure to give the ion pair.
1. Sulfopon(r) 1218G granules from Cognis were used.
Example 4: Complex of DEQ and Fatty Acid
[0086] DEEMA as described above (406.0 g, 0.671 mole) and hydrogenated tallow fatty acid
(180.9 g, 0.671 mole) were charged to an autoclave and the contents heated to 95°C.
Methyl chloride (48.0 g, 0.95 mole) was added over time and the contents of the reaction
digested for approximately seven hours. The excess methyl chloride was vented and
the contents of the reaction mass sparged with nitrogen for 30 minutes. The material
was discharged following which it solidified on standing.
Example 5: Softening-Through-the-Wash Compositions
[0087] The following compositions A-G, are solid particulate softening-through-the-wash
laundry detergent compositions in accordance with the present invention. Compositions
A-G have a bulk density of from 640g/l to 850g/l.
| Ingredient |
A |
B |
C |
D |
E |
F |
G |
| Dimethyl bis(steroyl oxyethyl) |
1.5% |
1% |
3% |
2% |
5% |
5% |
3% |
| ammonium chloride |
|
|
|
|
|
|
|
| Stearic acid |
1.5% |
5% |
|
1% |
2% |
2.5% |
1% |
| Palmitic acid |
|
|
2% |
|
|
|
|
| Smectite clay |
6% |
9% |
4% |
7% |
10% |
5% |
7% |
| Polyethylene oxide flocculant |
0.2% |
0.1% |
0.2% |
0.2% |
0.1% |
0.1% |
0.2% |
| Anionic surfactant |
5% |
10% |
7% |
6% |
6.5% |
7% |
8% |
| Cationic surfactant |
2% |
|
0.5% |
1.5% |
3% |
1% |
1.5% |
| Nononic surfactant |
1% |
2% |
|
|
|
|
|
| Zeolite A |
14% |
20% |
18% |
17% |
19% |
18% |
21% |
| Crystalline layered silicate |
4% |
3% |
3% |
2% |
4% |
3% |
4% |
| Anhydrous sodium carbonate |
25% |
15% |
22% |
23% |
20% |
22% |
21% |
| Anhydrous sodium sulphate |
15% |
20% |
17% |
18% |
17% |
22% |
17% |
| Acrylic/maleic copolymer |
1% |
2% |
2% |
1.5% |
1% |
1.5% |
1% |
| Sodium perborate tetrahydrate |
8% |
6% |
7% |
|
|
|
5% |
| Sodium percarbonate |
|
|
|
6% |
7% |
5% |
|
| Tetraacetate ethylene diamine |
1% |
1.2% |
0.8% |
1% |
1.1% |
1% |
0.9% |
| Hydrophobically modified |
0.7% |
0.5% |
1% |
0.8% |
|
|
0.8% |
| cellulose |
|
|
|
|
|
|
|
| Enzymes |
0.3% |
0.5% |
0.4% |
0.5% |
0.4% |
0.3% |
0.3% |
| Perfume |
0.2% |
0.1% |
0.2% |
0.2% |
0.1% |
0.1% |
0.3% |
| Miscellaneous |
to |
to |
to |
to |
to |
to |
to |
| |
100 |
100 |
100 |
100% |
100 |
100 |
100 |
| |
% |
% |
% |
|
% |
% |
% |