Note: Descriptions are shown in the official language in which they were submitted.
CA 02436861 2006-09-28
POUCH COMPRISING TRANSPARENT OR TRANSLUCENT LIQUID
COMPOSITION AND VISIBLE SOLID PARTICLES
Field of Invention
This invention relates to liquid composition comprising a transparent or
translucent liquid medium and solid particles contained within the liquid
medium.
Background to the Invention
GB-A-1 303 810, published on 24'h January 1973, discloses clear, liquid
compositions which comprise a visually distinct component of particle size at
least 0.5mm diameter. The liquid medium in which the visually distinct
components are suspended preferably has the rheological properties of a
Bingham body. That is to say that by virtue of its internal structure the
medium
will exhibit a yield value from which it is possible to calculate the maximum
size of
particle which can stably be suspended for a given difference in density
between
the medium and suspended particles.
However if the desired size of suspended particles exceeds the size which is
the
maximum theoretically which can be suspended without either sinking or
floating
then either the liquid medium would have to be modified in order to increase
the
yield value or the density difference between the medium and the suspended
particles would have to be decreased. Neither of these solutions may be
practical
and economical. Furthermore, if the yield point of the medium is too high,
then it
becomes difficult to pour the product.
It is an object of the present invention to provide visually appealing liquid
compositions comprising suspended particles. The suspended particles
themselves may either contribute to the aesthetic appearance of the product,
or
they may have some technically functionality, or both of these. The problems
of
instability, i.e. particles separating either by floating or sinking, and of
excessively
high yield points are overcome.
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CA 02436861 2006-09-28
Summary of Invention
The present invention provides a liquid composition which is a unit dose of a
laundry
composition comprising a transparent or translucent liquid medium and solid
particles contained within the liquid medium wherein the liquid medium
comprises
less than 10% by weight of water, the composition is contained within a pouch
made
from a transparent or translucent water-soluble material, so that the
individual solid
particles are visible from outside the pouch and the composition comprising at
least
an anionic surfactant and a fatty acid.
Preferably the water-soluble pouch material comprises a fiim of water-soluble
material selected from the group consisting of polyacrylates and water-soluble
acrylate copolymers, methylcellulose, carboxymethylcellulose sodium, dextrin,
ethylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose,
maltodextrin, polymethacrylates and mixtures and laminates thereof. More
preferably the water-soluble pouch material comprises polyvinyl alcohol (PVA).
In order to be visible to the human eye when viewed from the outside of the
pouch, it is preferred that the solid particles have a mean geometric diameter
of
at least 0.5 millimetres, more preferably the mean geometric diameter is
between
about 0.5 millimetres and about 12 millimetres, and most preferably it is
between
about 1 millimetre and about 5 millimetres. The geometric diameter of an
individual solid particle as defined herein is the diameter of a hypothetical
spherical particle having the same volume as the individual particle. When
more
than one solid particle is considered, the mean geometric diameter is the
arithmetical mean value of the geometric diameters of the individual
particles.
Various industries, including agrochemicals and laundry industries have been
trying to develop ways to make dosing of the products easier. One of method
for
this is to provide a "unit dose" enclosed within a water-soluble pouch. The
composition of the present invention is preferably a unit dose of a laundry
composition comprising at least anionic surfactant and fatty acid builder. One
of
the advantages of the present invention is that the solid particles do not
necessarily need to be stably suspended in the liquid medium, but rather the
solid
particles may sink or float in the liquid medium. This allows much more
flexibility
to the formulator because it is no longer necessary to match the densities of
the
solid particle and the liquid medium.
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Detailed Description of Invention
Pouch and Material Therefor
The pouch of the invention, herein referred to as "pouch", is typically a
closed
structure, made of a water-soluble film described herein, enclosing a volume
space which comprises a composition. Said composition is described in more
detail hereinafter. The pouch can be of any form, shape and material which is
suitable to hold the composition, e.g. without allowing the release of the
composition from the pouch prior to contact of the pouch to water. The exact
execution will depend on for example, the type and amount of the composition
in
the pouch, the number of compartments in the pouch, the characteristics
required
from the pouch to hold, protect and deliver or release the compositions.
The pouch may have one compartment, holding the liquid composition, or it may
have a number of compartment, attached to one another or non-attached to one
another, thus having one compartment enclosing (but not attaching) another
compartment.
The pouch may be of such a size that it conveniently contains either a unit
dose
amount of the composition herein, suitable for the required operation, for
example
one wash, or only a partial dose, to allow the consumer greater flexibility to
vary
the amount used, for example depending on the size and/or degree of soiling of
the wash load.
It may be preferred that the water soluble film and preferably the pouch as a
whole is stretched during formation and/or closing of the pouch, such that the
resulting pouch is at least partially stretched. This is to reduce the amount
of film
required to enclose the volume space of the pouch. When the film is stretched
the film thickness decreases. The degree of stretching indicates the amount of
stretching of the film by the reduction in the thickness of the film. For
example, if
by stretching the film, the thickness of the film is exactly halved then the
stretch
degree of the stretched film is 100%. Also, if the film is stretched so that
the film
thickness of the stretched film is exactly a quarter of the thickness of the
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unstretched film then the stretch degree is exactly 200%. Typically and
preferably, the thickness and hence the degree of stretching is non-uniform
over
the pouch, due to the formation and closing process.
Another advantage of stretching the pouch, is that the stretching action, when
forming the shape of the pouch and/or when closing the pouch, stretches the
pouch non-uniformly, which results in a pouch which has a non-uniform
thickness. This allows control of the dissolution of water-soluble pouches
herein,
and for example sequential release of the components of the detergent
composition enclosed by the pouch to the water.
Preferably, the pouch is stretched such that the thickness variation in the
pouch
formed of the stretched water-soluble film is from 10 to 1000%, preferably 20%
to
600%, or even 40% to 500% or even 60% to 400%. This can be measured by
any method, for example by use of an appropriate micrometer. Preferably the
pouch is made from a water-soluble film that is stretched, said film has a
stretch
degree of from 40% to 500%, preferably from 40% to 200%.
The pouch is made from a water-soluble film. The material in the form of a
film
can for example be obtained by casting, blow-moulding, extrusion or blow
extrusion of the polymer material, as known in the art. The film may be a
laminate
of two or more films.
The material is water-soluble and has a solubility of at least 50%, preferably
at
least 75% or even at least 95%, as measured by the method set out hereinafter
using a glass-filter with a maximum pore size of 50 micrometers, namely:
Gravimetric method for determining water-solubility or water-dispersability of
the
material of the compartment and/or pouch:
50 grams 0.1 gram of material is added in a 400 ml beaker, whereof the
weight
has been determined, and 245m1 1 ml of distilled water is added. This is
stirred
vigorously on magnetic stirrer set at 600 rpm, for 30 minutes. Then, the
mixture is
filtered through a folded qualitative sintered-glass filter with the pore
sizes as
defined above (max. 50 micrometer). The water is dried off from the collected
filtrate by any conventional method, and the weight of the remaining polymer
is
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determined (which is the dissolved or dispersed fraction). Then, the %
solubility
or dispersability can be calculated.
Preferred polymer copolymers or derivatives thereof are selected from
polyvinyl
alcohols, polyalkylene oxides, acrylic acid, cellulose, cellulose ethers,
cellulose
esters, polyvinyl acetates, polycarboxylic acids and salts, polyaminoacids or
peptides, polyamides, copolymers of maleic/acrylic acids, polysaccharides
including starch and gelatine, natural gums such as xanthum and carragum.
More preferably the polymer is selected from polyacrylates and water-soluble
acrylate copolymers, methylcellulose, carboxymethylcellu lose sodium, dextrin,
ethylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose,
maltodextrin, polymethacrylates, most preferably polyvinyl alcohols, polyvinyl
alcohol copolymers and hydroxypropyl methyl cellulose (HPMC). Preferably, the
level of a type polymer (e.g., commercial mixture) in the film material, for
example
PVA polymer, is at least 60% by weight of the film.
The polymer can have any weight average molecular weight, preferably from
about 1000 to 1,000,000, or even form 10,000 to 300,000 or even form 15,000 to
200,000 or even form 20,000 to 150,000.
Mixtures of polymers can also be used. This may in particular be beneficial to
control the mechanical and/or dissolution properties of the compartment or
pouch, depending on the application thereof and the required needs. For
example, it may be preferred that a mixture of polymers is present in the
material
of the compartment, whereby one polymer material has a higher water-solubility
than another polymer material, and/or one polymer material has a higher
mechanical strength than another polymer material. It may be preferred that a
mixture of polymers is used, having different weight average molecular
weights,
for example a mixture of PVA or a copolymer thereof of a weight average
molecular weight of 10,000- 40,000, preferably around 20,000, and of PVA or
copolymer thereof, with a weight average molecular weight of about 100,000 to
300,000, preferably around 150,000.
Also useful are polymer blend compositions, for example comprising
hydrolytically degradable and water-soluble polymer blend such as polylactide
and polyvinyl alcohol, achieved by the mixing of polylactide and polyvinyl
alcohol,
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typically comprising 1-35% by weight polylactide and approximately from 65% to
99% by weight polyvinyl alcohol, if the material is to be water-dispersible,
or
water-soluble.
It may be preferred that the polymer present in the film is from 60 to 98%
hydrolysed, preferably 80% to 90% hydrolysed, to improve the dissolution of
the
material.
Most preferred are films which are water-soluble and stretchable films, as
described above. Highly preferred water-soluble films are films which comprise
PVA polymers and that have similar properties to the film known under the
trade
reference Monosol 8630, as sold by Chris-Craft Industrial Products of Gary,
Indiana, US and also PT-75, as sold by Aicello of Japan.
The water-soluble film herein may comprise other additive ingredients than the
polymer or polymer material. For example, it may be beneficial to add
plasticisers, for example glycerol, ethylene glycol, diethylene glycol,
propylene
glycol, sorbitol and mixtures thereof, additional water, disintegrating aids.
It may
be useful that the pouch or water-soluble film itself comprises a detergent
additive to be delivered to the wash water, for example organic polymeric soil
release agents, dispersants, dye transfer inhibitors.
The pouch is typically made by a process comprising the steps of contacting a
composition herein to a water-soluble film in such a way as to partially
enclose
the composition to obtain a partially formed pouch. The composition may
already
contain at least one solid particle per pouch, or, alternatively, one or more
of the
solid particles may be added at this stage of the process. Optionally the
first
water-soluble film of the partially formed pouch is then contacted with a
second
water-soluble film, and the films are sealed together to provide the fully
formed
pouch. The first and second water-soluble films may be identical in terms of
material specifications and physical properties (e.g. thickness), but this
need not
necessarily be the case.
In a preferred process, the pouch is made using a mold, preferably the mold
has
round inner side walls and a round inner bottom wall. A liquid medium and at
least one solid particle may then be transferred into the mould, a second
water-
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soluble film may be placed over the mould with the composition and the pouch
may then be sealed. Preferably the first and second films are sealed by heat
sealing or by solvent sealing. The film is preferably stretched during the
formation
of the pouch. Suitable pouch-forming processes are disclosed in US-A-3 218
776, issued on 23rd November 1965, and assigned to Cloud Machine Corp.
Liquid Composition
Typically the liquid composition is contained in the inner volume space of the
pouch, and it may be divided over one or more compartments of the pouch.
The liquid composition preferably has a density of 0.8kg/I to 1.3kg/I,
preferably
about 1.0 to 1.1 kg/I. The liquid composition can made by any method and can
have any viscosity, typically depending on its ingredients. The viscosity may
be
controlled, if desired, by using various viscosity modifiers such as
hydrogenated
castor oil and/or solvents. Hydrogenated castor oil is commercially available
as
Thixcin . Suitable solvents are described in more detail below.
The liquid compositions of the present invention are concentrated and contain
low
levels of water. The liquid compositions comprise less than 10% by weight
water,
and preferably less than 6% by weight water. Suitable compositions may even
comprise less than 4% by weight water.
The compositions herein are typically cleaning compositions or fabric care
compositions, preferably hard surface cleaners, more preferably laundry or
dish
washing compositions, including pre-treatment or soaking compositions and
rinse
additive compositions, including fabric enhancers such as softeners, anti-
wrinkling agents, perfume compositions. Particularly preferred are fabric
cleaning
compositions (laundry detergents).
Preferred ingredients of the liquid composition
The preferred amounts of ingredients described herein are % by weight of the
composition herein as a whole.
If the liquid composition is a detergent composition, it is preferred that at
least a
surfactant and builder are present, preferably at least anionic surfactant and
preferably also nonionic surfactant, and preferably at least a builder, more
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preferably at least a water-soluble builder such as phosphate builder and/or
fatty
acid builder.
Other preferred components are enzymes and/or bleaching agents, such as a
preformed peroxyacid.
Highly preferred are also perfume, brightener, buffering agents (to maintain
the
pH preferably from 5.5 to 9, more preferably 6 to 8), fabric softening agents,
including clays and silicones benefit agents, suds suppressors.
In hard-surface cleaning compositions and dish wash compositions, it is
preferred
that at least a water-soluble builder is present, such as a phosphate, and
preferably also surfactant, perfume, enzymes, bleach.
In fabric enhancing compositions, preferably at least a perfume and a fabric
benefit agent are present for example a cationic softening agent, or clay
softening
agent, anti-wrinkling agent, fabric substantive dye.
Highly preferred in all above compositions are also additional solvents, such
as
alcohols, diols, monoamine derivatives, glycerol, glycols, polyalkylane
glycols,
such as polyethylene glycol. Highly preferred are mixtures of solvents, such
as
mixtures of alcohols, mixtures of diols and alcohols, mixtures. Highly
preferred
may be that (at least) an alcohol, diol, monoamine derivative and preferably
even
glycerol are present. The compositions of the invention are preferably
concentrated liquids having preferably less than 50% or even less than 40% by
weight of solvent (other than water), preferably less than 30% or even less
than
20% or even less than 35% by weight. Preferably the solvent is present at a
level
of at least 5% or even at least 10% or even at least 15% by weight of the
composition.
Highly preferred is that the composition comprises a plasticiser for the water-
soluble pouch material, for example. one of the plasticisers described above,
for
example glycerol. Such plasticisers can have the dual purpose of being a
solvent
for the other ingredients of the composition and a plasticiser for the pouch
material.
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Anionic Surfactant
The detergent compositions of the invention comprise preferably a surfactant
system. Preferably, at least an anionic surfactant is present, preferably at
least an
sulphonic acid surfactant, such as a linear alkyl benzene sulphonic acid, but
salt
forms may also be used. Preferably, at least 15% or even at least 20% or even
at least 30% by weight of the composition is a surfactant, up to 70% or even
60%
or even 50% by weight. Preferably, at least an anionic surfactant and an
nonionic surfactant are present in the surfactant system of the composition,
preferably in a ratio of 1:2 to 2:1, and more preferably 1.5:1 to 1:1.5.
The anionic surfactant(s), are preferably present at a level of at least 7.5%
by
weight of the composition. More preferably anionic surfactant is present at a
level
of from 10% or even at least 15%, or even from 22.5% by weight of the
composition.
Anionic sulfonate or sulfonic acid surfactants suitable for use herein include
the
acid and salt forms of a C5-C20, more preferably a C10-C16, more preferably a
C11-C13 alkylbenzene sulfonates, alkyl ester sulfonates, C6-C22 primary or
secondary alkane sulfonates, sulfonated polycarboxylic acids, and any mixtures
thereof, but preferably C11-C13 alkylbenzene sulfonates.
Anionic sulphate salts or acids surfactants suitable for use in the
compositions of
the invention include the primary and secondary alkyl sulphates, having a
linear
or branched alkyl or alkenyl moiety having from 9 to 22 carbon atoms or more
preferably C12 to C18 alkyl.
Highly preferred are beta-branched alkyl sulphate surfactants or mixtures of
commercial available materials, having a weight average (of the surfactant or
the
mixture) branching degree of at least 50% or even at least 60% or even at
least
80% or even at least 95%. It has been found that these branched sulphate
surfactants provide a much better viscosity profile, when clays are present,
particular when 5% or more clay is present.
It may be preferred that the only sulphate surfactant is such a highly
branched
alkyl sulphate surfactant. Accordingly only one type of commercially available
branched alkyl sulphate surfactant is present, whereby the weight average
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branching degree is at least 50%, preferably at least 60% or even at least
80%,
or even at least 90%. Preferred is for example Isalchem , as available form
Condea.
Mid-chain branched alkyl sulphates or sulfonates are also suitable anionic
surfactants for use in the compositions of the invention. Preferred are the
mid-
chain branched alkyl sulphates. Preferred mid-chain branched primary alkyl
sulphate surfactants are of the formula
R R1 R2
I I I
CH3CH2(CH2)R,CH(CH2)XCH(CH2)yCH(CH2)ZO SO3M
These surfactants have a linear primary alkyl sulphate chain backbone (i.e.,
the
longest linear carbon chain which includes the sulphated carbon atom), which
preferably comprises from 12 to 19 carbon atoms and their branched primary
alkyl moieties comprise preferably a total of at least 14 and preferably no
more
than 20, carbon atoms. In compositions or components thereof of the invention
comprising more than one of these sulphate surfactants, the average total
number of carbon atoms for the branched primary alkyl moieties is preferably
within the range of from greater than 14.5 to about 17.5. Thus, the surfactant
system preferably comprises at least one branched primary alkyl sulphate
surfactant compound having a longest linear carbon chain of not less than 12
carbon atoms or not more than 19 carbon atoms, and the total number of carbon
atoms including branching must be at least 14, and further the average total
number of carbon atoms for the branched primary alkyl moiety is within the
range
of greater than 14.5 to about 17.5.
Preferred mono-methyl branched primary alkyl sulphates are selected from the
group consisting of: 3-methyl pentadecanol sulphate, 4-methyl pentadecanol
sulphate, 5-methyl pentadecanol sulphate, 6-methyl pentadecanol sulphate, 7-
methyl pentadecanol sulphate, 8-methyl pentadecanol sulphate, 9-methyl
pentadecanol sulphate, 10-methyl pentadecanol sulphate, 11-methyl
pentadecanol sulphate, 12-methyl pentadecanol sulphate, 13-methyl
pentadecanol sulphate, 3-methyl hexadecanol sulphate, 4-methyl hexadecanol
sulphate, 5-methyl hexadecanol sulphate, 6-methyl hexadecanol sulphate, 7-
methyl hexadecanol sulphate, 8-methyl hexadecanol sulphate, 9-methyl
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hexadecanol sulphate, 10-methyl hexadecanol sulphate, 11-methyl hexadecanol
sulphate, 12-methyl hexadecanol sulphate, 13-methyl hexadecanol sulphate, 14-
methyl hexadecanol sulphate, and mixtures thereof.
Preferred di-methyl branched primary alkyl sulphates are selected from the
group
consisting of: 2,3-methyl tetradecanol sulphate, 2,4-methyl tetradecanol
sulphate, 2,5-methyl tetradecanol sulphate, 2,6-methyl tetradecanol sulphate,
2,7-methyl tetradecanol sulphate, 2,8-methyl tetradecanol sulphate, 2,9-methyl
tetradecanol sulphate, 2,10-methyl tetradecanol sulphate, 2,11-methyl
tetradecanol sulphate, 2,12-methyl tetradecanol sulphate, 2,3-methyl
pentadecanol sulphate, 2,4-methyl pentadecanol sulphate,. 2,5-methyl
pentadecanol sulphate, 2,6-methyl pentadecanol sulphate, 2,7-methyl
pentadecanol sulphate, 2,8-methyl pentadecanol sulphate, 2,9-methyl
pentadecanol sulphate, 2,10-methyl pentadecanol sulphate, 2,11-methyl
pentadecanol sulphate, 2,12-methyl pentadecanol sulphate, 2,13-methyl
pentadecanol sulphate, and mixtures thereof.
It is preferred that the anionic surfactants herein are present in the form of
sodium salts.
Nonionic alkoxylated surfactant
Ethoxylated and propoxylated nonionic surfactants are preferred. Preferred
alkoxylated surfactants can be selected from the classes of the nonionic
condensates of alkyl phenols, nonionic ethoxylated alcohols, nonionic
ethoxylated/propoxylated fatty alcohols.
Highly preferred are nonionic alkoxylated alcohol surfactants, being the
condensation products of aliphatic alcohols with from 1 to 75 moles of
alkylene
oxide, in particular about 50 or from 1 to 15 moles, preferably to 11 moles,
particularly ethylene oxide and/or propylene oxide, are highly preferred
nonionic
surfactants. The alkyl chain of the aliphatic alcohol can either be straight
or
branched, primary or secondary, and generally contains from 6 to 22 carbon
atoms. Particularly preferred are the condensation products of alcohols having
an
alkyl group containing from 8 to 20 carbon atoms with from 2 to 9 moles and in
particular 3 or 5 moles, of ethylene oxide per mole of alcohol.
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Polyhydroxy fatty acid amides are highly preferred nonionic surfactant
comprised
by the composition, in particular those having the structural formula R2CONR1Z
wherein : R1 is H, C1-18, preferably C1-C4 hydrocarbyl, 2-hydroxy ethyl, 2-
hydroxy propyl, ethoxy, propoxy, or a mixture thereof, preferable C1-C4 alkyl,
more preferably C1 or C2 alkyl, most preferably C1 alkyl (i.e., methyl); and
R2 is
a C5-C31 hydrocarbyl, preferably straight-chain C5-C19 or C7-C1 g alkyl or
alkenyl, more preferably straight-chain Cg-C17 alkyl or alkenyl, most
preferably
straight-chain C11-C17 alkyl or alkenyl, or mixture thereof; and Z is a
polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least 3
hydroxyls directly connected to the chain, or an alkoxylated derivative
(preferably
ethoxylated or propoxylated) thereof. Z preferably will be derived from a
reducing
sugar in a reductive amination reaction; more preferably Z is a glycityl.
Cationic surfactant
Suitable cationic mono-alkoxylated and bis-alkoxylated quaternary amine
surfactants with a C6-C18 N-alkyl chain, such as of the general formula I:
R~ 4
N X-
R2 R3
(I)
wherein R1 is an alkyl or alkenyl moiety containing from about 6 to about 18
carbon atoms, preferably 6 to about 16 carbon atoms, most preferably from
about
6 to about 14 carbon atoms; R2 and R3 are each independently alkyl groups
containing from one to about three carbon atoms, preferably methyl, most
preferably both R2 and R3 are methyl groups; R4 is selected from hydrogen
(preferred), methyl and ethyl; X- is an anion such as chloride, bromide,
methylsulphate, sulphate, or the like, to provide electrical neutrality; A is
a alkoxy
group, especially a ethoxy, propoxy or butoxy group; and p is from 0 to about
30,
preferably 2 to about 15, most preferably 2 to about 8.
The cationic bis-alkoxylated amine surfactant preferably has the general
formula
II:
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Rl ApR3
N X-
R2~ A,qR4
(II)
wherein R1 is an alkyl or alkenyl moiety containing from about 8 to about 18
carbon atoms, preferably 10 to about 16 carbon atoms, most preferably from
about 10 to about 14 carbon atoms; R2 is an alkyl group containing from one to
three carbon atoms, preferably methyl; R3 and R4 can vary independently and
are selected from hydrogen (preferred), methyl and ethyl, X' is an anion such
as
chloride, bromide, methylsulphate, sulphate, or the like, sufficient to
provide
electrical neutrality. A and A' can vary independently and are each selected
from
C1-C4 alkoxy, especially ethoxy, (i.e., -CH2CH2O-), propoxy, butoxy and
mixtures thereof; p is from 1 to about 30, preferably 1 to about 4 and q is
from 1
to about 30, preferably 1 to about 4, and most preferably both p and q are 1.
Another suitable group of cationic surfactants which can be used in the
detergent
compositions are cationic ester surfactants. Suitable cationic ester
surfactants,
including choline ester surfactants, have for example been disclosed in US
Patents No.s 4228042, 4239660 and 4260529.
Builder compounds
The compositions in accord with the present invention preferably contain a
water-
soluble builder compound, typically present in detergent compositions at a
level
of from 1% to 60% by weight, preferably from 3% to 40% by weight, most
preferably from 5% to 25% by weight of the composition.
Suitable water-soluble builder compounds include the water soluble monomeric
carboxylates, or their acid forms, or homo or copolymeric polycarboxylic acids
or
their salts in which the polycarboxylic acid comprises at least two carboxylic
radicals separated from each other by not more that two carbon atoms, and
mixtures of any of the foregoing.
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Highly preferred maybe that one or more fatty acids and/ or optionally salts
thereof (and then preferably sodium salts) are present in the detergent
composition. It has been found that this can provide further improved
softening
and cleaning of the fabrics. Preferably, the compositions contain 1% to 25% by
weight of a fatty acid or salt thereof, more preferably 6% to 18% or even 10%
to16% by weight. Preferred are in particular C12-C1$ saturated and/ or
unsaturated fatty acids, but preferably mixtures of such fatty acids. Highly
preferred have been found mixtures of saturated and unsaturated fatty acids,
for
example preferred is a mixture of rape seed-derived fatty acid and C16-C18
topped whole cut fatty acids, or a mixture of rape seed-derived fatty acid and
a
tallow alcohol derived fatty acid.
The detergent compositions of the invention may comprise phosphate-containing
builder material. Preferably present at a level of from 2% to 40%, more
preferably
from 3% to 30%, more preferably from 5% to 20%. Suitable examples of water-
soluble phosphate builders are the alkali metal tripolyphosphates, sodium,
potassium and ammonium pyrophosphate, sodium and potassium and
ammonium pyrophosphate, sodium and potassium orthophosphate, sodium
polymeta/phosphate in which the degree of polymerization ranges from about 6
to 21, and salts of phytic acid.
The compositions in accord with the present invention may contain a partially
soluble or insoluble builder compound, typically present in detergent
compositions at a level of from 0.5% to 60% by weight, preferably from 5% to
50% by weight, most preferably from 8% to 40% weight of the composition.
Preferred are aluminosilicates, such as Zeolite A or zeolite MAP and/or
crystalline
layered silicates such as SKS-6 , available from Clariant.
However, from a formulation point of view it may be preferred not to include
such
builders in the liquid composition, because it will lead to too much dispersed
or
precipitate material in the liquid, or it requires too much process or
dispersion
aids.
Chelating aaents
The composition may comprise a chelating agent, typically a high ionic
strength
chelating agent, having two or more phosphonic acid or phosphonate groups, or
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two or more carboxylic acid or carboxylate groups, or mixtures thereof. By
chelating agent it is meant herein components which act to sequester (chelate)
heavy metal ions, but these components may also have calcium and magnesium
chelation capacity.
Chelating agents are generally present at a level of from 1%, preferably from
2.5% from 3.5% or even 5.0% or even 7% and preferably up to 20% or even
15% or even 10% by weight of the composition herein.
Highly suitable organic phosphonates herein are amino alkylene poly (alkylene
phosphonates), alkali metal ethane 1-hydroxy bisphosphonates and nitrilo
trimethylene phosphonates. Preferred among the above species are diethylene
triamine penta (methylene phosphonate), ethylene diamine tri (methylene
phosphonate) hexamethylene diamine tetra (methylene phosphonate) and
hydroxy-ethylene 1,1 diphosphonate.
Other suitable chelating agents for use herein include nitrilotriacetic acid
and
polyaminocarboxylic acids such as ethylenediaminotetracetic acid,
ethylenetriamine pentacetic acid, ethylenediamine disuccinic acid,
ethylenediamine diglutaric acid, 2-hydroxypropylenediamine disuccinic acid or
any salts thereof. Especially preferred is ethylenediamine-N,N'-disuccinic
acid
(EDDS) or the alkali metal, alkaline earth metal, ammonium, or substituted
ammonium salts thereof, or mixtures thereof.
Glycinamide-N,N'-disuccinic acid (GADS), ethylenediamine-N-N'-diglutaric acid
(EDDG) and 2-hydroxypropylenediamine-N-N'-disuccinic acid (HPDDS) are also
suitable.
Suitable chelating agents with two or more carboxylates or carboxylic acid
groups
include the acid or salt forms of succinic acid, malonic acid, (ethylenedioxy)
diacetic acid, maleic acid, diglycolic acid, tartaric acid, tartronic acid and
fumaric
acid, as well as the ether carboxylates and the sulfinyl carboxylates.
Chelants
containing three carboxy groups include, in particular, the acids or salt
forms of
citrates, aconitrates and citraconates as well as succinate derivatives.
Preferred
carboxylate chelants are hydroxycarboxylates containing up to three carboxy
groups per molecule, more particularly citrates and citric acids.
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Chelating agents containing four carboxy groups include the salts and acid
forms
of oxydisuccinates, 1,1,2,2-ethane tetracarboxylates, 1,1,3,3-propane
tetracarboxylates and 1,1,2,3-propane tetracarboxylates, sulfosuccinate
derivatives.
Highly preferred it that at least one organo phosphonate or phosphonic acid
and
also at least one di- or tri-carboxylate or carboxylic acid is present. Highly
preferred is that at least fumaric acid (or salt) and citric acid (or salt)
and one or
more phosphonates are present. Preferred salts are sodium salts.
Perfume
Highly preferred are perfume components, preferably at least one component
comprising a coating agent and/ or carrier material, preferably organic
polymer
carrying the perfume or aluminosilicate carrying the perfume, or an
encapsulate
enclosing the perfume, for example starch or other cellulosic material
encapsulate. In a particularly preferred embodiment of the present invention
the
solid particle is a perfume encapsulate.
Fabric softening clays
Preferred fabric softening clays are smectite clays, which can also be used to
prepare the organophilic clays described hereinafter, for example as disclosed
in
EP-A-299575 and EP-A-313146. Specific examples of suitable smectite clays
are selected from the classes of the bentonites- also known as
montmorillonites,
hectorites, volchonskoites, nontronites, saponites and sauconites,
particularly
those having an alkali or alkaline earth metal ion within the crystal lattice
structure.
Preferably, hectorites or montmorillonites or mixtures thereof. Hectorites are
most preferred clays.
The softening clay if present, may be used at levels up to about 15%, more
preferably from about 3% to about 10% by weight, when the formulation is to be
a
fabric softening formulation.
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The hectorite clays suitable in the present composition should preferably be
sodium clays, for better softening activity. Sodium clays are either naturally
occurring, or are naturally-occuring calcium-clays which have been treated so
as
to convert them to sodium-clays. If calcium-clays are used in the present
compositions, a salt of sodium can be added to the compositions in order to
convert the calcium clay to a sodium clay. Preferably, such a salt is sodium
carbonate, typically added at levels of up to 5% of the total amount of clay.
Examples of hectorite clays suitable for the present compositions include
Bentone EW as sold by Elementis.
Another preferred clay is an organophilic clay, preferably a smectite clay,
whereby at least 30% or even at least 40% or preferably at least 50% or even
at
least 60% of the exchangeable cations is replaced by a, preferably long-chain,
organic cations. Such clays are also referred to as hydrophobic clays. The
cation
exchange capacity of clays and the percentage of exchange of the cations with
the long-chain organic cations can be measured in several ways known in the
art,
as for example fully set out in Grimshaw, The Chemistry and Physics of Clays,
Interscience Publishers, Inc.,pp. 264-265 (1971).
Whilst the organophilic smectite clay provides excellent softening benefit,
they
can increase the viscosity of the liquid compositions. Therefore, it will
depend on
the viscosity requirements of the composition, how much of these organophlic
clays can be used. Typically, they are used in the liquid detergent
compositions
of the invention at a level of from 0.1% to 10%, more preferably from 0.3% to
7%,
most preferably from 0.4% to 5% or even 0.5% to 4% by weight of the
composition.
These organophilic clays are formed prior to incorporation into the detergent
composition. Thus for example, the cations, or part thereof, of the normal
smectite clays are replaced by the long-chain organic cations to form the
organophilic smectite clays herein, prior to further processing of the
material to
form the detergents of the invention.
The organophilic clay is preferably in the form of a platelet or lath-shaped
particle.
Preferably the ratio of the width to the length of such a platelet is at least
1:2,
preferably at least 1:4 or even at least 1:6 or even at least 1:8.
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When used herein, a long-chain organic cation can be any compound which
comprises at least one chain having at least 6 carbon atoms, but typically at
least
carbon atoms, preferably at least 12 carbon atoms, or in certain embodiments
of the invention, at least 16 or even at least 18 carbon atoms. Preferred long-
chain organic cations are described hereinafter.
Preferred organophilic clays herein clay are smectite clays, preferably
hectorite
clays and/ or montmorillonite clays containing one or more organic cations of
formulae:
R1 Rs
R4-N R2 "lk
I R6(CH2)n-N N CH3
R3 or
where R, represents an organic radical selected from R7, R-CO-O-(CH2)n, or
R7-CO-NR8- in which R7 is an alkyl, alkenyl or alkylaryl group with 12-22
carbon
atoms, whereby R8 is hydrogen, CI-C4 alkyl, alkenyl or hydroxyalkyl,
preferably -
CH3 or -C2H5 or -H ; n is an integer, preferably equal to 2 or 3; R2
represents an
organic radical selected from R1 or Cl-C4 alkyl, alkenyl or hydroxyalkyl,
preferably
-CH3 or -CH2CH2OH; R3 and R4 are organic radicals selected from C1-C4 alkyl-
aryl, Cl-C4 alkyl, alkenyl or hydroxyalkyl, preferably -CH3, -CH2CH2OH, or
benzyl
group; R5 is an alkyl or alkenyl group with 12-22 carbon atoms; R6 is
preferably -
OH, -NHCO-R7, or -OCO-R7.
Highly preferred cations are quaternary ammonium cations having two C16-C28 or
even C16-C24 alkyl chains. Highly preferred are one or more organic cations
which have one or preferably two alkyl groups derived from natural fatty
alcohols,
the cations preferably being selected from dicocoyl methyl benzyl ammonium,
dicocoyl ethyl benzyl ammonium, dicocoyl dimethyl ammonium, dicocoyl diethyl
ammonium; more preferably ditallow diethyl ammonium, ditallow ethyl benzyl
ammonium; more preferably ditallow dimethyl ammonium and/ or ditallow methyl
benzyl ammonium.
It may be highly preferred that mixtures of organic cations are present.
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WO 02/057402 PCT/US02/01500
Highly preferred are organophilic clays as available from Rheox/Elementis,
such
as Bentone SD-1 and Bentone SD-3, which are registered trademarks of
Rheox/Elementis.
In a particularly preferred embodiment of the present invention the solid
particle is
a clay particle, such as a clay agglomerate or extrudate.
Cationic fabric softening agents
Cationic fabric softening agents are preferably present in the composition
herein.
Suitable cationic fabric softening agents include the water insoluble tertiary
amines or dilong chain amide materials as disclosed in GB-A-1 514 276 and EP-
B-0 011 340. Preferably, these water-insoluble tertiary amines or dilong chain
amide materials are comprised by the solid component of the composition
herein.
Cationic fabric softening agents are typically incorporated at total levels of
from
0.5% to 15% by weight, normally from 1% to 5% by weight.
Bleaching agent
Another ingredient which may be present is a perhydrate bleach, such as salts
of
percarbonates, particularly the sodium salts, and/ or organic peroxyacid
bleach
precursor. It has been found that when the pouch or compartment is formed from
a material with free hydroxy groups, such as PVA, the preferred bleaching
agent
comprises a percarbonate salt and is preferably free form any perborate salts
or
borate salts. It has been found that borates and perborates interact with
these
hydroxy-containing materials and reduce the dissolution of the materials and
also
result in reduced performance.
Inorganic perhydrate salts are a preferred source of peroxide. Preferably
these
salts are present at a level of from 0.01% to 50% by weight, more preferably
of
from 0.5% to 30% by weight of the composition or component.
Examples of inorganic perhydrate salts include percarbonate, perphosphate,
persulfate and persilicate salts. The inorganic perhydrate salts are normally
the
alkali metal salts. The inorganic perhydrate salt may be included as the
crystalline solid without additional protection. For certain perhydrate salts
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WO 02/057402 PCT/US02/01500
however, the preferred executions of such granular compositions utilise a
coated
form of the material which provides better storage stability for the
perhydrate salt
in the granular product. Suitable coatings comprise inorganic salts such as
alkali
metal silicate, carbonate or borate salts or mixtures thereof, or organic
materials
such as waxes, oils, or fatty soaps.
Alkali metal percarbonates, particularly sodium percarbonate are preferred
perhydrates herein. Sodium percarbonate is an addition compound having a
formula corresponding to 2Na2CO3.3H2O2, and is available commercially as a
crystalline solid.
The composition herein preferably comprises a peroxy acid or a precursor
therefor (bleach activator), preferably comprising an organic peroxyacid
bleach
precursor. It may be preferred that the composition comprises at least two
peroxy
acid bleach precursors, preferably at least one hydrophobic peroxyacid bleach
precursor and at least one hydrophilic peroxy acid bleach precursor, as
defined
herein. The production of the organic peroxyacid occurs then by an in situ
reaction of the precursor with a source of hydrogen peroxide.
The hydrophobic peroxy acid bleach precursor preferably comprises a compound
having a oxy-benzene sulphonate group, preferably NOBS, DOBS, LOBS and/or
NACA-OBS, as described herein.
The hydrophilic peroxy acid bleach precursor preferably comprises TAED, as
described herein.
Amide substituted alkyl peroxyacid precursor compounds are suitable herein,
including those of the following general formulae:
R1-C-N-R2-C-L R1-N-C-R2-C-L
O R5 0 or R5 O 0
wherein R1 is an alkyl group with from 1 to 14 carbon atoms, R2 is an alkylene
group containing from 1 to 14 carbon atoms, and R5 is H or an alkyl group
containing 1 to 10 carbon atoms and L can be essentially any leaving group.
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Amide substituted bleach activator compounds of this type are described in EP-
A-0 170 386.
The composition may contain a pre-formed organic peroxyacid.
A preferred class of organic peroxyacid compounds are the amide substituted
compounds of the following general formulae:
R1-C-N-R2-C-OOH R1 -N-C-R2-C-OOH
O R5 0 or R5 O 0
wherein R1 is an alkyl, aryl or alkaryl group with from 1 to 14 carbon atoms,
R2 is
an alkylene, arylene, and alkarylene group containing from 1 to 14 carbon
atoms,
and R5 is H or an alkyl, aryl, or alkaryl group containing 1 to 10 carbon
atoms.
Amide substituted organic peroxyacid compounds of this type are described in
EP-A-0 170 386.
Other organic peroxyacids include diacyl and tetraacylperoxides, especially
diperoxydodecanedioic acid, diperoxytetradecanedioic acid and
diperoxyhexadecanedioic acid. Mono- and diperazelaic acid, mono- and
diperbrassylic acid and N-phthaloylaminoperoxicaproic acid are also suitable
herein.
In a particularly preferred embodiment of the present invention the solid
particle is
a particulate bleach or bleach activator.
Suds suppressing system
The composition may comprise a suds suppresser at a level less than 10%,
preferably 0.001% to 10%, preferably from 0.01% to 8%, most preferably from
0.05% to 5%, by weight of the composition Preferably the suds suppresser is
either a soap, paraffin, wax, or any combination thereof. If the suds
suppresser is
a suds suppressing silicone, then the detergent composition preferably
comprises
from 0.005% to 0.5% by weight a suds suppressing silicone.
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Enzymes
Another preferred ingredient useful in the compositions herein is one or more
enzymes.
Preferred enzymatic materials include the commercially available lipases,
cutinases, amylases, neutral and alkaline proteases, cellulases, endolases,
esterases, pectinases, lactases and peroxidases conventionally incorporated
into
detergent compositions. Suitable enzymes are discussed in US Patents
3,519,570 and 3,533,139.
Preferred commercially available protease enzymes include those sold under the
trade marks Alcalase, Savinase, Primase, Durazym, and Esperase by Novo
Industries A/S (Denmark), those sold under the trade marks Maxatase, Maxacal
and
Maxapem by Gist-Brocades, those sold by Genencor International, and those sold
under the trade marks Opticlean and Optimase by Solvay Enzymes.
Protease enzyme may be incorporated into the compositions in accordance with
the invention at a level of from 0.0001% to 4% active enzyme by weight of the
composition.
Preferred amylases include, for example, a-amyiases obtained from a special
strain of B licheniformis, described in more detail in GB-1,269,839 (Novo).
Preferred commercially available amylases include for example, those sold
under
the trade mark Rapidase by Gist-Brocades, and those sold under the trade marks
Termamyl, Duramyl and BAN by Novo Industries A/B. Highly preferred amylase
enzymes maybe those described in WO 96/03276, and in W095/26397 and
W096/23873.
Amylase enzyme may be incorporated into the composition in accordance with
the invention at a level of from 0.0001% to 2% active enzyme by weight of the
composition.
In a particularly preferred embodiment of the present invention the solid
particle is
an enzyme encapsulate.
Useful additional non-alkoxylated organic polymeric compounds for inclusion in
the compositions herein include the water soluble organic homo- or co-
polymeric
22
CA 02436861 2006-09-28
polycarboxylic acids or their salts in which the polycarboxyfic acid comprises
at
least two carboxyl radicals separated from each other by not more than two
carbon atoms. Polymers of the latter type are disclosed in GB-A-1,596,756.
Examples of such salts are polyacrylates of MWt 1000-5000 and their
copolymers with maleic anhydride, such copolymers having a molecular weight of
from 2000 to 100,000, especially 40,000 to 80,000.
Other organic polymeric compounds suitable for incorporation in the detergent
compositions herein include cellulose derivatives.
Suitable suds suppressing systems for use herein may comprise essentially any
known antifoam compound, including for example silicone antifoam compounds
and 2-alkyl alcanol antifoam compounds.
Other suitable antifoam compounds include the monocarboxylic fatty acids and
soluble salts thereof, as also described as builders above. These materials
are
described in US Patent 2,954,347, issued September 27, 1960 to Wayne St.
John. The monocarboxylic fatty acids, and salts thereof, for use as suds
suppressor typically have hydrocarbyl chains of 10 to 24 carbon atoms,
preferably 12 to 18 carbon atoms. Suitable salts include the alkali metal
salts
such as in particular sodium but also potassium salts.
The compositions herein may also comprise from 0.01.% to 10 %, preferably from
0.05% to 0.5% by weight of polymeric dye transfer inhibiting agents. The
polymeric dye transfer inhibiting agents are preferably selected from
polyamine
N-oxide polymers, copo(ymers of N-vinylpyrrolidone and N-vinylimidazole,
polyvinylpyrrolidonepolymers or combinations thereof, whereby these polymers
can be cross-linked polymers.
The compositions herein also optionally contain from about 0.005% to 5% by
weight of certain types of hydrophilic optical brighteners. Preferred
brighteners
include 4,4',-bis[(4-anilino-6-(N-2-bis-hydroxyethyl)-s-triazine-2-yl)aminoJ-
2,2'-
stilbenedisulfonic acid and disodium salt, commercially marketed under the
trade mark Tinopal-UNPA-GX by Ciba-Geigy Corporation; 4,4'-bis[(4-anilino-6-(N-
2-
hydroxyethyl-N-methylamino)-s-triazine-2-yl)amino]2,2'-stilbenedisulfonic acid
disodium salt, commercially marketed under the trade mark Tinopal 5BM-GX by
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Ciba-Geigy Corporation; 4,4'-bis[(4-anilino-6-morphilino-s-triazine-2-
yl)aminoj2,2'-
stilbenedisulfonic acid, sodium salt, commercially marketed under the trade
mark
Tinopal-DMS-X and Tinopal AMS-GX by Ciba Geigy Corporation.
Also preferred may be bleaches, neutralizing agents, buffering agents, phase
regulants, hydrotropes, enzyme stabilizing agents, opacifiers, anti-oxidants,
bactericides, photo-bleaches.
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WO 02/057402 PCT/US02/01500
Examples
Example 1
The following low-moisture liquid detergent media were prepared. Moisture
level
as made was about 3.8% (Formula 1A) and about 5.5% (Formula 1B).
ingredient 1A. 1 B.
ei ht percent weight percent
1 ,2- ro anediol 15.7% 16.6%
Neodol 23-9 18.7% 20.9%
C11.8 linear alkylbenzene sulfoni 22.0% 29.1%
acid
ormic acid 1.1% 1.0%
citric acid (50% soln.) 1.6% 2.3%
monoethanolamine 11.0% 10.4%
alm kernal fatty acid 16.6% .9%
sodium diethylenetriamineO.9% 0.3%
entaacetate (40% soln.)
decyl amido ro lamine 1.8% 1.8%
ol mer 1 80% ' 1.6% 1.1%
ol mer 2 (80%)2 1.6% 2.3%
calcium formate (10% soln.) 0.06%
rotease enzyme 2.5% 2.5%
amylase enzyme 0.3% 0.3%
brightener 15 0.2% 0.2%
dye 0.003% 0.003%
erfume 0.6% 0.8%
water o balance o balance
'Polymer 1 is a polyethyleneimine (MW = 182) with av. degree of ethoxylation =
15.
2Polymer 2 is a polyethyleneimine (MW = 600) with av. degree of ethoxylation =
20.
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Example 2
Uniform spherical particles containing a polymeric profragrance were prepared
by
adding a reaction product of s-damascone and Lupasol0 WF into molten
Pluracol0 E 4000 at 60 C. The melt was then cast into 10 mm spheres in a
mold.
Ingredient a b
profragrance 6.0 % 6.0 %
Pluracol0 E 4000 94.0 % 93.4 %
Ex ancel0 091 DE50 0.6 %
weight of 10 mm diameter 0.57 g 0.46 g
capsule
Samples a and b were placed in the low moisture liquid detergent media of
Examples 1A and 1B and sealed in pouches of soluble polyvinyl alcohol film,
Mono-SolO 8630, (50 ml of detergent and one 10 mm capsule per pouch) to
provide unitized dose liquid detergent compositions with visible fragrance
capsules. The particles were stable in the low moisture detergent of Examples
1A and 1B and dissolved in the wash to impart a fresh scent to laundry after
drying. The spherical particles of sample b are less dense than the detergent
and float in the detergent in the pouch and rapidly dissolve when the pouch is
added to the wash.
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Example 3
Extruded particles containing sodium citrate were prepared by combining 54.4 g
of Pluracol E 4000 solution (48.7% in water), 204.1 g of sodium citrate
dihydrate, and 41.2 g of water. The mixture was extruded through an 8 mm axial
dye and cut into 8 mm lengths. After drying, the composition was:
ingredient weight percent
Pluracol E 4000 11.1 %
sodium citrate (as 74.8 %
anh drous
water 14.1 %
Samples of the solid citrate particles were placed in the low moisture liquid
detergent media of Examples 1A and 1 B and sealed in pouches of soluble
polyvinyl alcohol film, Mono-Sol 8630, (50 ml of detergent and two solid
particles per pouch) to provide unitized dose liquid detergent compositions
with
visible solid particles. The particles were visible and stable in the low
moisture
liquid detergent and rapidly dissolve when added to the wash.
Example 4
Uniform spherical particles containing an oxidation catalyst were prepared by
combining dichloro(4,11-diethyl-1,4,8,11-
tetraazabicyclo[6.6.2]hexadecane)manganese with molten Pluracol E 4000 at
60 C followed by casting in a mold to give the following composition.
Ingredient weight percent
bleach catalyst 6.0 %
Pluracol E 4000 94.0 %
weight of 10 mm diameter 0.59 g
capsule
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Samples of the solid bleach catalyst particle were placed in the low moisture
liquid detergent media of Examples 1A and 1B and sealed in pouches of soluble
polyvinyl alcohol film, Mono-SolO 8630, (50 ml of detergent and one solid
particle
per pouch) to provide unitized dose liquid detergent compositions with visible
bleach catalyst particles and rapidly dissolve when added to the wash.
Example 5
Solid particles containing a fabric anti-abrasion agent and dye anti-fading
agent
were prepared by combining 25.0 g of modified cellulose, 5.60 g of solution of
an
imidazole-epichlorohydrin condensation oligomer (44.6% in H20), 20.8 g of
sodium citrate dihydrate, 6.5 g of Acusol0 445N (45.0% in H20), and 38.5 g of
H20, forming into particles approximately 10 mm in diameter, and drying. After
drying the individual particles weighed approximately 0.6 g each and the
composition was:
ingredient weight percent
modified cellulose3 44.5 %
imidazole-epichlorohydrin 4.5 %
condensation oli omer3
sodium citrate (as anh drous 32.4 %
sodium polyacrylate, Acusol0 445N 5.2 %
water 13.4%
3 as described in WO 00/22078 Al
Samples of the solid particles were placed in the low moisture liquid
detergent
media of Examples 1 A and 1 B and sealed in pouches of soluble polyvinyl
alcohol
film, Mono-SolO 8630, (50 mi of detergent) to provide unitized dose liquid
detergent compositions with visible solid particles.
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Example 6
In a further example coloured particles with a mean geometric diameter of a)
2mm and b) 5mm are made by adding dye onto starch base particles. These
coloured particles or "speckles" are added to the liquid compositions of the
previous examples for consumer desirable aesthetics. The speckles rapidly
dissolve when added to the wash.
29
