Note: Descriptions are shown in the official language in which they were submitted.
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DETERGENT COMPOSITION CONTAINING PARTICULATE ZEOLITE BUILDER AND
LUBRICANT THEREFOR.
The present invention relates to a detergent composition comprising both a
particulate zeolite component having a small particle size as a sequestering
agent for water hardness and an agent capable of reducing the abrasive
contact of said particulate zeolite with laundry fabrics, when employed in a
laundry w~shin~ method.
Detergent compositions for fabric w~hin~ conventionally contain
delelge"cy builders which lower the concentration of calcium and
magnesium water hardness ions in the wash liquor and thereby provide
good detergency effect in both hard and soft water.
Conventionally, inorganic phosphates, such as sodium tripolyphosphate,have been used as builders for laundry detel~ellls. More recently, alkali
metal aluminosilicate ion-exchangers, particularly crystalline sodium
aluminosilicate zeolite A, have been proposed as replacements for the
inorganic phosphates.
For example, EP 21 491A (Procter & Gamble) discloses detergent
compositions cont~ining a building system which includes zeolite A, X or
P (B) or a mixture thereof. EP 384070A (Unilever) discloses specific
zeolite P materials having an especially low silicon to aluminium ratio not
greater than 1.33 (hereinafter referred to as zeolite MAP) and describes its
use as a detergency builder, optionally with cobuilders.
The Applicants have now surprisingly found that a problem may
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occur when a water insoluble zeolite having a small particle size, is
used as a detergency builder. The problem has been found to be
particularly pronounced when the zeolite builder is zeolite MAP.
The choice of a small particle size for a zeolite MAP component, that is to
say particles having a particle size, measured as a dso value, of up to 1.0
micrometres has previously been taught to be preferred in the art, as
represented, for example, by EP 384070 A. The small particle size can
enhance the capacity of the builder to absorb liquid components, which
can be advantageous in the preparation of high active zeolite agglomerate
particles cont~ining liquid detergent components.
The problem relates to the aforementioned detergent compositions having
a marked incompatibility with printed fabrics, particularly printed cotton
fabrics. In particular, it has been found that the use of detergent
compositions cont~inin~ small particle size zeolite tends to lead to the
removal of printed pigment from a printed fabric surface.
The Applicant has surprisingly found that this problem can be ameliorated
by the use in the detergent composition of a lubricating agent which is
capable of forming a partial or complete lubricant coating on the zeolite
particles, thereby reducing their abrasive affect on the surface of the
printed cotton fabrics which they come into contact with as the wash
proceeds.
The present invention is thus based on the unexpected finding that theprinted fabric care profile of a detergent composition comprising an
insoluble zeolite of small particle size and a 'small particle zeolite
lubricating agent' is superior to that of comparable compositions not
cont~inin~? the zeolite lubricating agent.
This finding allows the formulation of detergent compositions providing
both excellent cle~ning and printed fabric care properties on fabrics,
especially cotton fabrics.
Whilst the prior art, as represented for example by European Patent
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Aplications, EP 384070 A, EP 448297 A, EP 522726 A, EP 533392 A, EP
544492 A, EP 552053 A, and EP 552054 A has envisaged the use of
various detergent components in combination with zeolite in laundry
detergent compositions, none of these prior art documents specifically
disclose the use of a lubricating agent with a small particle size zeolite
component. Furthermore, none of these prior art documents provides any
teaching relating to the small particle size zeolite specific printed fabric
care problem addressed by the current invention, nor of any solution
thereto involving the use of a zeolite particle lubricating agent.
Thus, the present invention provides a detergent composition suitable for
use in a method of w~hin~ soiled fabrics cont~inin~
(a) a surfactant selected from a~ionic, cationic, nonionic, amphoteric
and zwitterionic detergent active compounds and mixtiures thereof;
(b) a particulate zeolite builder having a particle size, dso, of less
than 1.0 micrometres; and
(c) an agent capable of acting as a lubricant for the particulate
zeolite builder thereby reducing any abrasive contact of the zeolite
builder with said fabrics when employed in said method of w~shin~
In a prefemed embodiment of the invention the zeolite builder compriseszeolite P having a silcon to aluminium ratio of not greater than 1.33
(zeolite MAP).
In a further preferred embodiment the detel~ellt composition according to
the invention is formulated to be especially useful in the launderimg of
coloured fabrics and preferably is free of bleach. According to another
aspect of the invention, the composition is subst~nti~lly free of an optical
brightener.
According to another aspect of the present invention there is provided the
use of a detergent composition cont~inin~ a particulate zeolite builder
having a particle size, dso, of less than 1.0 micrometres in a method o f
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washing printed fabrics, particularly printed cotton fabrics, wherein said
composition contains an agent capable of acting as a lubricant for said
particulate zeolite builder thereby reducing the abrasive contact of the
zeolite builder with said printed fabrics.
Surfactant
The detergent composition according to the invention contains as an
essential component a surfactant selected from anionics, nonionics,
zwitterionics, ampholytics and cationics.
The surfactant is preferably present in the detergent compositions at a level
of from 1% to 50%, preferably from 3% to 30%, most preferably from 5%
to 20% by weight of the compositions.
Many suitable detergent-active compounds are available and fully
described in the literature (for example "Surface Active Agents and
Detergents" Volumes I and II by Schwartz, Perry and Berch).
Examples of suitable additional anionic surfactants include anionic
slllf~tes, olefin sulphonates, alkyl xylene sulphonates,
dialkylsulphosuccinates, and fatty acid ester sulphonates. Sodium
salts are generally preferred.
Anionic sulfate surfactant
Anionic sulfate surfactants suitable for use herein include the linear and
branched primary alkyl sl-lf~tes, alkyl ethoxysulfates, fatty oleoyl glycerol
snlf~tes, alkyl phenol ethylene oxide ether sulfates, the Cs-C17 acyl-N-
(Cl-C4 alkyl) and -N-(Cl-C2 hydroxyalkyl) gl~lc~mine slllf~tes, and
sulfates of alkylpolysaccharides such as the sulfates of alkylpolyglucoside
(the nonionic nonsulfated compounds being described herein).
Alkyl ethoxysulfate surfactants are preferably selected from the group
consisting of the C6-C 18 alkyl sulfates which have been ethoxylated with
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from 0.5 to 20 moles of ethylene oxide per molecule. More preferably, the
alkyl ethoxysulfate surfactant is a C6-C 18 alkyl sulfate which has been
ethoxylated with from O.S to 20, preferably from 0.5 to 5, moles of
ethylene oxide per molecule.
Anionic sulfonate surfactant
Anionic sulfonate surfactants suitable for use herein include the salts of
Cs-C20 linear alkylbenzene sulfonates, alkyl ester sulfonates, C6-C22
primary or secondary alkane sulfonates, C~-C2~ olefin sulfonates,
sulfonated polycarboxylic acids, alkyl glycerol sulfonates, fatty acyl
glycerol sulfonates, fatty oleyl glycerol sulfonates, and any mixtures
thereof.
Nonionic surfactant
The nonionic surf~ct~nt is preferably a hydrophobic nonionic
surfactant, particularly an alkoxylated nonionic surfactant, having a
hydrophilic lipophilic balance (hlb) value of < 9.5, more preferably
< 10.5.
Examples of suitable hydrophobic alkoxylated nonionic surfactants
include alkoxylated adducts of fatty alcohols cont~inin~ an average of
less than S alkylene oxide groups per molecule.
The alkylene oxide residues may, for example, be ethylene oxide
residues or mixtures thereof with propylene oxide residues.
Preferred alkylene oxide adducts of fatty alcohols useful in the
present invention can suitably be chosen from those of the general
formula:
~ R-O-(CnH2nO)yH
wherein R is an alkyl or alkenyl group having at least 10 carbon
atoms, most preferably from 10 to 22 carbon atoms, y is from 0.5 to
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3.5 and n is 2 or 3.
Preferred nonionic surfactants include primary C 11 -C 15 aliphatic
alcohols condensed with an average of no more than five ethylene
oxide groups per mole of alcohol, having an ethylene oxide content of
less than 50% by weight, preferably from 25% to less than 50% by
weight.
A particularly preferred aliphatic alcohol ethoxylated is a primary
alcohol having an average of 12 to 15 carbon atoms in the alkyl chain
condensed with an average of three ethoxy groups per mole of
alcohol.
Specific examples of suitable alkoxylated adducts of fatty alcohols
are Synperonic A3 (ex ICI), which is a C13-C 15 alcohol with about
three ethylene oxide groups per molecule and Empilan KB3 (ex
Marchon), which is lauric alcohol 3EO.
Another class of nonionic sufactants comprises alkyl polyglucoside
compounds of general formula
RO(CnH2nO)tzx
wherein Z is a moiety derived from glucose; R is a saturated
hydrophobic alkyl group that contains from 12 to 18 carbon atoms; t
is from 0 to 10 and n is 2 or 3; x is from 1.1 to 4, the compounds
including less than 10% unreacted fatty alcohol and less than 50%
short chain alkyl polyglucosides. Compounds of this type and their
use in de~ergent compositions are disclosed in EP-B 0070074,
0070077, 0075996 and 0094118.
Zeolite builder
The second essential component of the detergent compositions of the
present invention is an aluminosilicate zeolite builder, optionally in
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conjunction with one or more cobuilders. Such aluminosilicate zeolil:e
builders are generally water-insoluble.
The zeolite builder is typically present at a level of from 1% to 80%,more preferably from 15% to 40% by weight ofthe compositions.
Suitable aluminosilicate zeolites have the unit cell fonnula
Naz~(A102)z(SiO2)y]. XH2O wherein z and y are at least 6; the molar
ratio of z to y is from 1.2 to 0.5 and x is at least 5, preferably from 7.5 to
276, more preferably f~om 10 to 264. ~he aluminosilicate material are in
hydrated form and are preferably crystalline, cont~ining f~om 10% to 28%,
more preferably from 18% to 22% water in bound form.
The aluminosilicate zeolites can be naturally occurring materials, but are
preferably synthetically derived. Synthetic crystalline aluminosilicate ion
exchange materials are available under the designations Zeolite A, Zeolite
B, Zeolite P, Zeolite X Zeolite MAP, Zeolite HS and mixtures thereof.
Zeolite A has the formula
Na 12 ~A1~2) 12 (sio2)l2]. xH2O
wherein x is from 20 to 30, especially 27. Zeolite X has the formula Na86
[(Alo2)86(sio2) 106]- 276 H2O.
Zeolite MAP is described in EP 384070A (Unilever). It is defined as
an alkali metal alumino-silicate of the zeolite P type having a silicon
to aluminium ratio not greater than 1.33, preferably within the range
from 0.9 to 1.33 and more preferably within the range of from 0.9 to
1.2.
Of particular interest is zeolite MAP having a silicon to aluminium
ratio not greater than 1.15 and, more particularly, not greater than
1.07.
Zeolite P having a Si:Al ratio of 1.33 or less may be prepared by the
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following steps:
(i) mixing together a sodium alumin~te having a mole ratio
Na2O:A12O3 within the range of from 1.4 to 2.0 and a
sodium silicate having a mole ratio SiO2:Na2O within
the range of from 0.8 to 3.4 with vigorous stirring at a
temperature within the range of from 25~C to boiling
point usually 95~C, to give a gel having the following
composition; A12O3: (1.75-3.5) SiO2: (2.3-7.5) Na2O :P
(~Q-45Q)H20;
(ii) ageing the gel composition for 0.5 to 10 hours,
preferably 2 to 5 hours, at a temperature within the range
of from 70~C to boiling point, usually to 95~C, with
sufficient stirring to m~int~in any solids present in
suspension;
(iii) separating the crystalline sodium aluminosilicate thus
formed, w~hing to a pH within the range of from 10 to
12.5, and drying, preferably at a temperature not
excee-linp 1 50~C, to a moisture content of not less than S
wt.%.
Preferred drying methods are spray-drying and flash-drying. It
appears that oven drying at too high a temperature may adversely
affect the calcium binding capacity of the product under certain
circum~t~nces.
Commercial sodium metasilicate pentahydrate dissolved in water and
commercial sodium silicate solution (waterglass) are both suitable
silica sources for the production of zeolite P in accordance with the
invention. The reactants may be added together in any order either
rapidly or slowly. Rapid addition at ambient temperature, and slow
addition at elevated temperature (90-95~C) both give the desired
product.
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Vigorous stirring of the gel during the addition of the reactants, and at
least moderate stirring during the subsequent ageing step, however,
appear to be essential for the formation of pure zeolite P. In the
absence of stirring, various mixtures of crystalline and amorphous
materials may be obtained.
Zeolite MAP generally has a calcium binding capacity of at least 150
mg CaO per g of anhydrous aluminosilcate, as measured by the
standard method described in GB 1473201 (Henkel). The calcium
binding capaci~y is nor~nally 160 mg CaC~/g and may be 2S high 170
mg CaO/g.
Although zeolite MAP like other zeolites contains water of hydration,
for the purposes of the present invention amounts and percentages of
zeolite are expressed in terms of the notional anhydrous material.
The amount of water present in hydrated zeolite ~AP at ambient
temperature and humidity is generally about 20 wt.%.
The zeolite builder used in the present invention has a particle size dso of
less than 1.0 micrometres, preferably from 0.05 to 0.9 micrometres, most
preferably from 0.2 to 0.7 micrometres. The dso value indicates that 50%
by weight of the particles have a diameter smaller than that figure. The
particle size may be determined by conventional analytical techniques
such as, for èxample, microscopic determination utili7in~ a sc~nnin~
electron microscope or by means of a laser granulometer.
Zeolite builder having the required particle size according to the present
invention can be prepared by the conventional techniques as described
above while adopting one or more of the following steps:-
a) decreasing cryst~ tion time;
b) decreasing the size of the seed crystals used to produce the zeolite;
c) screening the zeolite product to remove coarse material.
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An article by D. Vucelic, published in Progr Colloid Polymer Science,
1994, Volume 95, pages 14 - 38 describes methods for the synthesis of
zeolite particles, and in particular how to influence the particle size
characteristics of the zeolites by modification of the synthesis process
steps.
~ubricant
The detergent compositions contain as an essential component an
agent capable 'in use' of acting as a lubricant for the zeolite particles,
thereby reducing the abrasive effect associated with the contact of the
particles with any fabrics, particularly printed cotton fabrics, in the
wash. The agent therefore acts such as to reduce the frictional forces
which can arise when the zeolite particles contact any fabric in the
wash. One mech~ni~m for such reduction of abrasive frictional
contact is for the lubricant 'in use' to partially or completely coat the
zeolite particles.
The lubricant should moreover not significantly compromise the
ability of the zeolite to provide builder capacity to a wash solution,
and is most preferably water soluble. Biodegradable lubricants are
preferred.
The zeolite particle lubricant is preferably present at a level of from0.05% to 50%, more preferably from 1% to 20% by weight ofthe
detergent composition.
Preferably, the level of incorporation of the lubricant will be selected
to be such as to reduce the level of abrasive contact to an acceptable
level. A low lubricant to zeolite ratio is preferred from a cost
standpoint. In particular, the weight ratio of lubricant to zeolite
should be less than 1:3, preferably less than 1:5, more preferably less
than 1 :7.
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Suitable zeolite lubricants are preferably polymers which are nonionic in
character, particularly those cont~ining a plurality of glycol components.
In particular, fatty alcohol poly(ethylene glycol) ethers of molecular
weights of from 400 to 5000 are suitable herein. WO 93/16159 describes
particularly suitable fatty alcohol poly (ethylene glycol) ethers which
contain from 4 to 7 glycol units. DE ~124247 A similarly describes
suitable fatty alcohol poly (ethylene glycol) ethers. DE 3401861 A
describes suitable alkylphenol polyglycol ethers. DE 3444311 A describes
suitable isotridecyl polyglycol ethers.
Particulate zeolite colubricants which are based on alcohol ethoxylates,
especially those having at least a proportion of branched carbon chains, are
also suitable herein, particularly when present in combination with the
hereinbefore described glycol cont~ining lubricants. The degree of carbon
chain branching is preferably at least 10% by weight, more preferalbly at
least 20% by weight. US 5298185 A describes suitable oxo alcohol
ethoxylates and their use in detergent compositions in combination with
polyethylene glycols.
Additional deter~ent components
The detergent composition according to the invention may contain
other detergent components such as cobuilders, bleaches, fluorescers,
antiredeposition agents, inorganic salts such as sodium sulphate, other
enzymes, lather control agents, fabric softening agents, pigments,
coloured speckles and perfumes.
Cobuilder
In addition to zeolite, the detergent compositions may contain an
organic or inorganic cobuilder.
Suitable organic cobuilders can be monomeric or polymeric
carboxylates such as citrates or polymers of acrylic, methacrylic
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and/or maleic acids in neutralised forrn. Suitable inorganic
cobuilders include carbonates and amorphous and crystalline layered
silicates.
Suitable crystalline layered silicates have the composition:
NaMSix02x+l . yH20
where M is sodium or hydrogen, preferably sodium; x is a number
from 1.~ to 4; and y is a number ~rom ~ to ~0. Such rnaterials are
described in US Patents No.4664839; No.4728443 and No.4820439
(Hoechst AG). Especially preferred are compounds in which x = 2
and y = O. The synthetic material is commercially available from
Hoechst AG as ~ -Na2 Si2Os (SKS6) and is described in US Patent
No.4664830.
The total amount of detergency builder in the granular composition
typically ranges from 10 to 80 wt.%, more preferably from 15 to 60 wt%
and most preferably from 10 to 45 wt.%.
In a highly preferred aspect the level of carbonate builder, that is of
inorganic compound capable of releasing carbonate ions into a wash
solution, is less than 7% by weight, preferably less than 4% by weight of
the detergent composition. High levels of carbonate have been found to
further exacerbate the printed cotton fabric abrasion problem. Most
preferably the detergent composition is free from carbonate builder.
Bleach
Detergent compositions according to the invention may also contain a
bleach system. Where present, this preferably comprises one or more
peroxy bleach compounds, for example, inorganic persalts or organic
peroxyacids, which may be employed in conjunction with bleach
precursors to improve bleaching action at low temperatures.
The bleach system preferably comprises a peroxy bleach compound,
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preferably an inorganic persalt, optionally in conjunction with a
peroxyacid bleach precursor. Suitable persalts include sodium
perborate monohydrate and tetrahydrate and sodium percarbonate,
with sodium percarbonate being most preferred.
Preferred bleach precursors are peracetic acid precursors, such as
tetraacetylethylene ~ mine (TAED); peroxybenzoic acid precursors.
In one preferred aspect, the detergent compositions are free of bleachand of par$icular utili$y in the w~hin~ of loads cont~inin~; brightly
coloured fabrics.
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14
Low pH/~lk~linity deter~ent compositions
Preferred detergent compositions according to the invention are
characterised by having a pH measured as a 1% solution of the detergent
composition in distilled water at 25~C of < 10.5, preferably < 10.4, most
preferably < 10.3.
It has been found that compositions having a low level of reserve ~lk~linity
are advantageous in that they have a further reduced tendency to cause the
removal of printed p;gment from printed cotton fabrics. ~eserve ~lk~linity
is expressed as g of NaOH per 100 g of composition as deterrnined by acid
titration of a sample, as 1% solution in distilled water to a pH of 9.5.
Preferred values of reserve ~lk~linity are ' 8.0 g preferably < 5.0 g, most
preferably < 3 .0 g NaOH per 1 00g of composition.
Physical form
The detergent composition according to the invention may be of any
physical type, for example powders, liquids and gels. However,
granular and liquid compositions are preferred.
Makin~ process
The detergent compositions of the invention may be prepared by any
suitable method. The particulate detergent compositions are suitably
prepared by any tower (spray-drying) or non-tower process.
In processes based around a spray-drying tower, a base powder is first
prepared by spray-drying a slurry and then other components
unsuitable for processing via the slurry can be sprayed on or admixed
(postdosed).
The zeolite builder is suitable for inclusion in the slurry, although it
may be advantageous for processing reasons for part of the zeolite
builder to be incorporated post-tower. The crystalline layered
silicate, where this is employed, is also incorporated via a non-tower
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process and is preferably postdosed.
Alternatively, particulate detergent compositions in accordance with
the invention may be prepared by wholly non-tower processes such as
granulation.
The granular detergent compositions of the invention may be
prepared to any suitable bulk density. The compositions preferably
have a bulk density of at least 400 g/l preferably at least 550 g/l, most
preferably at least 700 g/l and, with particular preference at least 800
g/l.
The benefits of the present invention are particularly evident in
powders of high bulk density, for example, of 700 g/l or above. Such
powders may be prepared either by post-tower densification of spray-
dried powder, or by wholly non-tower methods such as dry mixing
and granulation; in both cases a high-speed mixer/gr~mll~tor may
advantageously be used. Processes using high-speed
mixer/gr~n~ tors are disclosed, for example, in EP340 013A, EP 367
339A, EP 390 25 lA and EP 420 317A (Unilever).
The detergent composition of the invention may be formulated as a
liquid detergent composition which may be aqueous or anhydrous.
The term "liquid" used herein includes pasty viscous formulations
such as gels. The liquid detergent composition generally has a pH of
from6.5to 10.5.
The total amount of detergency builder in the liquid composition is
preferably from 5 to 70% of the total liquid composition.
Illustrative compositions according to the present invention are presented
in the following Examples. In the detergent compositions, the abbreviated
component i-len~ifications have the following me~nin~:
24AS : Sodium alkyl sulfate surfactant cont~ining
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16
predomin~ntly C12 and C14 alkyl chains
TAS : Sodium alkyl sulfate surfactant cont~ining
predominantly C 16 - C 18 alkyl chains derived
from tallow oil.
24AE3S : C12-C14 alkyl ethoxysulfate cont~inin,Q an
average of three ethoxy groups per mole
35E3 : A C 13-1 5 alcohol having 10% alkyl chain
branching condensed with an average of 3 moles
of ethylene oxide
25E3 : A C12-Cls alcohol having 30% alkyl chain
branching condensed with an average of 3 moles
of ethylene oxide
PEG 1 : A C12-C1s primary fatty alcohol condensed with
an average of 5 moles of ethylene glycol
PEG 2 : A C12-C1s alkylphenol condensed with an
average of 5 moles of ethylene glycol
Carbonate : Anhydrous sodiumcarbonate
Perborate : Sodium perboratetetrahydrate
Percarbonate : Sodium percarbonate
TAED : Tetra acetyl ethylene ~ mine
Silicate : Amorphous Sodium Silicate (SiO2:Na2O ratio
norlnally follows)
SKS6 : Crystalline layered silicate available from
Hoechst AG as SKS6 (tradename)
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17
Zeolite MAP : Hydrated sodium aluminosilicate zeolite MAP
having a silicon to aluminium ratio of 1.07
having a particle size, expressed as a dso value,
of 0.7 micrometres
Zeolite A : Hydrated sodium aluminosilicate zeolite A
having a particle size, expressed as a dso value,
of 0.6 micrometres
MA/AA : Copolymer of 1:4 maleic/acrylic acid, average
molecular weight about 80,000.
Alcalase : Proteolytic enzyme sold under the tradename
Alcalase by Novo Industries A/S (approx 1%
enzyme activity by weight)
BSA : Amylolytic enzyme sold under the tradename
LEl 7 by Novo Industries A/S (approx 1%
enzyme activity)
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18
Example 1
The following granular laundry detergent compositions were prepared
(parts by weight) in accordance with the invention.
A B C D E
24AS 7.6 6.5 4.8 6.8
TAS - - - - 8.6
24AE3 S 2.4 - 1.2 1.7
25E3 3.26 - - - 6.3
35E3 - 5.0 5.0 5.0
Zeolite MAP 20.0 25.0 25.0 - 16.0
Zeolite A - - - 25.0 15.0
PEG 1 2.0 - 3.0 - 2.0
PEG 2 - 3.0 - 2.0 1.0
SKS6 7.0 5.0 10.0
Carbonate 5.0 3.0
MA/AA 4.25 4.25 4.25 4.25 2.0
Perborate - 16.0 - 16.0 20.0
Percarbonate 20.0 - 20.0
TAED 5.0 5.0 5.0 5.0 6.7
Alcalase 0.2 0.5 0.3 0.2 0.1
BSA - - 0.1
Protease 0.04 0.08 - 0.05 0.05
Silicate(2.0 4.0 - - 4.0 3.0
ratio)
Water and miscellaneous (Including suds suppressor, sodium sulphate,
perfume) to balance
The detergent compositions A to E according to the invention, which
comprise a zeolite particle lubricant ~i.e. PEG 1 or PEG 2), show good
results in stain removal and lower printed cotton fabric ~ ge as
co~ ed with a composition comprising no zeolite particle lubricant.
