Note: Descriptions are shown in the official language in which they were submitted.
GRANULAR LAUNDRY DETERGENT COMPOSITIONS
HAVING IMPROVED SOLUBILITY
Jeffrey E. Boucher
Eugene J. Pancheri
FIE~D 0~ THE INVENTION
The present invention relates to granular detergent
compositions having improved solubility. More particularly, it
relates to granular detergent laundry compositions and additives
containing sodium carbonate and sodium phosphate and low levels
of potassium salt for improved cold water solubility.
Processes for improving solubility of granular detergent
compositions are also included.
BACKGROUND OF THE INVENTION
This invention was made during a search for a way to
improve solubility of granular laundry detergent products and
prevent clumps of detergent from remaining in the washer and
on washed clothes. Such clumps, which may appear as solid white
masses ranging from about 5 to 40 millimeters in diameter and
about 2 to 10 millimeters in lsngth, have occurred during cold
water washes when the order of addition to the washing machine
is laundry detergent product first, clothes second, and water
last. It has been found that the primary contributors to this
solubility problem are the sodium carbonate and sodium phosphate
in the granular laundry detergent. It has been discovered that
surprisingly low levels of potassium salts can be included in
the granular detergent composition to improve solubility and
eliminate or reduce this clumping problem.
Sodium carbonate and sodium pyrophosphate have been used
in granular detergent compositions (for example, U.S. Patent
25 4,299,717/ Cottrell et al, issued November 10, 1981). Potassium
salt has been substituted for sodium salt to eliminate giant
micelles of sodium salt of washed fatty acid in the washing
liquid. The solubility of a solid is lower in a solution of a
salt containing a common ion than in pure water (Chemical
Principles, 4th ed., Masterton Slowinski, W.B. Saunders Co.
1977, pg. 435). Lastly, a water~so~tening composition
comprising tetrasodium pyrophosphate and an alkaline material
selected from the group consisting of trisodium
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phosphate, sodium hydroxide, sodium carbonates, potassium
hydroxide, potassium carbonates, soap and sodium silicate is
disclosed in U.S. Patent 2,381,960, Johnson, patented August 14,
1945. HowevPr, it has not been disclosed that low levels of
potassium salt can be added to a granular laundry detergent
compos;tion or additive contain;ng sodium carbonate and sodium
phosphate to improve solubility of the composition in water.
SUMMARY OF THE INVENTION
The instant invention presents a granular laundry detergent
0 composition comprising:
(a) from about 5 to 70 weight % detergent surfactant
selected from the group consisting of an;onics,
non;onics, zwitterionics, ampholytics, cationics, and
mixtures thereof;
lS (b) from about 5 to 70 weight % sodium phosphate;
(c) from about 5 to 70 weight % sodium car-bonate; and
(d) from about 0.1 to 10 weight % potassium salt.
A process for improving solubility of a granular laundry detergent
composition according to the above is also presented.
DESCRIPTION OF THE INVENTION
This invention covers a granular laundry detergent
composition or additive which is soluble in cold or cool water,
i.e. the composition or additive readily dissolves/disperses in
water at a temperature between about 32-F ~0C) and 90-F (32.~'C~,
preferably between about 35'F (1.6'C) and 50'F (10 C). Because of
the incorporation of a surprisingly low level of potassium salt in
the product, no significant amount of product remains bound in the
clothes or in the bottom of the washing machine tub after a
typical cold ~ater wash cycle, even with a product first, clothes
second, water last order of addition. A process for improving
solubility or dispersibility of a granular detergent composition
is also included in the invention.
The claimed granular laundry detergent composition or
additive comprises:
(a) from about 5 to 70 weight % detergent surfactant
selected from the group consisting of anionics,
nonionics, zwitterionics, ampholytlcs, cationics, and
mixtures thereof;
S (b) from about 5 to 70 weight % sodium phosphate;
(c) from about 5 to 70 weight % sodium carbonate; and
(d) from about 0.1 to 10 weight % potassium salt.
A. Deterqent Surfactant
The first ingredient, present at a level of from about 5 to
70 weight %, preferably about 10 to 30 weight %, is detergent
surfactant selected from the group consisting of anionics,
nonionics, zwitterionics, ampholytics, cationics, and mixtures
thereof. Preferred is from about 10 to 30 weight %, most
preferably from about 12 to 20 weight %1 detergent surfactant
select`ed from the group consisting of anionics, nonionics,
cationics, and mixtures thereof.
Water-soluble salts of the higher fatty acids, i.e., "soaps~,
are useful anionic surfactants in the compositions herein. This
includes alkal; metal soaps such as the sodium, potassium,
ammonium, and alkylolammonium salts of higher fatty acids
containing from about 8 to about 24 carbon atoms, and preferably
from about 12 to about 18 carbon atoms. Soaps can be made by
direct saponification of fats and oils or by the neutral kation of
free fatty acids. Par~icularly useful are the sodium and
potassium salts of the mixtures of fatty acids derived from
coconut oil and tallow, i.e., sodium or potassium tallow and
coconut soap.
Useful anionic surfactants also include the water-soluble
salts, preferably the alkali metal, ammonium and alkylolammonium
salts, of organic sulfuric reaction products having in their
molecular strueture an alkyl group containing from about 10 to
about 20 carbon atoms and a su1fonic acid or sulfuric acid ester
group. (Included in the term "alkyl" is the alkyl portion of acyl
groups.) Examples of this group of synthetic surfactants are the
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sodium and potassium alkyl sulfates, especially those obtained by
sulfating the higher alcohols (C12-Clg carbon atoms) such as those
produced by reducing the glycerides of tallow or coconut oil; and
the sodium and potassium alkylbenzene sulfonates in which the
alkyl group contains from about 10 to about 16 carbon atoms, in
straight chain or branched chain configurat;on, e.g., see U.S.
Patents 2,220,099 and ?,477,383, Especially valuable are linear
straight chain alkylbenzene sulfonates in which the average number
of carbon atoms in the alkyl group is from about 11 to 14,
abbreviated as C11 14 LAS.
Especially preferred is from about 12 to 20 weight % of a
mixture of C10-l6 linear alkylbenzene sulfonate and C12 18 alkyl
sulfatè. These are preferably in a weight ratio of between 50:50
and 80:20, preferably 70:30, sodium Clo-l6 (preferably C11-14)
LAS:sodium C12-l8 (preferably Cl~ 1~) alkyl sulfate.
Other anionic surfactants herein are the sodium alkyl
glyceryl ether sulfonates, especially those ethers of higher
alcohols derived from tallow and coconut oil, sodium coconut oil
fatty acld monoglyceride sulfonates and sulfates; sodium or
potassium salts of alkyl phenol ethylene oxide ether sulfates
containing from about 1 to about 10 units of ethylene oxide per
molecule and wherein the alkyl groups contain from about 8 to
about 12 carbon atoms; and sodium or potassium salts of alkyl
ethylene oxide ether sulfates containing about 1 to about 10 units
of ~thylene oxide per molecule and wherein the alkyl group
contains from about 10 to about 20 carbon atoms.
Other useful anionic surfactants herein include the
water-soluble salts of esters of alpha-sulfonated fatty acids
containing from about 6 to 20 carbon atoms in the fatty acid group
and from about 1 to 10 carbon atoms in the ester group;
water-soluble salts of 2-acyloxyalkane-1-sulfonic acids containing
from about 2 to 9 carbon atoms in the acyl group and from about 9
to about 23 carbon atoms in the alkane moiety; water-soluble salts
of olefin and paraffin sulfonates containing from about 12 to 20
2 ,i
carbon atoms; and beta-alkyloxy alkane sulfonates conta;ning from
about 1 to 3 carbon atoms in the alkyl group and from about 8 to
20 carbon atoms in the alkane moiety.
Water-soluble nonionic surfactants are also useful in the
instant detergent granules. Such nonionic materials include
compounds produced by the condensation of alkylene oxide groups
(hydrophil;c in nature) with an organic hydrophobic compound,
which may be aliphatic or alkyl aromatic in nature. The length of
the polyoxyalkylene group which is condensed with any particular
hydrophobic group can be readily adjusted to yield a water-soluble
compound having the desired degree of balance between hydrophilic
and hydrophobic elements.
Suitable nonionic surfactants include the polyethylene oxide
condensates of alkyl phenols, e.g., the condensation products of
alkyl phenols having an alkyl group containing from about 6 to 15
carbon atoms, in either a straight chain or branched chain
configuration, with from about 3 to 80 moles of ethylene oxide per
mole of alkyl phenol.
Included are the water-soluble and water-dispersible
condensation products of aliphatic alcohols containing from 8 to
22 carbon atoms, in either straight chain or branched
configuration, with from 3 to 12 moles of ethylene oxide per mole
of alcohol.
Semi-polar nonionic surfactants include water-soluble amine
oxides containing one alkyl moiety of from abut 10 to 18 carbon
atoms and two moieties selected from the group of alkyl and
hydroxyalkyl moieties of from about 1 to about 3 carbon atoms;
water-soluble phosphine oxides containing one alkyl moiety of
about 10 to 18 carbon atoms and two moieties selected from the
group consisting of alkyl groups and hydroxyal kyl groups
containing from about 1 to 3 carbon atoms; and water-soluble
sulfoxides containing one alkyl moiety of from about 10 to 18
carbon atoms and a moiety selected from the group consisting of
alkyl and hydroxyalkyl moieties of from about 1 to 3 carbon atoms.
,
.
Preferred nonionic surfactants are of the formula
Rl(OC2H4)nOH, wherein R1 ;s a Clo-C16 alkyl group or a Cg-C12
alkyl phenyl group, and n ;s from 3 to about 80.
Particularly preferred are condensation products of C12-Cls
S alcohols w;th from about 5 to about 20 moles of ethylene oxide per
mole of alcohol, e.g., C12-C13 alcohol condensed ~ith about 6.5
moles of ethylene oxide per mole of alcohol.
Ampholytic surfactants include derivatives of aliphatic or
aliphatic derivatives of heterocyclic secondary and tertiary
amines in which the aliphatic moiety can be straight chain or
branched and wherein one of the aliphatic substituents contains
from about 8 to 18 carbon atoms and at least one aliphatic
substituent contains an anionic water-solubilizing group.
Zwitterionic surfactants include derivatives of aliphatic,
quaternary, ammonium, phosphonium, and sulfonium compounds in
which one of the aliphatic substituents contains from about 8 to
18 carbon atoms.
Cationic surfactants can also be included in the present
detergent granules. Cationic surfactants comprise a wide variety
of compounds characterized by one or more organic hydrophobic
groups in the cation and generally by a quaternary nitrogen
associated with an acid radical. Pentavalent nitrogen ring
compounds are also considered quaternary nitrogen compounds.
Halides, methyl sulfate and hydroxide are suitable. Tert;ary
amines can have characteristics similar to cationic surfactants at
washing solution pH values less than about 8.5. A more complete
disclosure of these and other cationic surfactants useful herein
can be found ;n U.S. Patent 4,228,044, Cambre, issued October 14,
1980
Cationic surfactants are often used in detergent compos;tions
to prov;de fabric softening and/or antistatic benefits.
Antistat;c agents which provide some softening benef;t and which
are preferred here;n are the quaternary ammonium salts described
in U.S. Patent 3,936,537, Baskerville, Jr. et al., ;ssued February
3, 1976
Useful cat;on;c surfactants also include those described in
U.S. Patent 4,222,905, ~ockrell, issued September 16, 1980, and in
U.S. Patent 4,239,659, ~urphy, issued December 16, 198
B. Sodium PhosPhate
The second required ingredient, present in the instant
granular detergent composition at a level of from about 5 to 70
weight /O1 preferably from about 10 to 40 weight %, most preferably
about 15 to 3~ weight %, is sodium phosphate.
Sod;um phosphates for use herein may be sodium orthophosphate
(Na3P04), sodium pyrophosphate ~Na4P207), sodium tripolyphosphate
(NasP301o), and/or sodium metaphosphate (NaP03) and amorphous
phosphate glasses. Tripolyphosphate generally has better
detergency than pyrophosphate, which is better than
orthophosphate. Metaphosphate and many of the phosphate glasses
(supercooled solutions) are equal to or better than
tripolyphosphate in detergency, but they are undesirable in that
they can be unstable at normal crutcher pH and they may form
sticky product.
I Sodium tripolyphosphate is an especially good bu;lder and,
along with sodium pyrophosphate, is preferred for use herein.
Sodium tripolyphosphate is formed by condensing together three
orthophosphate molecules w;th el;m;nat;on of water, yield;ng a
straight chain molecule. It may be anhydrous or hydrated. Some
hydrolysis (reversion~ occurs during processing of the sodium
tripolyphosphate (STPP). Therefore the actual builder ratio
(versus formulated ratio) may consist of a higher ratio of STPP to
pyrophosphate.
0 The instant granular detergent composit;on preferably
comprises from about 1 to 10 weight % sodium tripolyphosphate
(STPP). It is preferred that th;s granular laundry detergent
compos;tion have a phosphate builder system comprising:
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(a) crutched phosphate builder selected from S~PP and TSPP
and mixtures thereof; wherein the crutched builder ;s in
spray-dried detergent granules; and
(b) admixed phosphate builder selected from S~PP and TSPP
and mixtures thereof; and
wherein (a) and (b) have a ratio of from about 1:25 to about 25:1;
the phosphate builder system having from 0 to about 50% of the
adm;xed TSPP by weight of the phosphate builder system, according
to pending U.S. Patent Application Serial No. 231,108, Beerse et
al, f;led August 11, 1988.
Most useful herein are sodium pyrophosphate salts, which can
be obta;ned commercially or can be formed by neutralization of the
corresponding pyrophosphoric acids or acid salts. Readily
a~ailable commercially are tetrasodium pyrophosphate (TSPP~
Na4P207 and its decahydrate Na4P207.10H20, sodium acid
pyrophosphate or "acid pyro" Na2H2P207 and its hexahydrate
Na2H2P207.6H20, and pyrophosphoric acid H~P207. The generic
formula for the anhydrous forms of these compounds can be ex-
pressed as NaxHyp2o7~ where x and y are integers having the sum of
4~
The sodium pyrophosphate herein can be tetrasodium
pyrophosphate (TSPP; preferred), trisodium pyrophosphate, d;sodium
pyrophosphate, monosodium pyrophosphate, or mixtures thereof.
These may be anhydrous (preferred) or hydrated.
C. Sodium Carbonate
The third re~uired ingredient in the instant granular
detergent composition is present at a level o~ from about S to 70
weight %, preferably from about 8 to 50 weight %, most preferably
from about 11 to 30 weight %, and is sodium carbonate. Ssdium
carbonate tNa2C03) can easily be obtained commercially.
a. Potassium Salts ~
The fourth required ingredient herein, which is present at a
le~el of from about 0.1 to 10 weight rO, preferably from about 0.5
to 5 weight %, most preferably ~rom about 1 to 3 ~eight %, is
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potassium salt. When thP potassium salt is sprayed on the
sodium carbonate rather than being crutched or admixed in the
granular detergent composition (see below), the preferred amount
of potassium sa1t is from about 0.l to 2 weight %, preferably
from about 0.2 to l weight %.
Of the potassium salts, inorganic potassium salts are
preferred, and are more preferably selected from the group
consisting of potassium chloride (KCl), potassium carbonate
(K2CO3), potassium sulfate (K2SO~), and mixtures thereof. These
are commercially available. Potassium carbonate is most
preferred.
Inorganic potassium salts may include dehydrated
(preferably) or hydrated tetrapotassium pyrophosphate (K4P2O7);
preferred), tripotassium pyrophosphate (HK3P2O7), dipotassium
pyrophosphate (H2K2P2O7), and monopotassium pyrophosphate
(H3KP2O7). Of the hydrates, those which are stable up to about
120F (48.9C) are preferred.
Other potassium salts for use herein are dehydrated
(preferably) or hydrated pentapotassium tripolyphosphate
(KsP3O10), tetrapotassium tripolyphosphate (HK4P301~),tripotassium
tripolyphosphate (H2K3P3O10), dipotassium tripolyphosphate
(H3K2P3O10), and monopotassium tripolyphosphate (~4KP3o10);
potassium hydroxide (KOH); potassium silicate; and potassium
neutralized surfactant such as linear potassium alkylbenzene
sulfonate, potassium alkyl sullate, and/or potassium
alkylpolyethoxylate.
Also suitable for use herein are salts of film forming
polymers as described in U.S. Patent 4,379,080, Murphy, issued
April 5, 1983, column 8, line ~4 to column l0, line 37, which
are either partially or wholly neutralized with potassium.
Particularly preferred are the potassium salts of copolymers of
acrylamide and acrylate having a molecular weight between about
4,000 and 20,000.
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It is preferred that the potassium salts herein have a
mean particle size of less than about 200 microns, more
preferably between 1 and 100 microns, most preferably between
about 1 and 10 micronsO
E. Other In~redients
Additional detergent inyredients suitable for inclusion in
a granular detergent compositlon may be added to the instant
composition. These include other detergency builders,
bleaches, bleach activators, suds boosters or suds suppressors,
anti-tarnish and anticorrosion agents, soil suspending agents,
soil release agents, germicides, pH adjustiny agents, non-
builder alkalinity sources, chelating agents, smectite clays,
enzymes, enzyme-stabilizing agents and perfumes. See U.S.
Patent 3,936,537, issued February 3, 1976 to Baskerville, Jr.
et al.
Bleaching agents and a~tivators are described in U.S.
Patent 4,412,934, Chung et al., issued November 1, 1983, and in
U.S. Patent 4,483,781, Hartman, issued November 20, 1984.
Chelating agents are also described in U.S. Patent 4,663,071,
Bush et al., from column 17, line 54 through Column 18, line 68.
Suds modifiers are also optional ingredients and are describsd
in U.S. Patents 3,933,672, issued January 20, 1976 to Bartoletta
et al., and 4,136,045, issued January 23, 1979 to Gault et al.
Suitable smectite clays for use herein are descrihed in
U.S. Patent 4,762,645, Tucker et al, issued August 9, 1988,
Column 6, line 3 through Column 7, line 24. Suitable additional
detergency builders for use herein are enumerated in the
Baskerville patent, Column 13, line 54 through Column 16, line
16, and in U.S. Patent 4,663,071, Bush 8~ al., issued May 5,
1987.
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F. Process
Also included in the instant invention is a process for
improving solubility or dispersibility of a granular detergent
composition as described above. The process comprises:
(a) producing detergent granules comprising detergent
surfactant selected from the group consisting of
anionics, nonionics, zwitterionics, ampholytics,
cationics, and mixtures thereof; and sodium phosphate;
and
~b) admixins with said detergent granules sodium carbonate
and potassium salt;
wherein the final detergent composition comprises from about S to
70 weight % of the detergent surfactant, from about 5 to 70 weight
% sodium phosphate, from about 5 to 70 weight ~/0 sodium carbonate,
and from about 0.1 to 10 weight % of the potassium salt.
Preferably, this process comprises:
(a) forming a paste comprising sodium linear C10-l6
alkylbenzene sulfonate and sodium C12-l8 alkyl sulfate
in a ratio between 50:50 and 80:20;
(b) crutching the paste with sod;um pyrophosphate;
(c) spray drying the mixture of step (b) to form detergent
granules; and
(d) admixing the detergent granules with sodium carbonate
and inorganic potassium salt selected from the group
cons;sting of potassium chloride, potassium carbonate,
potassium sulfate, and mixtures thereof, and having a
mean part;cle size of less than about 200 microns;
wherein the final detergent composition comprises from about 12 to
20 weight % sodium linear C10-l6 alkylbenzene sulfonate and sodium
C12-l8 alkyl sulfate, from about 15 to 30 weight ~O sodium
pyrophosphate, from about 15 to 30 weight % sodium carbonate, and
from about 0.5 to 5 weight % of the inorganic potassium salt.
It is preferred that step (b) above additionally comprise
crutching the paste with sodium tripolyphosphate so that the ~inal
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detergent composition comprise~ from about I to 10 weight % sodium
tripolyphosphate.
Although the potassium salt and sodîum carbonate are
preferably admixed, step (d), in any order, they may be added in
S the crutcher, step tb).
Bleach and bleach activator and/or C12 13 a1kylpolyethoxylate
are preferably also admixed in step (d). Polyethylene glycol,
preferably of a molecular weight between about 6,000 and 12,000,
sodium silicate, sodium sulfate and/or brightener are preferably
added in the crutcher, step (b).
Instead of admixing or directly crutching the potassium salt,
an aqueous solution of the potassium salt is distributed on the
sodium carbonate in a preliminary step before admixing (preferred)
or crutching the coated sodium carbonate. The potassium salt may
(less preferably) be agglomerated ~ith the sodium carbonate in,
for example, a Schugi agglomerator using an aqueous solution of
the potassium salt at levels sufficient to cause agglomeration.
The distribution of the potassium salt may be by coating or,
preferably, by spraying an aqueous solution on the surface of the
sodium carbonate. Spraying on may be done in a Schugi
agglomerator with the blades down and minimal residence time so
the sodium carbonate is coated but not agglomerated. A rotating
spray drum may alternatively be used to spray an aqueous solution
of the potassium salt onto the sodium carbonate.
If the potassium salt (preferably inorganic salt, most
preferably potassium carbonate, potassium chloride or potassium
sulfate), is sprayed on, the percentage of it in the finished
product can be lower than if it is admixed ~or directly crutched~,
~ithout losing effectiveness. From about 0.1 to 10 weight %,
preferably from about 0.1 to 2 weight %, most preferably from
about 0.2 to 1 wei~ht % potassium salt may be sprayed on the
sodium carbonate. The potassium salt can be m;xed in water, at a
concentration at less than saturation for a given temperature, for
subsequent distribution over the surfaces of the sodium carbonate
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particles. The coated sodium carbonate is then incorporated into
the granular detergent composition.
Certain ratios of sodium carbonate, sodium pyrophosphate
and/or potassium salt are preferred, as follows, when th~
potassium salt is admixed:
More Most
Preferred Preferred Preferred
Potassium salt: 2:1 to 1:140 1:2 to 1:40 1:5 to 1:20
sod;um pyrophosphate
Potassium salt: 2:1 to 1:140 1:2 to 1:50 1:5 to 1:30
sodium carbonate
Sodium pyrophosphate: 15:1 to 1:15 5:1 to 1 6 1:1 to 1:2
sodium carbonate
Certain ratios of the above are preferred when the potassiu~
salt is sprayed on the sodium carbonate:
More Most
Preferred Preferred Preferrqd
Potassium salt: 3:1 to 1:280 1:2 to 1:80 1:5 to 1:20
sodium pyrophosphate
Potassium salt: 3:1 to 1:280 1:2 to 1:110 1:5 to 1:25
sodium carbonate
Sodium pyrophosphate: 14:1 to i:l4 5:1 to 1:6 1:1 to 2:1
sodium carbonate
The following examples illustrate the compositions and
processes of the present invention. All parts, percentages, and
ratios herein are by weight unless otherwise specified.
EXAMPLE I
A granular laundry detergent composition of the present
inYention is as follows:
30 Com~onent Active Weight %
Sodium C12.3 linear alkylbenzene sulfonate 8.66
Sodium C1~ 15 alkyl sulfate 4.14
Sodium tripolyphosphate 2.0g
Tetrasodium pyrophosphate 17.44
- 14 -
Sodium silicate 7.04
Pentasodium diethylenetriamine pentaacetate0.30
Polyethylene glycol 0.25
Sodium polyacrylate 0.88
Brightener 0.l1
Moisture 4.61
Sodium perborate monohydrate 4.32
Nonanoyloxybenzene sulfonate 5.04
Sodium carbonate 20.72
10 Potassium carbonate 4.80
Sodium sulfate/Miscellaneous 19.60
The process used to make this composition is as follows:
Stock Material Weiqht ~O
Step 1
Sodium C12,3 linear alkylbenzene 6.51
Sulfuric acid 5,47
Sodium C14 15 fatty alcohol 2.77
Sulfuric acid 2.57
Sodium hydroxide 4.39
Water 17.18
Sodium polyacrylate 2.14
Step 2
Polyethylene glycol 0.58
Tetrasodium pyrophosphate 17.16
25 Sodium tripolyphosphate 4.54
Sodium silicate 16.01
Sodium sulfate 12.51
Brightener 0.17
Pentasodiu~ diethylenetriamine pentaacetate1.05
30 ~e_~
Sodium perborate monohydrate 4.32
Nonanoyloxybenzene sulfonate 6.47
Sodium carbonate 20.72
Potassium rarbonate 4.~0
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The ingredients listed in step 1 are added together to form a
paste. This paste is then crutched with the ingredients listed in
step 2. This mixture is then spray dried to eYaporate the excess
moisture and form detergent granules. The ingredients listed in
step 3 are then admixed to form the finished granular detergent
composition.
The composition ("product") is eYaluated in a washing machine
test designed to simulate consumer wash conditions that promote
insoluble clump formation (cold water, product/clothes/water order
of addition, normal cycle, large load). V;sually, the insoluble
clumps appear as solid7 white masses, about 5 ~o 40 millimeters in
diameter and about 2 to 10 millimeters in length, which rema;n
bound in the washed cl othes or can be seen at the bottom of the
washing machine tub after the clothes are remoYed. In this test,
1 the composition containing potassium carbonate has little to no
product remaining while the same compositiôn without potassium
carbonate has a significant amount of product remaining as
insoluble clumps. Consumer complaint information suggests that
insoluble clumps remaining after washing are unacceptable.
YO Product Remaininq*
(at the end of wash/rinse)
Standard
Deviatio~
Product without potassium carbonate 7.5% 1.4
25 Product with potassium carbonate 0.7% 0.6
*These numbers represent the average across 3 replicates.
EXAMPLE II
A granular laundry detergent composition of the present
-invention is as follows:
30 Component Active Weight %
Sodium C12 3 linear alkylbenzene sulfonate 8.92
Sodium C14 15 alkyl sulfate 4.26
Sodium tripolyphosphate 2.15
Tetrasodium pyrophosphate 17.96
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- 16 -
Sodium silicate 7 75
Pentasodium d;ethylenetriamine pentaacetate0.31
Polyethylene glycol 0.26
Sodium polyacrylate 0.91
Brightener 0.12
Moisture 4-74
Sodium perborate monohydrate 4.44
Nonanoyloxybenzene sulfonate 5.19
Sodium carbonate 21.34
10 Sodium sulfate/Miscellaneous 20.20
Potassium chloride -1.98
The process used to make this composition is as follows:
Stock Material Weiqht X
Step l
lS Sodium C12.3 linear alkylbenzene 6.51
Sulfuric acid 5-47
Sodium C14 15 fatty alcohol 2.77
Sulfuric acid 2.57
Sodium hydroxide 4.39
Water 17.18
Sodium polyacrylate 2.14
Ste~ 2
Polyethylene glycol 0.58
Tetrasodium pyrophosphate 17.16
25 Sodium tripolyphosphate 4.54
Sodium silicate 16.01
Sodium sulfate 12.51
Bri~htener 0.17
Pentasodium diethylenetriamine pentaacetate1.05
30 SteP 3
Sodium perborate monohydrate 4.32
Nonanoyloxybenzene sulfsnate 6.47
Sodium carbonate 21.34
Potassium chloride* 1.98
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*Micronized to mean particle size of 1.5 microns.
The ingredients listed in step 1 are added together to form a
paste. This paste is then crutched with the ingredients listed in
step 2. This mixture is then spray dried to evaporate the excess
moisture and form detergent granules. The ingredients listed in
step 3 are then admixed to form the finished granular detergent
composition.
The composition ("product") is evaluated in a washing machine
test designed to simulate consumer wash conditions that promote
insoluble clump formation (cold water, product/clothes/water order
of addition, normal cycle, large load). Yisually, the insoluble
clumps appear as solid, white masses which remain bound in the
washed clothes or can be seen at the bottom of the washing machine
tub after the clothes are removed. In this test, the com,oosition
containing potassium chloride has significantly fewer insoluble
clumps than the same composition with no potassium chloride,
% Product Remainina* Standard
(at the end of wash/rinse) Deviation
Product without potass;um chloride 7.5% 1.4
Product w;th potassium chloride 1,0% 1.7
*These numbers represent the aYerage across 3 replicates.
EXAMPlE I I I
A granular laundry detergent composition of the present
invention is as follows:
25 Component Active We7~ht %
Sodium C12.3 linear alkylbenzene sulfonate ~.92
Sodium C14 15 alkyl sulfate 4.26
Sodium tripolyphosphate 2.15
Tetrasodium pyrophosphate 17.96
30 Sodium silicate 7.25
Pentasodium diethylenetriamine pentaacetate 0.31
Polyethylene glycol 0.2
Sodium polyacrylate 0.91
Brightener 0,12
- 18 -
Water 4 74
Sodium perborate monohydrate 4.~4
Nonanoyloxybenzene sulfonate 5.19
Sodium carbonate 21.34
Sodium sulfate/Miscellaneous 20.20
Potassium sulfate 1.98
The process used to make this composition is as follows:
Stock Material Weiqht Y0
Step l
Sodium C12,3 linear alkylbenzene 6.51
Sulfuric acid 5.47
Sodium C14 15 fatty alcohol 2.77
Sulfuric acid 2.57
Sodium hydroxide 4.39
Water 17.18
Sodium polyacrylate 2.14
Step 2
Polyethylene glycol 0.58
Tetrasodium pyrophosphate 17.16
20 Sodium tripolyphosphate 4.54
Sodium silicate 16.01
Sodium sulfate 12.51
Brightener 0.17
Pentasod;um diethylenetriamine pentaacetate 1.05
25 SteP 3
Sodium perborate monohydrate 4.32
Nonanoyloxybenzene sulfonate 6.47
Sodium carbonate 21.34
Potassium sulfate* 1.98
30 *Micronized to mean particle size of 1.5 microns.
The ingredients listed in step 1 are added together to form a
paste. Th;s paste is then crutched with the ingredients listed in
step 2. This mixture is then spray dried to evaporate the excess
moistllre and form detergent granules. The ingredients listed in
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step 3 are then admixed to form the finished granular detergent
somposition.
The composition ("productn) is evaluated in a washing machine
test designed to simulate consumer wash conditions that promote
insoluble clump formation (cold water, product/clothes/water order
of addition, normal cycle, large load). Visually, the insoluble
clumps appear as solid, white ~asses which remain bound in the
washed clothes or can be seen at the bottom of the washing machine
tub after the clothes are removed. In this test, the composition
containing potassium sulfate had little to no product rema;ning
while the same compos;tion with no potassium sulfate had a
s;gnificant amount of product remaining as insoluble clumps.
~O Product Rema;ninq* Standard
(at the end of wash/rinse) Deviation
Product without potassium sulfate 7~5% 1.4
Product with potassium sulfate 1.0% 0
*These numbers represent the aYerage across 3 replicates.
EXAMPLE IV
A granular laundry detergent composition of the present
20 invention is as follows:
Component Active Weiqht
Sodium C12 3 linear alkylbenzene sulfonate 9.10
Sodium C14 15 alkyl sulfate 4.35
Sodium tripolyphosphate 2.19
25 Tetrasodium pyrophosphate 18.32
Sodium silicate 7.39
Pentasodium diethylenetriam;ne pentaacetate 0.31
Polyethylene glycol 0.27
Sodium polyacrylate 0.92
30 Brightener 0.12
Water 4.84
Sodium perborate monohydrate ~.53
Nonanoyloxybenzene sulfonate 5.2g
Potassium sulfate coated sodium carbonate21.77
` ' ,
- 20 -
Sodium sulfate/Miscellanecus 20.59
The process used to make this composition is as fol10ws:
Stock Material Weiqht %
Step nl
Sodium C12,3 linear alkylbenzene 6.51
Sulfuric acid 5.47
Sodium C14 15 fatty alcohol 2.77
Sulfuric acid 2.57
Sodium hydroxide 4.39
Water 17.18
Sodium polyacrylate 2.14
Step 2
Polyethylene glycol 0.58
Tetrasodium pyrophosphate 17.16
15 Sod;um tripolyphosphate 4.54
Sodium silicate 16.01
Sodium sulfate 12.51
Brightener 0.17
Pentasodium diethylenetriamine pentaacetate 1.05
20 SteP 3
Potassium sulfate* 0.41
Water 1.22
Sodium carbonate 20.14
25 Sodium perborate monohydrate 4.32
Nonanoyloxybenzene sulfonate 6.47
*Micron ked to mean particle s;ze of 1.5 m;crons.
The ingredients listed in step 1 are added together to form a
paste. This paste is then crutched with the ingredients listed in
step 2. Th;s m;xture ;s then spray dried to evaporate the excess
moisture and form detergent granules. The f;rst two ingredients
listed in step 3 are then mixed together and sprayed onto the
sodium carbonate. Th;s sodium carbonate a10ng with the
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ingredients listed ;n step 4 are then admixed to form the f;nishedproduct.
The product is evaluated ;n a wash;ng mach;ne test des;gned
to simulate consumer wash conditions that promote insoluble clump
format;on (cold water, product/clothes/water order o~ addition,
normal cycle, large load). Visually, the clumps are white solid
masses which can be found bound up in the clothes or in the bottom
of the washer after the clothes are removed. In th;s test, the
product with potassium sulfate coated sodium carbonate showed
little to no product remaining while ths same product with
uncoated sod;um carbonate had a significant amount of product
remaining as ;nsoluble clumps.
% Product Remainlnq* Standard
(at the end of wash~r;nse) Dev;ation
15 Product without potassium sulfate 7.5% 1.4
Product with potassium sulfate 0.7% 1.2
*These numbers represent the average across 3 replicates.
EXAMPLE V
A granular laundry detergent composit;on is as follows:
20 Component Active Weiqht %
Sodium C12.3 linear alkylbenzene sulfonate 12.01
Sodium C14 15 alkyl sulfate 5.59
Sodium tripolyphosphate 33.73
Tetrasodium pyrophosphate 7.70
25 Sodium silicate 8.00
Sodium carbonate 9.17
Potassium carbonate 2.00
Sodium perborate monohydrate 0.40
Sodium polyacrylate 1.52
30 Enzyme 0.84
Silicone 0.16
Brightener 0.28
Polyethylene glycol 0.61
C12 13 alkylpolyethoxylate 0 10
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Sodium sulfate 8.9~
Perfume 0.40
Water 7-34
Miscellaneous 1.20
The process used to make this composition is as follows:
Step 1
Sodium C12 3 linear alkylbenzene, sodium C1~ 15 fatty
alcohol, sulfuric acid, sodium hydroxide7 sodium polyacrylate, and
water are added together to form a paste. This paste is thcn
crutched with the ingredients in step 2.
Step 2
Polyethylene glycol, tetrasodium pyrophosphate, sodium
tripolyphosphate, sodium silicate, sodium sulfate, and brightener
are then crutched with the paste formed in step 1. This mixture
;s then spray dried to evaporate the excess moisture and form
detergent granules.
Step_3
Sodium perborate monohydrate, sodium carbonate, potassium
carbonate~ silicone, C12 13 alkylpolyethoxylate, and enzyme are
admixed to form the finished product. Perfume is sprayed on.
The product is ~valuated in a washing machine test designed
to simulate consumer wash conditions that promote insoluble clump
formation ~cold water, product/clothes/water order of addition,
normal cycle, large load). In this test, the product with
potassium carbonate showed a significant reduction in insoluble
clumps (Y0 product remaining) compared to the same product without
potassium carbonate.
/0 Product Remain_n3~
(at the end of wash/rinse) Standard
Product w;thout potassium carbonate 32.3% 2.4
Product with potassium carbonate 3.5% 3.5
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Note: ~he number associated with the no-potassium product is an
average of 2 replicates. The number associated with the potassium
product is an aYerage of 3 replicates.
EXAMPLE Yl
A granular laundry detergent composition is as follows:
Component e5~1Y3_~19hh_~
Sodium C12.3 linear alkylbenzene sulfonate 9.49
Sodium C14 15 alkyl sulfate 4.06
Tetrasodium pyrophosphate 8.67
10 Crutched sodium tripolyphosphate 16.07
Admixed sodium tripolyphosphate ~ 5.86
Sodium silicate 8.18
Sodium carbonate 20.04
Potassium carbonate 2.00
15 Sod;um perborate monohydrate 4.18
Nonanoyloxybenzene sulfonate 5.91
Pentasodium diethylenetriamine pentaacetate 0.4g
Enzymè 0.63
Sodium polyacrylate 1.10
20 Brightener
Polyethylene glycol 0.34
Sodiùm sulfate 9.72
C12 13 alkylpolyethoxylate 0.5
Perfume 0.25
Water 2.00
Miscellaneous 0.32
The process used to make th;s composit;on is as follows:
SteDI
Sodium Cl~.3 linear alkylbenzene, sodium C14 15 fatty
alcohol, sulfur;c acid, sodium hydroxide, sodium polyacrylate~ and
water are added together to form a paste. This paste is then
crutched with the ingredients in step 2.
7~ 2~ ~
- 24 -
Step~2
Polyethylene glycol, tetrasodium pyrophosphate, crutched
sodium tripolyphosphate, sodium silicatet sodium sulfate,
brightener9 and pentasodium diethylenetriamine pentaacetate are
crutched with the paste formed in step 1. This mixture is then
spray dried to evaporate the excess moisture and form detergent
granules.
Step 3
Oxygen bleach, bleach activator, sodium carbonate, potassium
carbonate, admixed sodium tripolyphosphate, and C12 13
alkylpolyethoxylate9 and enzyme are then admixed to form the
finished product. Perfume is sprayed on.
The product is evaluated in a washing machine test designed
to simulate consumer wash conditions that promote insoluble clump
formation (cold water, product/clothes/water order of addition,
normal cycle, large load). In this test, the product with
potassium carbonate showed a significant reduction in insoluble
clumps (% product remaining) compared to the same product without
potassium carbonate.
% Product Remaininq*
(at the end of wash/rinse)Standard
Dev1at~on
Product without potassium carbonate 8.2% 6.0
Product with potassium carbonate 1.9% 3.4
Note: These numbers represent the average across 3 replicates.
EXAMPLE VII
A granular laundry detergent of the present invention is as
follows:
Component Active Weiqht %
30 Alkylpolyethoxylate 7.52
Sodium tripolyphosphate 21.42
Sodium carbonate 51.90
Sodium silicate 4.95
Oxygen bleach 2.03
35 Enzyme ~Protease) 0.85
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- 25 -
Brightener 0.26
Carboxymethyl cellulose 0.29
Perfume 0.24
Sodium sulfate/miscellaneous 1.31
Moisture 4.48
Potassium sulfate 4.76
This composition is based on laboratory analysis of a
representative sample of a competitive granular laundry detergent
product. The product is eva1uated in a washing machine test
designed to simulate consumer wash conditions that promote
insoluble clump formation (cold water, product/clothes/water order
of addition normal cycle, large load). Visually, the clumps are
white solid masses which can be found bound up in the clothes or
in the bottom of the washer after the clothes are removed. In
this test, the product with potassium sulfate showed a significant
reduction in insoluble clumps compared to the same product without
potassium sulfate.
% Product Remainin~
(at the end of wash/r;nse)Standard
Deviation
Product without potassium sulfate 5.8 5.0
Product with potassium sulfate 0.7 1.2
* These numbers represent the average across 6 replicates.
WHAT IS CLAIMED IS:
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