CA1275019A - Granular detergent compositions having improved solubility - Google Patents

Granular detergent compositions having improved solubility

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Publication number
CA1275019A
CA1275019A CA000520140A CA520140A CA1275019A CA 1275019 A CA1275019 A CA 1275019A CA 000520140 A CA000520140 A CA 000520140A CA 520140 A CA520140 A CA 520140A CA 1275019 A CA1275019 A CA 1275019A
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Prior art keywords
composition
weight
base granules
builder material
detergent builder
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CA000520140A
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French (fr)
Inventor
Richard Hansen
Jeffrey Elijah Moore
Brett Alan Evans
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Procter and Gamble Co
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Procter and Gamble Co
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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/37Mixtures of compounds all of which are anionic
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/02Preparation in the form of powder by spray drying
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065High-density particulate detergent compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/08Silicates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)

Abstract

Abstract Spray dried detergent granules containing high levels of surfactants are compacted and admixed with other ingredients to form a dense, rapidly dissolving detergent composition. The composition is prepared by: (1) forming base granules comprising, by weight: (a) from about 30%
to about 85% of a mixture of a C11-C13 alkylbenzene sulfonate surfactant and a C12-C16 alkyl sulfate surfactant in a weight ratio of sulfonate surfactant to sulfate surfactant of from about 4:1 to about 1:4; (b) an alkali metal silicate having a molar ratio of SiO2 to alkali metal oxide of from about 1.0 to about 3.2; the weight ratio of (a) to (b) being from about 1.5:1 to about 6:1; (c) from about 10% to about 60% of a water-soluble sulfate; and (d) from 0% to about 20% of a pyrophosphate or anhydrous Form I tripolyphosphate detergent builder material, or mixtures thereof. The base granules are prepared by drying an aqueous slurry comprising the above components; (2) admixing said base granules with from 0 to about 300%, by weight of the base granules, of a detergent builder material; (3) compacting said admix at a pressure of from about 20 to about 200 psi; (4) granulating the resulting compacted admix; and (5) admixing an additional 0% to about 300%, by weight of the base granules, of a detergent builder material. The composition has a bulk density of from about 0.55 to about 1.2 g/cc and an average particle size of from about 20 to about 1500 microns.

Description

~2~

GRANULAP~ D~TERGENT S~OMPOSITIONS
HAVING IMPROVED SOLUBII.~ Y
Jeffrey E. Moore Brett A. Evans Richard Hansen Technical Field The present invention re~ates to granMlar detergent compositions containing a specific mixture oP alkylben-zene sulfonate surfactant, alkyl sulfate surfactant, alkali metal silicate and water-soluble sulfate, The compositions are prepared by drying, preferably by spray-drying, an aqueous slurry comprising the above components. While the composi ions preferably also contain detergent builder materials, there should be relatively little or no pyrophospha~e or anhydrous Form I tripolyphosphate builder in that portion of the composition prepared by drying th~ slurry comprising the ~ sulfonate and sulfate surfactants, silicate and sulfate.
; Mixtures of alkylbenzene sulfonate and alkyl sulfate surfactants are desired for optimum detergency perform-ance. However, such mixtures tend to gel on contact with water. This can result in poor solubility of granules ; having high level~ of alkylbenzene sulfonate and alkyl sulfate surfactants, particularly when such granules are incorporated in dense detergent compositions.
It has now been found that very soluble granular detergent compositio~s containing high levels of alkyl-benzene sulfonate and alkyl sulfate surfactants can be obtained by drying an aqueous slurry comprising the surfactants, silicate in a weight ratio of surfactant to silicate within the range of from about l.5:l to about 6:l, sulfate and relatively little or no pyrophosphate or anhydrous Form I tripolyphosphate detergent builder material. In preferred compositions, these soluble detergent granules are admixed or agglomerated with builders and other optional detergent ingredients.
Particularly preferred compositions are obtained by admixing the soluble granules with builders, compacting the admix at relatively low pressures (e.g., about 20 to about 200 p5i), and optionally admixing additional builders and other ingredients to provide finlshed granular deter~ent compositions.
ackground Art U.5. Patent 4,028,283, Murata et al~ issued June 7, 1977, discloses granular detergents containing surfac-tants having a tendency to cake and an anticaking agent formed by reacting polyethylene glycol with an acid anhydride. The compositions can also contain 0-20% of other surfactants such as alkylbenzene sulfonates.
Spray-dried detergents containing mixtures of alkyl-benzene sulfonate and alkyl ethoxy sulfate surfactants, silicate and builders are exemplified.
U.S. Patent 4,141,841, McDanald, issued February 27, 1979, discloses granular detergents containing particulate antistatic/softening additives. In Example 8, the particles are mixed with spray-dried base granule containing about 27~ of a mixtuxe of alkylbenzene sul-fonate and alkyl ethoxy qulfate surfactants, 18% sili-cate and about 22~ sodium tripolyphosphate.
Japanese OPI 106509, publ shed August 21, 1979~
discloses spray-dried granular detergents containing 15-40% surfactant, 5-20~ silicate and no more than 12%
phosphate. The compositions are said to have good physical properties and to cause less deposition of insolubles on clothes.
Japanese OPI 72998 and 72999, published April 25, 1985, disclose dense granular detergents formed by high shear mixing of alkylbenz~ne sulfuric acid and alkyl sulfuric acid with sodium carbonate and water to cause neutralization, admixing other ingredients such as builders, and then crushing and yranulating the mixture.

~2~

Summary_of the Invention This invention relates to a granular detergent composition prepared by:
(1) forming base granules comprising, by weight:
(a) from about 30~ to about 85% of a mixture of a C11-C13 alkylbenzene sulfonate surfactant and a C12-C16 alkyl sulfate surfactant in a wleiyht ratio of sulfonate surfactant to sulfate surfactant of from about 4:1 to about 1:4;
(b) an alkali metal silicate having a molar ratio of SiO2 to alkali metal oxide of from about 1.0 to about 3.2 the weight ratio of ~a) to (b) being from about 1.5:1 to about 6:1;
(c) from about 10~ to about 60% of a water-soluble sulfate; and (d) from 0% to about 20% of a pyrophosphate or anhydrous Foxm I tripolyphosphate detergent builder material, or mixtures thereof, said ~ase granules prepared by drying an aqueous slurry comprising the above components;
(2) admixing said base granules with from 0% to about 300%, by weight of the base granules~ of a deter-gent builder material:
(3~ compacting said admix at a pressure of from about 20 to about 200 psi;
(4) granulating the rPsulting compacted admix; and (5~ admixing an additional 0% to about 300~, by weight of the base granules, of a detergent builder material;
said composition having a bulk density of from about 0.55 to about 1.2 g/cc and an average particle size of from about 20 to about 1500 microns.

~ ;27~19 Detailed Description of the Invention The granular detergent compositions of the present invention contain from about 30% to a~out 85~, preferably from about 35~ to about 60~, more preferably from about 40~ to about 50%, by weight of a mixture of Cll-C13 alkylbenzene sulfonate surfactant and ~12-C16 alkyl sulfate surfactant in a weight ratio of sulfonate surfactant to sulfate surfactant of from about 4:1 to about 1:4, pxeEerably fxom about 3:1 to about 1:3, more preferahly from a~out 2:1 to about 1:2.
Sulfonate surfactants useful herein are the water-soluble salts, particularly the alkali metal, ammonium and alkanolammonium (e.g., monoe~hanolammonium or tri-ethanolammonium) salts of alkylbenzene sulfonates in which the alkyl group contains from about 11 to about 13 carbon atoms, in straight chain or branched chain con-figuxation, e.g., those of the type described in U.S.
Patents 2,220,099 and 2,477,383. Preferred are linear straight chain alkyl-benzene sulfonates in which the average number of carbon atoms in the alkyl group is Erom about 12 to about 13.
Useful alkyl sulfate surfactants are the water-soluble salts, particularly the alkali metal, ammonium and alkanolam~onium (e.g., monoethanolammonium or triethanolammonium~ salts of C12-C16 linear or ~ranched alkyl sulfates. Preferred are those containing a C12-C15, especially C14-Cl5, linear ~l~yl group.
The compositions herein can a~so contain minor amounts ~generally less than about 30~, but preferably less than about 15~, by weight of the above sulfvnate and sulfate surfactants3 of other detergent surfactants Xnown in the art. These can include anionic, nonioni~, cationic, ampholytic and zwitterionic surfactants, such as those disclosed in U.S. Patent 3,919,678, Laughlin, et al, issued December 30, 1975, ~%~

~ 5 --The compositions ~f the present invention also contain an alkali metal silicate having a molax ratio of SiO2 to alkali metal oxide of from about 1.0 to about
3.2, preferably from about 1.6 to about 2.4~ Sodium silicate, particularly having a molar ratio of from about 1.6 to about 2.2, is preferred.
The alkali metal silicates can be purchased in either liquid or granular form. Silicate solutions or slurries can conveniently be used to avoid haviny to l dissolve the dried form in the aqueous slurry (e.q., crutcher mix) of the components herein.
In addition, the weight ratio of the alkylbenzene sulfonate plus alkyl sulfate surfactants herein to the alkali metal silicate should be from about 1.5:1 to about 6:1, preferably from about 2:1 to about 4:1, more preferably from about 2.5:1 to about 3.5:1.
The present compositions fur~her contain from about 10g to about 60~, preferably from about ~0~ to about 50%, by weight of a water~soluble ~preferably sodium) sulfate. Sodium sulfate is usually formed during the sulfationtsulfonation and neutrali~ation steps in the production of the alkylbenzene sulfonate and alkyl sulfate surfactants herein.
The compositions herein are prepared by drying an aqueous slurry comprisi~g the components, The slurry generally contains from about 25~ to about 70%, prefer-ably from about 40~ to about 60%, water, whereas the dried granules initially contain from about l~ to about 10%, preferably from abouk 1~ to about 3%, water~ Tlle drying operation can be accomplished by any convanient means, such as by using spray-drying towers, both counter-current and co-current, fluid heds, flash drying equipment, or industrial microwave or oven-drying equip~
ment. These are more fully described in U.S. Patent
4,019,998, Benson et al, issued April 26, 1977, ~7~

The granular detergents herein are very soluble in the wash water even though they contain high levels of alkylbenzene sulfonate and alkyl sulfate surfactants Good solubility is obtained when the weight ratio of total sulfonate plus sulfate surfactant to silicate is within the about 1.5:1 to about 6:1 range specified above. While not intending to be limited by theory, it is believed that this relatively high level of silicate provides structure and help~ to maintain integrity o~ the lo high surfactant granules and that this min~mizes gelling when the surfactants contact the wash water. However, if the ~ilicate level becomes too high ~e.g., a ~urfactant to silica~e ratio of l:l), overall solubility can suffer due to the formation of silicate insolubles. On the lS other hand, granules having a sur~actant to silicate ratio of, for example, a: 1, have insufficient structure and tend to be too mushy at these high surfactant levels.
For good solubility, the amount of pyxophosp31ate or anhydrous Form I tripolyphosphate deteryent builder material in the portion of the granular detergent obtained by drying an aqueous slurry of the essential components herein should also be minimized. Thus the compositions can contain from 0~ to about 2~, preferably from 0~ to about 15~, more preferab7y from 0~ to about 10%, by weight of such detergent builder material, or mixtures thereof. Most preferably, the compositions are substantially free of such detergent builder (e.g., they contain less than about 5~, preferably less than about 3%, by weight of builder~.
The compositions can contain up to about 60~, preferably ~rom about 1% to about 45~, by weight of other detergent builders, including those described in U.S. Patent 3,925,262, Laughlin et al, is~ued December 9, 1975. Builders are generally selec~ed from the various water-soluble alkali ~A

metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbon ates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates. Preferred are the alkali matal, especially sodium, salts of the above.
Specific examplPs of inorganic phosphate b~ilders are sodium and potassium tripolyphosphalte ~Form II or hydrated Porm I), polymeric metaphoslphate having a degree of polymerization o~ from about 6 to 2.1, and orthophosphate. Examples of polyphosphonate builders are the sodium and potassium salts of ethylene diphos-phonic acid, the sodium and potassium salts of ethane .
1-hydroxy~ diphosphonic acid and the sodium and potassium salts of ethane, 1,1,2-triphosphonic acid.
Other phosphorus builder compounds are disclosed in U.S.
Patents 3,159,581 3,213,030; 3,422,021; 3,422,137;
3,400,176; and 3,400,148~

Examples of nonphosphorus, inoxganic builders are sodium and potassium carbonate, bicarbonate, ses~uicar-bonate, and tetraborate decahydrate.
Water-soluble, nonphosphorus organic builders useful hexein include the various alkali metal, ammonium and substitu~ed ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates. Examples of polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylene diamine tetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benæene polycarboxylic acids, and citric acid.
Polymeric polycarboxylate bui~dexs are also described in U.S. Patent 3,30~,067, Diehl, issued March 7, 1967. Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic ~7~

acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylenemalonic acidO
Other useful builders herein are sodium and potas~
sium carboxymethyloxymalonate, carboxymethyloxysuc-cinate, cis-cyclohexanehexacarboxylate, cis-cyclopen tanetetracarboxylate, phloroglucinol trisulfonate, and the copolymers of maleic anhydride with vinyl methyl ether or ethylene. -..
Other suitable polycarboxylates are the polyacetal carboxylates described in U.S. Patent 4,144,226, issued March 13, 1979 to Crutchfield et al, and U.S. Patent 4,246,495, issued March 27, 1979 to Crutchfield et al, These polyacetal carboxylates can be prepared by bringng together under polymerization conditions an ester of glyoxylic aci.d and a polymerization initiator. The resulting polyacetal carboxylate ester is then attached to chemically stable end groups to stabilize the polyacetal carboxylate against rapid depolymerization in alkaline solution and converted to the corresponding salt.
:
A preferred phosphate builder is Form II sodium tripolyphosphate (STPj (pre~erably anhydrous). A
preferred builder for use in compositions that a.re substantially free of phosphate builders is soditLm citrate.
When admixed, the builders herein should have the same particle size as the remainder of the composition, as described hexeinafter.
~he above granular detergent compositions can be used as is as finished detergent compositions or as detergent additive compositionsO However, they are preferably used as (and hereinafter referred to as~
detergent base granule~ which are then admixed or agglomerated with builder material and with other ~v optional ingredients to provide finished detergent compositions exhibiting good solubility. Such finished compositions can comprise by weight from about 5% to about 50%, preferably from about 10% to about 40%, more preferably from about 12% to about 25%, of the alkylben-zene sulfonate and alkyl sulfate surfactants herein and from about 5% to about 95%, preferably from about 10% to about 85%~ more prefexably from about 15% to about 75%~
of detergent builder material, such as de~cribed above.
lG However, for best solubility, the amount of pyrophos-phate and anhydrous Form I tripolyphosphate should be minimized, i.e., the finished compositions preferably contain from 0% to about 20%, preferably from 0% to about 10%, of such material, or mixtures thereof.
The compositions can also contain minor amounts, generally less than 30%, preferably less than 20%, by weight of other ingredients usually included in deter-gent compositions. These include auxiliary detergent surfactants, color speckles, bleaching agent~ and bleach activators, suds boosters or suds suppressors, antitarnish and anticorrosion age~ts, soil suspending agents, soil release agentst dyPs, fillers, optical brighteners, germicides, pH adjusting agents, nonbuilder alkalinity sources, enzymes, enzyme-stabilizing agents and perfumes.
Agglomeration can be accompli~hed by agitating in the presence of a sllitable binder (e.g., in a fluidized bed, tumble mixer, or a rotating drum or pan) or by mechanically mixing under pressure (e.g., extruding, pressing, milling, compacting or pell~ti~ing). Final sizing can then be achieved by grinding and screening.
In a preferred embodiment, the detergent base granules are admixed with from 0~ to about 300%, pre-ferably from abc~ut 25% to about 200~, more preferably from about 50~ to about 150%, by weight of the base granules, of a detergent builder material such as ~2~

described above. The resulting admix is th~n preferably compacted at a relatively low pressure of from about 20 to about 200, preferably from about 40 to about 150, more preferably from about 50 to about 100, pounds per square inch (psi~. The composition is then preferably admixed with an additional 0% to about 300%, preferably from about 25~ to abou 200%, more preferably from about 50~ to about 150~, by weight of the base granules, of a detergent builder material. The above levels and types of builder material and compaction pressure are prefer-ably selected so that the final detergent composition has a bulk density of from about 0.55 to about 1.2;
preferably from about 0.65 to about 1.1, more preferably from about 0.7 to about 0.9 g/cc and an average particle size of from about 20 to about 1500 microns, preferably from about 50 to about 1200 microns, more preferably from about 100 to about 800 microns.
The above compaction step is preferably accom-plished by using equipment that applies a relatively uniform compaction pressure, for example, by using compaction rollers with smooth (i.e., noncorrugated3 surfaces. After compaction, the composition is prefer-ably granulated and screened to provide an average particle size similar to that desired for the final composition.
The following nonlimiting examples illustrate the detergent compositions of the present inven~ion~
All percentages, parts and rat~os are by weight unless otherwise specified.
Example I
The following granular detergent composi~ion was prepared.
Base Granules Grams Final Composi-Weight ~ tion ~er use Sodium C13 linear alkyl-benzene sulfonate 22.1 5.110 Sodium Clq 15 alkyl 5ulfate 22.1 5O110 Sodium silicate (1.6 ratio)13.7 3.172 Sodium sulfate 32.2 7.455 Polyethylene glycol (m. w~. 8000) 1.5 0.340 Sodium polyacrylate (m. wt. 4500) 2.0 0.453 C12-13 alcohol poly-ethoxylate (6) 3.0 0.680 Sodium diethylenetriamine pentaacetate 1.5 0.340 Moisture 2.0 0.462 23.12Z
Preblend Base granules 23.122 15 Sodium tripolyphosphate hexahydrate ~powdered fo~m) 20.576 43.698 Admix Preblend 43.698 20 Sodium tripolyphosphate hexahydrate ~granular) 19.429 Dye 0-003 Brightener 0.613 Suds suppressor prill comprising dimethylsilicone, silica, sodium tripolyphosphate and polyethylene glycol ~MW = 8000) 1.703 Protease 2.044 Sodium carbonate 4.000 71.490 Spray-On Admix 71.490 Mineral oil 0O710 72.200 The base granules were produced by spray-drying an aqueous crutcher mix of the components on a ten foot tower using a crutcher temperature of 200aF, a si2e 3-1/2 nozzle to make fine granules, and silicone deaeratants.
If the base granules contained more thall 2~ moisture, a second drying stage on a continuou~ fluid bed was per-formed to reduce moisture to 2~
The base granules were then admixed with powdered STP hexahydrate to form the preblend. The preblend was compacted at 50 psig roll pressure on a 4 in. by l0 in.
chilsonator, and screened to select a -14(1168 microns)/
+65(208 microns~ particle size cut ~Tyler mesh). Ovex-sized particles were collected and granulated on a Fitzmill using a 14 mesh screen and low rpm's. This was screened to select a -20~833 microns)/~48(295 microns) particle size cut. Both materials were dedusted by blowing off fines in a fluid bed dryer using ambient alr .
The admix was prepared at 400 pounds per batch in a drum mixer. Carbonate, granular STP twith dye sprayed~
on~ brightener, enzymes, and suds supressor prills were blended with the compacted mainstream product cut and regranulated overs. The ratio of mainstream product cut to overs was 7 to 1~ Mineral oil was sprayed on the final admix in 30 to 40 pound batches at a 1~ level using a Porberg Mixer.
The composition of Example 1 is preferably incor-porated into a laminated laundry product form~d from ~wo plies of water insoluble tissues, at least one of which is water permeable, which are ~aminated together. At least one of the plies has cup li~e depressions, sur-rounded by rims and the other ply being attached to the first ply at the rim to physically separate the cups.
In one embodiment the laminate is made with plies of the ~ 27~

tissue paper described by Trokhan in U.S. Patent 4,529,480, issued July 16, 7985. The tissue had good air permeabilit~ as set Eorth in U.S. Patent 4,170,565, Flesher et al, issued October 9, 1979. There are 12 cups, having about 20 cc capacity each and at least 8 of the cups are Eilled with about 9 gm (11 cc) of the detergent composition and the other cups are filled with at least one detergent adjuvant. Other materials which can be use~
to form suitable laminates and processes for forming suitable laminates are disclosed in U.S. Patent No.
4,638,907, issued January 27, 1987.
When the composition of Exa~ple 1 is incorporated itl said laminated laundry product, it exhibits superior solubil1ty.
Example II
The ~ollowing granular detergent composition can be prepared and used according to Example 1.
ase Granules Grams Final Composi-~ t~on per_use Sodium C13 linear alkyL-benzene sulfonate 15.?5 6.81 Sodium C14_15 alkyl sulate 15.75 6.81 Sodium silicate ~1.6 ratio) 7.88 3.41 Sodium sulfate 23.01 9.95 Polyethylene glycol (m. wt. 8000) a . 7~ 0.34 Sodium polyacrylate Im. wt. 45~0) 1.05 0.46 C12 13 alcohol poly-ethoxylate ~6) 1.57 0.68 Sodium citrate 32.15 13.90 Unreacted 0.35 0.15 Moisture 1.7 - ?3 43.23 Preblend Base granules 43.23 Sodium aluminosilicate (hydrated Zeolite A, avg. dia 3 microns) lA.90 Sodium carbonate 3.00 61.13 Admix Preblend 61.13 ~rishtener 0.53 Suds suppressor prill comprising dimethylsilicone, silica, sodium tripolyphosphate and polyethylene glycol IMW = 8000) 0.91 Protease . 1.00 63.57 WHAT IS CLAIMED IS:

Claims (24)

Claims:
1. A granular detergent composition prepared by:
(1) forming base granules comprising, by weight:
(a) from about 30% to about 85% of a mixture of a C11-C13 alkylbenzene sulfonate surfactant and a Cl2-C16 alkyl sulfate surfactant in a weight ratio of sulfonate surfactant to sulfate surfactant of from about 4:1 to about 1:4;
(b) an alkali metal silicate having a molar ratio of SiO2 to alkali metal oxide of from about 1.0 to about 3.2;
the weight ratio of (a) to (b) being from about 1.5:1 to about 6:1;
(c) from about 10% to about 60% of a water-soluble sulfate; and (d) from 0% to about 20% of a pyrophosphate or anhydrous Form I tripolyphosphate detergent builder material, or mixtures thereof;
said base granules prepared by drying an aqueous slurry comprising the above components;
(2) admixing said base granules with from 0% to about 300%, by weight of the base granules, of a detergent builder material;
(3) compacting said admix at a pressure of from about 20 to about 200 psi;
(4) granulating the resulting compacted admix; and (6) admixing an additional 0% to about 300%, by weight of the base granules, of a detergent builder material;
said composition having a bulk density of from about 0.55 to about 1.2 g/cc and an average particle size of from about 20 to about 1500 microns.
2. The composition of Claim 1 wherein the base granules comprise from about 35% to about 60% of the sulfonate and sulfate surfactants, in a weight ratio of sulfonate surfactant to sulfate surfactant of from about 2:1 to about 1:2.
3. The composition of Claim 2 wherein the sulfonate surfactant is sodium C12 C13 linear alkylbenzene sul-fonate and the sulfate surfactant is sodium C14-C15 linear alkyl sulfate.
4. The composition of Claim 1 wherein the weight ratio of (a) to (b) is from about 2.5:1 to about: 3.5:1.
5. The composition of Claim 3 wherein the weight ratio of (a) to (b) is from about 2:1 to about 4:1, and the alkali metal silicate is sodium silicate having a molar ratio of SiO2 to alkali metal oxide of from about 1.6 to about 2.4.
6. The composition of Claim l wherein the base granules comprise from 0% to about 10% of a pyrophosphate or anhydrous Form I tripolyphosphate detergent builder material, or mixtures thereof.
7. The composition of Claim 5 wherein the base granules are substantially free of pyrophosphate or anhydrous Form I tripolyphosphate detergent builder material.
8. The composition of Claim 1 wherein the base granules are admixed with from about 50% to about 150%, by weight of the base granules, of a detergent builder material in step (2).
9. The composition of Claim 8 wherein the detergent builder material comprises sodium tripolyphosphate hexahydrate.
10. The composition of Claim 1 wherein the admix of step (2) is compacted at a pressure of from about 40 to about 150 psi.
11. The composition of Claim 10 wherein the admix of step (2) is compacted at a pressure of from about 50 to about 100 psi.
12. The composition of Claim 10 wherein the compacted admix of step (3) is admixed with an additional from about 50% to about 150%, by weight of the base granules, of a detergent builder material.
13. The composition of Claim 1 having a bulk density of from about 0.7 to about 0.9 g/cc.
14. The composition of Claim 8 wherein the admix of step (2) is compacted at a pressure of from about 40 to about 150 psi.
15. The composition of Claim 14 wherein the compacted admix of step (3) is admixed with an additional from about 50% to about 150%, by weight of the base granules, of a detergent builder material.
16. The composition of Claim 7 wherein the base granules are admixed with from about 50% to about 150%, by weight of the base granules, of sodium tripolyphosphate hexahydrate in step (2).
17. The composition of Claim 16 wherein the admix of step (2) is compacted at a pressure of from about 50 to about 100 psi.
18. The composition of Claim 17 wherein the compacted admix of step (3) is admixed with an additional from about 50% to about 150%, by weight of the base granules, of a detergent builder material.
19. The composition of Claim 18 having a bulk density of from about 0.7 to about 0.9 g/cc.
20. The composition of Claim 1 wherein the base gran-ules further comprise up to about 60% by weight of detergent builder material, other than pyrophosphate or anhydrous Form I tripolyphosphate builders.
21. The composition of Claim 20 wherein the base gran-ules comprise from about 1% to about 45% by weight of detergent builder material, other than pyrophosphate or anhydrous Form I tripolyphosphate builders.
22. The composition of Claim 1 which is substantially free of phosphate builder materials.
23. The composition of Claim 22 further comprising sodium citrate.
24. A laminated laundry product comprising two plies of water insoluble tissue in which:
(1) at least one ply is water permeable;
(2) at least one ply defines more than one cup, each cup being surrounded by a rim of that ply;
(3) the second ply is sealed to the first ply at least at the rims of the cups to physically separate the cups so that the contents of the cups remain in place; and more than one cup contains the product of Claim 1.
DEH/rr(111/C36)
CA000520140A 1985-10-09 1986-10-08 Granular detergent compositions having improved solubility Expired - Lifetime CA1275019A (en)

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EP0220024A3 (en) 1988-11-09
JPH07116476B2 (en) 1995-12-13
JPS62169900A (en) 1987-07-27
DE3688821D1 (en) 1993-09-09
DE3688821T2 (en) 1994-03-10
EP0220024B1 (en) 1993-08-04
NZ217877A (en) 1989-10-27
AU6359786A (en) 1987-04-16
AU582519B2 (en) 1989-03-23
EP0220024A2 (en) 1987-04-29

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