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WO1997010326A1 - Procede de fabrication d'une composition detergente haute densite a partir d'une pate de tensioactif contenant un liant non aqueux - Google Patents

Procede de fabrication d'une composition detergente haute densite a partir d'une pate de tensioactif contenant un liant non aqueux Download PDF

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Publication number
WO1997010326A1
WO1997010326A1 PCT/US1996/014279 US9614279W WO9710326A1 WO 1997010326 A1 WO1997010326 A1 WO 1997010326A1 US 9614279 W US9614279 W US 9614279W WO 9710326 A1 WO9710326 A1 WO 9710326A1
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WO
WIPO (PCT)
Prior art keywords
detergent
agglomerates
densifier
speed mixer
surfactant paste
Prior art date
Application number
PCT/US1996/014279
Other languages
English (en)
Inventor
Scott William Capeci
David Robert Nassano
Original Assignee
The Procter & Gamble Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Priority to EP96932960A priority Critical patent/EP0876473B1/fr
Priority to CA002232071A priority patent/CA2232071C/fr
Priority to BR9610548A priority patent/BR9610548A/pt
Priority to DE69636309T priority patent/DE69636309T2/de
Priority to JP9512001A priority patent/JPH11512473A/ja
Publication of WO1997010326A1 publication Critical patent/WO1997010326A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3707—Polyethers, e.g. polyalkyleneoxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/10—Carbonates ; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/1233—Carbonates, e.g. calcite or dolomite
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/1273—Crystalline layered silicates of type NaMeSixO2x+1YH2O
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

  • the present invention generally relates to a process for producing a high density detergent composition. More particularly, the invention is directed to a continuous process during which high density detergent agglomerates are produced by feeding a surfactant paste with a non-aqueous binder and adjunct dry starting detergent material into two serially positioned mixer/densifiers. The process produces a high density detergent composition with unexpectedly improved flow properties which can be commercially sold as a low dosage or "compact" detergent composition.
  • the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant.
  • a binder such as a nonionic or anionic surfactant.
  • the present invention meets the aforementioned needs in the art by providing a process which produces a high density detergent composition in the form of agglomerates directly from a surfactant paste and adjunct dry starting detergent ingredients.
  • the surfactant paste has a relatively low amount of water, but retains its transportability and processability by including a sufficient amount of a non-aqueous binder to which the formation of agglomerates having unexpectedly improved flow properties are attributed.
  • the agglomerates exiting the instant process are less sticky and do not require recycling of oversized agglomerate particles back into the process to the extent of previous processes.
  • the oversized agglomerate particles can be appropriately sized by more economical grinding processes subsequent to the instant process.
  • agglomerates refers to particles formed by agglomerating more porous starting detergent ingredients (particles) which typically have a smaller median particle size than the formed agglomerates. All percentages and ratios used herein are expressed as percentages by weight (anhydrous basis) unless otherwise indicated. All documents are incorporated herein by reference. All viscosities referenced herein are measured at 70°C ( ⁇ 5°C) and at shear rates of about 10 to 100 sec - 1 .
  • a process for preparing a crisp, free flowing, high density detergent composition comprises the steps of: (a) continuously mixing a detergent surfactant paste and dry starting detergent material into a high speed mixer/densifier to obtain detergent agglomerates, wherein the surfactant paste includes, by weight of the surfactant paste, from about 0.1% to about 50% of a non-aqueous binder, from about 30% to about 95% of a detersive surfactant, and the balance water; (b) mixing the detergent agglomerates in a moderate speed mixer/densifier to further densify and agglomerate the detergent agglomerates; and (c) drying the detergent agglomerates so as to form the high density detergent composition.
  • the process comprises the steps of: (a) continuously mixing a detergent surfactant paste and a dry starting detergent material comprising a builder selected from the group consisting of aluminosilicates, crystalline layered silicates, sodium carbonate, Na 2 Ca(C0 3 )2, K 2 Ca(C0 3 )2, Na 2 Ca2(C0 3 )3, NaKCa(C0 3 ) 2 , NaKCa 2 (C0 3 ) 3> K 2 Ca (C0 3 ) 3 , and mixtures thereof, into a high speed mixer/densifier to obtain detergent agglomerates, wherein said surfactant paste includes, by weight of said surfactant paste, from about 0.1 % to about 50% of a non-aqueous binder, from about 30% to about 95% of a detersive surfactant, and the balance water, the weight ratio ofthe surfactant paste to the dry detergent material is from about 1 : 10 to about 10: 1 ; (b) mixing the detergent a builder selected from the group consist
  • FIG. 1 is a flow chart illustrating a preferred process in which two agglomerating mixer/densifiers, fluid bed dryer, fluid bed cooler and screening apparatus are serially positioned in accordance with the invention.
  • the present process is used in the production of low dosage detergent agglomerates directly from starting detergent ingredients rather than conventional "post-tower” detergent granules.
  • post-tower detergent granules we mean those detergent granules which have been processed through a conventional spray-drying tower or similar apparatus.
  • the process ofthe invention allows for production of low dosage detergents in an environmentally conscious manner in that the use of spray drying techniques and the like which typically emit pollutants though their towers or stacks into the atmosphere is eliminated. This feature ofthe process invention is extremely desirable in geographic areas which are especially sensitive to emission of pollutants into the atmosphere.
  • Fig. 1 presents a flow chart illustrating the instant process and various embodiments thereof.
  • the invention entails continuously mixing into a high speed mixer/densifier 10 several streams of starting detergent ingredients including a surfactant paste stream 12 and a dry starting detergent material stream 14.
  • the surfactant paste 12 preferably comprises from about 30% to about 95%, preferably from about 60% to about 85% and, most preferably from about 70% to about 75%, by weight of a detergent surfactant in paste form.
  • the surfactant paste 12 includes a non-aqueous binder to facilitate production of high density detergent agglomerates with improved flow properties. It has been found that by including a non-aqueous binder in the surfactant paste 12 which at least partially replaces the water in the paste su ⁇ risingly results in the formation of agglomerates having substantially improved flow properties.
  • the non-aqueous binder in the paste not only improves the agglomerates ultimately formed by the instant process, but also retains the processability and transportability of the paste in that the viscosity remains low enough for such tasks.
  • the surfactant paste also comprises from about 0.1% to about 50%, more preferably from about 1% to about 15%, and most preferably from about 2% to about 8%, by weight ofthe non-aqueous binder and the balance water, and optionally, other conventional detergent ingredients.
  • the binder enhances agglomeration by providing a "binding" or "sticking" agent for the detergent components in the process.
  • the particular binder need only be non-aqueous in nature, it preferably has a viscosity of from about 100 cps to about 100,000 cps, most preferably from about 1000 cps to about 25,000 cps. Also, it is preferable for the binder to have a melting point of from about 35 °C to about 70 °C, most preferably of from about 40 °C to about 60 °C, so that it can operate most effectively in the instant process.
  • the binder is preferably selected from the group consisting of anionic surfactants, nonionic surfactants, polyethylene glycol, polyvinyl pyrrolidone polyacrylates, citric acid and mixtures thereof. The most preferable binder is polyethylene glycol.
  • the dry starting detergent material 14 comprises from about 20% to about 50%, preferably from about 25% to about 45% and, most preferably from about 30% to about 40% of an aluminosilicate or zeolite builder, and from about 10% to about 40%, preferably from about 15% to about 30% and, most preferably from about 15% to about 25% of a sodium carbonate.
  • the builder is selected from the group consisting of aluminosilicates, crystalline layered silicates, sodium carbonate, Na 2 Ca(C0 3 )2, K Ca(C0 3 ) , Na 2 Ca 2 (C0 3 ) 3 , NaKCa(C0 3 ) 2 , NaKCa 2 (C0 3 ) 3 , K Ca 2 (C0 3 ) 3 , and mixtures thereof.
  • additional starting detergent ingredients several of which are described hereinafter may be mixed into high speed mixer/densifier 10 without departing from the scope ofthe invention.
  • the ratio ofthe surfactant paste 12 to the dry starting detergent material 14 is from about 1 : 10 to about 10: 1 , more preferably from about 1 :4 to about 4: 1 and, most preferably from about 2: 1 to about 2:3. It has been found that the flrst processing step can be successfully completed, under the process parameters described herein, in a high speed mixer/densifier 10 which preferably is a Lodige CB mixer or similar brand mixer. These types of mixers essentially consist of a horizontal, hollow static cylinder having a centrally mounted rotating shaft around which several plough-shaped blades are attached.
  • the shaft rotates at a speed of from about 100 ⁇ m to about 2500 ⁇ m, more preferably from about 300 ⁇ m to about 1600 ⁇ m.
  • the mean residence time ofthe detergent ingredients in the high speed mixer/densifier 10 is preferably in range from about 2 seconds to about 45 seconds, and most preferably from about 5 seconds to about 15 seconds.
  • the resulting detergent agglomerates formed in the high speed mixer/densifier 10 are then fed into a lower or moderate speed mixer/densifier 16 during which further agglomeration and densification is carried forth
  • This panicular moderate speed mixer/densifier 16 used in the present process should include liquid distribution and agglomeration tools so that both techniques can be carried forth simultaneously
  • the moderate speed mixer/densifier 16 should be, for example, a Lodige KM (Ploughshare) mixer, Drais® K-T 160 mixer or similar brand mixer
  • the residence tune in the moderate speed mixer/densifier 16 is preferably from about 0 5 minutes to about 15 minutes, most preferably the residence time is about 1 to about 10 minutes
  • the liquid distribution is accomplished by cutters, generally smaller in size than the rotating shaft, which preferably operate at about 3600 ⁇ m
  • the high speed mixer/densifier 10 and moderate speed mixer/densifier 16 in combination preferably impart a requisite amount of energy to form the desired agglomerates More particularly, the moderate speed mixer/densifier imparts from about 5 x 10 -0 erg/kg to about 2 x 10*-- erg kg at a rate of from about 3 x 10 ⁇ erg/kg-sec to about 3 x 10 ⁇ erg/kg-sec to form free flowing high density detergent agglomerates
  • the energy mput and rate of mput can be determined by calculations from power readings to the moderate speed mixer/densifier with and without granules, residence time of the granules m the mixer/densifier, and the mass ofthe granules in the mixer/densifier Such calculations are clearly withm the scope ofthe skilled artisan
  • the density ofthe resulting detergent agglomerates exiting the moderate speed mixer/densifier 16 is at least 650 g/I, more preferably from
  • the detergent agglomerates produced by the process preferably have a surfactant level of from about 25% to about 55%, more preferably from about 35% to about 55% and, most preferably from about 45% to about 55%
  • the particle porosity ofthe resulting detergent agglomerates ofthe composition is preferably in a range from about 5% to about 20%, more preferably at about 10%
  • a low porosity detergent agglomerate provides a dense or low dosage detergent product, to which the present process is primarily directed
  • an attribute of dense or densified detergent agglomerates is the relative particle size
  • the present process typically provides agglomerates havmg a median particle size of from about 400 microns to about 700 microns, and more preferably from about 400 microns to about 500 microns
  • Another optional process step involves adding a coating agent to improve flowability and/or minimize over agglomeration ofthe detergent composition in one or more ofthe following locations ofthe instant process: (1) the coating agent can be added directly after the fluid bed cooler 20 as shown by coating agent stream 22 (preferred); (2) the coating agent may be added between the fluid bed dryer 18 and the fluid bed cooler 20 as shown by coating agent stream 24; (3) the coating agent may be added between the fluid bed dryer 18 and the moderate speed mixer/densifier 16 as shown by stream 26; and/or (4) the coating agent may be added directly to the moderate speed mixer/densifier 16 and the fluid bed dryer 18 as shown by stream 28. It should be understood that the coating agent can be added in any one or a combination of streams 22. 24, 26, and 28 as shown in Fig. 1.
  • the coating agent stream 22 is the most preferred in the instant process.
  • the coating agent is preferably selected from the group consisting of aluminosilicates, silicates, carbonates and mixtures thereof.
  • the coating agent not only enhances the free flowability ofthe resulting detergent composition which is desirable by consumers in that it permits easy scooping of detergent during use, but also serves to control agglomeration by preventing or minimizing over agglomeration, especially when added directly to the moderate speed mixer/densifier 16. As those skilled in the art are well aware, over agglomeration can lead to very undesirable flow properties and aesthetics ofthe final detergent product.
  • finishing step 32 in Fig. 1 Another optional step ofthe instant process entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients, collectively referenced as the finishing step 32 in Fig. 1.
  • the finishing step encompasses spraying perfumes, brighteners and enzymes onto the finished agglomerates to provide a more complete detergent composition.
  • Such techniques and ingredients are well known in the art.
  • the detergent surfactant paste used in the process is preferably in the form of a non-aqueous viscous paste.
  • This so-called viscous surfactant paste has a viscosity of from about 5.000 cps to about 100.000 cps, more preferably from about 10.000 cps to about 80.000 cps. The viscosity is measured at 70°C and at shear rates of about 10 to 100 sec.” ' .
  • the surfactant itself, in the viscous surfactant paste is preferably selected from anionic, nonionic. zwitterionic, ampholytic and cationic classes and compatible mixtures thereof. Detergent surfactants useful herein are described in U.S.
  • Useful cationic surfactants also include those described in U.S. Patent 4,222,905, Cockrell, issued September 16, 1980, and in U.S. Patent 4,239,659, Mu ⁇ hy, issued December 16, 1980, both of which are also inco ⁇ orated herein by reference.
  • anionics and nonionics are preferred and anionics are most preferred.
  • Nonlimiting examples ofthe preferred anionic surfactants useful in the surfactant paste include the conventional C* J -C J g alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C *o-C 2 o alkyl sulfates ("AS"), the C j Q -C - g secondary (2,3) alkyl sulfates of the formula CH 3 (CH 2 ) x (CHOS0 3 " M + ) CH 3 and CH 3 (CH 2 ) y (CHOS0 3 " M + ) CH 2 CH 3 where x and (y + 1 ) are integers of at least about 7, preferably at least about 9, and M is a water-solubiiizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the C - Q-C • g alkyl alkoxy sulfates ("AE X S”; especially EO 1-7 ethoxy sulfates).
  • exemplary surfactants useful in the paste ofthe invention include and Cj -C j g alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C* ⁇ -
  • the conventional nonionic and amphoteric surfactants such as the C* 2 -C* g alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and Cg-C* 2 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy /propoxy ), C * -C* g betaines and sulfobetaines ("sultaines”), Cj Q -Ci g amine oxides, and the like, can also be included in the overall compositions.
  • AE alkyl ethoxylates
  • sulfobetaines especially Cj Q -Ci g amine oxides, and the like
  • Cj Q -Ci g amine oxides can also be included in the overall compositions.
  • the C ⁇ Q-C • g N-alkyl polyhydroxy fatty acid amides can also be used.
  • Typical examples include the C* 2 -C* g N-methylglucamides. See WO 9,206, 154.
  • Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C i Q-C • g N-(3-methoxypropyl) glucamide. The N-propyl through N-hexyl C • -C • g glucamides can be used for low sudsing.
  • C * ⁇ -C 2 conventional soaps may also be used. If high sudsing is desired, the branched-chain C- ⁇ -C j g soaps may be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
  • Dry Detergent Material T e starting dry detergent material ofthe present process preferably comprises a detergent aluminosilicate builder which are referenced as aluminosilicate ion exchange materials and sodium carbonate.
  • the aluminosilicate ion exchange materials used herein as a detergent builder preferably have both a high calcium ion exchange capacity and a high exchange rate. Without intending to be limited by theory, it is believed that such high calcium ion exchange rate and capacity are a function of several interrelated factors which derive from the method by which the aluminosilicate ion exchange material is produced.
  • the aluminosilicate ion exchange materials used herein are preferably produced in accordance with Corkill et al, U.S.
  • the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms ofthe instant aluminosilicate do not exhibit the as high of an exchange rate and capacity as provided by the sodium form.
  • the aluminosilicate ion exchange material preferably is in over dried form so as to facilitate production of crisp detergent agglomerates as described herein.
  • the aluminosilicate ion exchange materials used herein preferably have particle size diameters which optimize their effectiveness as detergent builders.
  • particle size diameter represents the average particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic determination and scanning electron microscope (SEM).
  • the preferred particle size diameter ofthe aluminosilicate is from about 0.1 micron to about 10 microns, more preferably from about 0.5 microns to about 9 microns. Most preferably, the particle size diameter is from about 1 microns to about 8 microns.
  • the aluminosilicate ion exchange material has the formula
  • the aluminosilicate has the formula Na 12 [(Al ⁇ 2) 12 .(Si0 2 ) 12 ]xH 2 0 wherein x is from about 20 to about 30, preferably about 27.
  • These preferred aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X.
  • Naturally-occurring or synthetically derived aluminosilicate ion exchange materials suitable for use herein can be made as described in Krummel et al, U.S. Patent No. 3,985,669, the disclosure of which is incorporated herein by reference.
  • the aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaC0 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC0 3 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further characterized by their calcium ion exchange rate which is at least about 2 grains Ca ++ /gallon/minute/-gram gallo ⁇ , and more preferably in a range from about 2 grains Ca "H" /gallon minute/-gram/gallon to about 6 grains Ca ++ /gallon minute/-gram gallon.
  • a water-soluble cation selected from the group consisting of hydrogen, water-soluble metals, hydrogen, boron, ammonium, silicon, and mixtures thereof, more preferably, sodium, potassium, hydrogen, lithium, ammonium and mixtures thereof, sodium and potassium being highly preferred
  • Nonlimiting examples of noncarbonate anions include those selected from the group consisting of chloride, sulfate, fluo ⁇ de, oxygen, hydroxide, silicon dioxide, chromate, nitrate, borate and mixtures thereof
  • Preferred builders of this type in their simplest forms are selected from the group consisting of Na 2 Ca(C0 3 ) 2 , K 2 Ca(C0 3 ) 2 , Na 2 Ca (C0 3 ) 3 , NaKCa(C0 3 ) 2 , NaKCa (C0 3 ) 3 , K 2 Ca (C0 3 ) 3 , and combinations thereof
  • An especially preferred material for the builder described herem is Na Ca(C0 3 ) 2 in any of its crystalline modifications
  • Suitable builders of the above-defined type are further illustrated by, and mclude, the natural or synthetic forms of any one or combinations ofthe following mineralssammlungite, Andersonite, AshcroftineY, Beye ⁇ te, Borcarite, Burbankite, Butschlnte, Canc ⁇ nite, Carbocemaite, Carletonite, Davyne, DonnayiteY, Fairchildite, Fer ⁇ su ⁇ te, Franzinite, Gaudefroyite, Gaylussite, Girvasite, Gregoryite, Jouravskite, KamphaugiteY, Kettne ⁇ te, Khanneshite, LepersonniteGd, Liottite, MckelveyiteY, Microsommite, Mroseite, Natrofairchildite, Nyerereite, RemonditeCe, Sacrofanite, Schrockinge ⁇ te, Shortite, Su ⁇ te, Tunisite, Italyite, Tyrolite, Vishnevite, and Zemko ⁇
  • T e starting dry detergent matenal in the present process can mclude additional detergent ingredients and/or, any number of additional ingredients can be l ⁇ co ⁇ orated in the detergent composition durmg subsequent steps ofthe present process
  • adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressers, anti-tarnish and anticorrosion agents, soil suspend g agents, soil release agents, germicides, pH adjusting agents. non-builder alkalinity sources, chelatmg 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 , inco ⁇ orated herem by reference.
  • Other builders can be generally selected from the va ⁇ ous water-soluble, alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates
  • alkali metal especially sodium
  • salts ofthe above Preferred for use herein are the phosphates, carbonates, C • Q. ⁇ g fatty acids, polycarboxylates, and mixtures thereof More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate mono- and di-succinates, and mixtures thereof (see below)
  • silicates prefer magnesium ions over calcium ions, a feature necessary to insure that substantially all of the "hardness" is removed from the wash water.
  • These crystalline layered sodium silicates are generally more expensive than amo ⁇ hous silicates as well as other builders. Accordingly, in order to provide an economically feasible laundry detergent, the proportion of crystalline layered sodium silicates used must be determined judiciously.
  • the crystalline layered sodium silicates suitable for use herein preferably have the formula
  • the crystalline layered sodium silicate has the formula NaMSi 2 0 5 .yH 2 0 wherein M is sodium or hydrogen, and y is from about 0 to about 20.
  • inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from about 6 to 21, and oithophosphates.
  • polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1 -hydroxy- 1, 1 -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, all of which are inco ⁇ orated herein by reference.
  • nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of SiO. to alkali metal oxide of from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4.
  • Water-soluble, nonphosphorus organic builders useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates.
  • 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, benzene polycarboxylic acids, and citric acid.
  • Polymeric polycarboxylate builders are set forth in U.S. Patent 3,308,067, Diehl, issued March 7, 1967, the disclosure of which is inco ⁇ orated herein by reference.
  • Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylene malonic acid.
  • Some of these materials are useful as the water-soluble anionic polymer as hereinafter described, but only if in intimate admixture with the non-soap anionic surfactant.
  • Other suitable polycarboxylates for use herein are the polyacetal carboxylates described in
  • Particularly preferred polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tartrate monosuccinate and tartrate disuccinate described in U.S. Patent 4,663,071 , Bush et al., issued May 5, 1987, the disclosure of which is inco ⁇ orated herein by reference.
  • Bleaching agents and activators 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, both of which are inco ⁇ orated herein by reference.
  • 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, inco ⁇ orated herein by reference.
  • Suds modifiers are also optional ingredients and are described 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., both inco ⁇ orated herein by reference.
  • Suitable smectite clays for use herein are described in U.S. Patent 4,762,645, Tucker et al, issued August 9, 1988, Column 6, line 3 through Column 7, line 24, incorporated herein by reference.
  • Suitable additional detergency builders for use herein are enumerated in d e Baskerville patent. Column 13, line 54 through Column 16, line 16, and in U.S. Patent 4,663,071, Bush et al, issued May 5, 1987, both inco ⁇ orated herein by reference.
  • EXAMPLE I This Example illustrates the process ofthe invention which produces free flowing, crisp, high density detergent composition in the form of agglomerates.
  • Two feed streams of various detergent starting ingredients are continuously fed, at a rate of 1270 kg hr, into a L ⁇ dige CB-30 mixer/densifier, one of which comprises a surfactant paste containing surfactant and the non-aqueous binder, polyethylene glycol, and the other stream containing starting dry detergent material containing aluminosilicate and sodium carbonate.
  • the rotational speed ofthe shaft in the L ⁇ dige CB-30 mixer/densifier is about 1400 ⁇ m and the mean residence time is about 10 seconds.
  • the contents from the L ⁇ dige CB-30 mixer/densifer are continuously fed into a L ⁇ dige KM 600 mixer/densifer for further agglomeration during which the mean residence time is about 6 minutes.
  • the resulting detergent agglomerates are then fed to a fluid bed dryer and then to a fluid bed cooler, the mean residence time being about 10 minutes and 15 minutes, respectively.
  • a coating agent, aluminosilicate is fed about midway down the moderate speed mixer/densifier 16 to control and prevent over agglomeration.
  • the detergent agglomerates are then screened with conventional screening apparatus resulting in a uniform particle size distribution.
  • Table I The composition ofthe detergent agglomerates exiting the fluid bed cooler is set forth in Table I below:
  • the density ofthe resulting fully formulated detergent composition is 561 g/1, the median particle size is 450 microns.
  • the density ofthe agglomerates alone is 810 g/1.
  • Example II This Example illustrates another process in accordance with the invention in which the steps described in Example I are performed except the coating agent, aluminosilicate, is added after the fluid bed cooler as opposed to in the moderate speed mixer/densifier
  • the composition of the detergent agglomerates exiting the fluid bed cooler after the coating agent is added is set forth in Table III below:
  • the density ofthe resulting detergent composition is 560 g/1, the median particle size is 450 microns.
  • the density ofthe agglomerates alone is 860 g/1.

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Abstract

L'invention concerne un procédé de fabrication d'agglomérats détergents haute densité, celle-ci équivalant au moins à 650 g/l. Le procédé comprend les étapes suivantes: (a) mélange continu d'une pâte de tensioactif détergent et d'un produit de départ détergent sec dans un mélangeur/densificateur à grande vitesse, en vue d'obtenir des agglomérats détersifs, ladite pâte comprenant, en poids, entre 0,1 et 50 % environ de liant non aqueux, entre 70 et 95 % environ de tensioactif détergent, le solde étant de l'eau; (b) mélange des agglomérats détersifs dans un mélangeur/densificateur à vitesse modérée, en vue de pousser la densification et l'agglomération des agglomérats détersifs et c) séchage desdits agglomérats détersifs en vue de former la composition détergente haute densité. Le procédé peut comporter une ou plusieurs étapes de traitement supplémentaire, à savoir par exemple: d'adjonction d'un agent d'enduction après le mélangeur/densificateur à vitesse modérée en vue de faciliter et de réguler l'agglomération.
PCT/US1996/014279 1995-09-14 1996-09-06 Procede de fabrication d'une composition detergente haute densite a partir d'une pate de tensioactif contenant un liant non aqueux WO1997010326A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP96932960A EP0876473B1 (fr) 1995-09-14 1996-09-06 Procede de fabrication d'une composition detergente haute densite a partir d'une pate de tensioactif contenant un liant non aqueux
CA002232071A CA2232071C (fr) 1995-09-14 1996-09-06 Procede de fabrication d'une composition detergente haute densite a partir d'une pate de tensioactif contenant un liant non aqueux
BR9610548A BR9610548A (pt) 1995-09-14 1996-09-06 Processo para preparação de uma composição detergente de alta densidade a partir de uma pasta tensoativa contendo um aglutinante não-aquoso
DE69636309T DE69636309T2 (de) 1995-09-14 1996-09-06 Verfahren zur herstellung eines kompaktwaschmittels aus einer tensidpaste mit wasserfreiern binder
JP9512001A JPH11512473A (ja) 1995-09-14 1996-09-06 非水性バインダーを含有する界面活性剤ペーストからの高密度洗剤組成物の製法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US52828395A 1995-09-14 1995-09-14
US08/528,283 1995-09-14

Publications (1)

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WO1997010326A1 true WO1997010326A1 (fr) 1997-03-20

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EP (1) EP0876473B1 (fr)
JP (1) JPH11512473A (fr)
CN (1) CN1126811C (fr)
AR (1) AR003570A1 (fr)
AT (1) ATE331780T1 (fr)
BR (1) BR9610548A (fr)
CA (1) CA2232071C (fr)
DE (1) DE69636309T2 (fr)
ES (1) ES2263162T3 (fr)
WO (1) WO1997010326A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999046359A1 (fr) * 1998-03-10 1999-09-16 Unilever Plc Procede de preparation de compositions detergentes granulaires
WO2000018877A1 (fr) * 1998-09-25 2000-04-06 The Procter & Gamble Company Compositions de detergent granulaires comportant des particules homogenes et procede de production de celles-ci
EP1106678A3 (fr) * 1999-12-11 2003-06-04 Henkel Kommanditgesellschaft auf Aktien Granules de surfactant nonionique et procédé d'obtention
US6906022B1 (en) 1998-09-25 2005-06-14 The Procter & Gamble Company Granular detergent compositions having homogenous particles and process for producing same

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011005803A1 (fr) * 2009-07-09 2011-01-13 The Procter & Gamble Company Procédé continu de fabrication d'une composition de détergent pour le linge

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993025378A1 (fr) * 1992-06-15 1993-12-23 The Procter & Gamble Company Procede de preparation de compositions detersives compactes
WO1995006109A1 (fr) * 1993-08-27 1995-03-02 The Procter & Gamble Company Procede de fabrication d'agglomerats detersifs de masse volumique elevee
WO1995010595A1 (fr) * 1993-10-15 1995-04-20 The Procter & Gamble Company Procede continu pour produire un detergent granulaire a haute densite
US5431857A (en) * 1994-01-19 1995-07-11 The Procter & Gamble Company Process for producing a high density detergent composition having improved solubility by agglomeration of anionic surfactants and an agglomerating agent
WO1995032276A1 (fr) * 1994-05-20 1995-11-30 The Procter & Gamble Company Procede de fabrication d'un detergent a haute densite a partir d'ingredients detergents de depart

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993025378A1 (fr) * 1992-06-15 1993-12-23 The Procter & Gamble Company Procede de preparation de compositions detersives compactes
WO1995006109A1 (fr) * 1993-08-27 1995-03-02 The Procter & Gamble Company Procede de fabrication d'agglomerats detersifs de masse volumique elevee
WO1995010595A1 (fr) * 1993-10-15 1995-04-20 The Procter & Gamble Company Procede continu pour produire un detergent granulaire a haute densite
US5431857A (en) * 1994-01-19 1995-07-11 The Procter & Gamble Company Process for producing a high density detergent composition having improved solubility by agglomeration of anionic surfactants and an agglomerating agent
WO1995032276A1 (fr) * 1994-05-20 1995-11-30 The Procter & Gamble Company Procede de fabrication d'un detergent a haute densite a partir d'ingredients detergents de depart

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999046359A1 (fr) * 1998-03-10 1999-09-16 Unilever Plc Procede de preparation de compositions detergentes granulaires
WO2000018877A1 (fr) * 1998-09-25 2000-04-06 The Procter & Gamble Company Compositions de detergent granulaires comportant des particules homogenes et procede de production de celles-ci
US6906022B1 (en) 1998-09-25 2005-06-14 The Procter & Gamble Company Granular detergent compositions having homogenous particles and process for producing same
EP1106678A3 (fr) * 1999-12-11 2003-06-04 Henkel Kommanditgesellschaft auf Aktien Granules de surfactant nonionique et procédé d'obtention

Also Published As

Publication number Publication date
MX9802022A (es) 1998-08-30
CN1126811C (zh) 2003-11-05
ES2263162T3 (es) 2006-12-01
EP0876473B1 (fr) 2006-06-28
CA2232071A1 (fr) 1997-03-20
CA2232071C (fr) 2001-10-30
ATE331780T1 (de) 2006-07-15
DE69636309D1 (de) 2006-08-10
CN1202198A (zh) 1998-12-16
BR9610548A (pt) 1999-07-06
EP0876473A1 (fr) 1998-11-11
AR003570A1 (es) 1998-08-05
JPH11512473A (ja) 1999-10-26
DE69636309T2 (de) 2007-05-31

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