EP0876473B1 - 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
EP0876473B1
EP0876473B1 EP96932960A EP96932960A EP0876473B1 EP 0876473 B1 EP0876473 B1 EP 0876473B1 EP 96932960 A EP96932960 A EP 96932960A EP 96932960 A EP96932960 A EP 96932960A EP 0876473 B1 EP0876473 B1 EP 0876473B1
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Prior art keywords
detergent
agglomerates
densifier
surfactant paste
erg
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EP96932960A
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German (de)
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EP0876473A1 (fr
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Scott William Capeci
David Robert Nassano
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Procter and Gamble Co
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Procter and Gamble Co
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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 first type of process involves spray-drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules.
  • 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 most important factors which govern the density of the resulting detergent granules are the density, porosity and surface area of the various starting materials and their respective chemical composition. These parameters, however, can only be varied within a limited range. Thus, a substantial bulk density increase only can be achieved by additional processing steps which lead to densification of the detergent granules.
  • 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 non-aqueous polyethylene glycol, having a melting point temperature of from 35 to 70°C, 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 viscosities referenced herein are measured at 70°C ( ⁇ 5°C) and at shear rates of about 1o 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 polyethylene glycol having a melting point temperature of from 35 to 70°C, introduced as non-aqueous polyethylene glycol, 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(CO 3 ) 2 , K 2 Ca(CO 3 ) 2 , Na 2 Ca 2 (CO 3 ) 3 , NaKCa(CO 3 ) 2 , NaKCa 2 (CO 3 ) 3 , K 2 Ca 2 (CO 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 polyethylene glycol having a melting point temperature of from 35 to 70°C, introduced as non-aqueous polyethylene glycol, from about 30% to about 95% of a detersive surfactant, and the balance water, the weight ratio of the surfactant paste to the dry detergent material is
  • the invention also provides a high density detergent composition made according to the process of the invention and its various embodiments.
  • 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 of the 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 of the process invention is extremely desirable in geographic areas which are especially sensitive to emission of pollutants into the atmosphere.
  • 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 comprises from about 30% to about 95%, preferably from about 60% to about 95% and, most preferably from about 70% to about 75%, by weight of a detergent surfactant in paste form.
  • the surfactant paste 12 includes polyethylene glycol, having a melting point temperature of from 35 to 70°C, to facilitate production of high density detergent agglomerates with improved flow properties. It has been found that by including non-aqueous polyethylene glycol in the surfactant paste 12 which at least partially replaces the water in the paste surprisingly 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 of the the non-aqueous polyethylene glycol and the balance water, and optionally, other conventional detergent ingredients.
  • the polyethylene glycol enhances agglomeration by providing a "binding" or "sticking" agent for the detergent components in the process.
  • the polyethylene glycol 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 preferably has a melting point of from about 40°C to about 60 °C, so that it can operate most effectively in the instant process.
  • 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(CO 3 ) 2 , K 2 Ca(CO 3 ) 2 , Na 2 Ca 2 (CO 3 ) 3 , NaKCa(CO 3 ) 2 , NaKCa 2 (CO 3 ) 3 , K 2 Ca 2 (CO 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 of the invention.
  • the ratio of the 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.
  • the first processing step can be successfully completed, under the process parameters described herein, in a high speed mixer/densifier which preferably is a Lödige CB mixer or similar brand mixer.
  • a high speed mixer/densifier which preferably is a Lödige 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 rpm to about 2500 rpm, more preferably from about 300 rpm to about 1600 rpm.
  • the mean residence time of the 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 are then fed into a lower or moderate speed mixer-densifier 16 during which further agglomeration and densification is carried forth.
  • This particular moderate speed mixer densifier used in the present process should include liquid distribution and agglomeration tools so that both techniques can be carried forth simultaneously. It is preferable to have the moderate speed mixer/densifier 16 to be, for example, a Lödige KM (Ploughshare) mixer. Drais® K-T 160 mixer or similar brand mixer.
  • the residence time in the moderate speed mixer densifier 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 rpm.
  • the high speed mixer/densifier and moderate speed mixer/densifier in combination impart a requisite amount of energy to form the desired agglomerates.
  • the moderate speed mixer/densifier imparts from about 5 ⁇ 10 10 erg/kg to about 2 ⁇ 10 12 erg/kg at a rate of from about 3 ⁇ 10 8 erg/kg-sec to about 3 ⁇ 10 9 erg/kg-sec to form free flowing high density detergent agglomerates.
  • the energy input and rate of input can be determined by calculations from power readings to the moderate speed mixer/densifier with and without granules, residence time of the granules in the mixer/densifier, and the mass of the granules in the mixer/densifier. Such calculations are clearly within the scope of the skilled artisan.
  • the density of the resulting detergent agglomerates exiting the moderate speed mixer/densifier 16 is at least 650 g/l, more preferably from about 700 g/l to about 875 g/l.
  • the detergent agglomerates are dried in a fluid bed dryer or similar apparatus to obtain the high density granular detergent composition which is ready for packaging and sale as a low dosage, compact detergent product at this point.
  • 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 of the resulting detergent agglomerates of the 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 having a median particle size of from about 400 microns to about 700 microns, and more preferably from about 400 microns to about 500 microns.
  • the phrase "median particle size" refers to individual agglomerates and not individual particles or detergent granules.
  • the combination of the above-referenced porosity and particle size results in agglomerates having density values of 650 g/l and higher Such a feature is especially useful in the production of low dosage laundry detergents as well as other grartular compositions such as dishwashing compositions.
  • the detergent agglomerates exiting the fluid bed dryer are further conditioned by cooling the agglomerates in a fluid bed cooler or similar apparatus as are well known in the art.
  • Another optional process step involves adding a coating agent to improve flowability and/or minimize over agglomeration of the detergent composition in one or more of the following locations of the instant process: (1) the coating agent can be added directly after the fluid bed cooler as shown by coating agent stream (preferred); (2) the coating agent may be added between the fluid bed dryer and the fluid bed cooler as shown by coating agent stream (3) the coating agent may be added between the fluid bed dryer and the moderate speed mixer/densifier as shown by stream and/or (4) the coating agent may be added directly to the moderate speed mixer/densifier and the fluid bed dryer as shown by stream.
  • the coating agent can be added in any one or a combination of streams.
  • 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 of the 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 As those skilled in the art are well aware, over agglomeration can lead to very undesirable flow properties and aesthetics of the final detergent product.
  • the process can comprises the step of spraying an additional binder in one or both of the mixer/densifiers.
  • the binder can comprise the same non-aqueous binder materials used in the surfactant paste described previously.
  • finishing step 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.
  • 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. -1 .
  • 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. Patent 3,664,961, Norris, issued May 23, 1972, and in U.S. Patent 3,919,678, Laughlin et al., issued December 30, 1975.
  • 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, Murphy, issued December 16, 1980.
  • anionics and nonionics are preferred and anionics are most preferred.
  • Nonlimiting examples of the preferred anionic surfactants useful in the surfactant paste include the conventional C 11 -C 18 alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C 10 -C 20 alkyl sulfates (“AS”), the C 10 -C 18 secondary (2,3) alkyl sulfates of the formula CH 3 (CH 2 ) x (CHOSO 3 - M + )CH 3 and CH 3 (CH 2 ) y (CHOSO 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-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the C 10 -C 18 alkyl alkoxy sulfates ("AE x S"; especially EO 1-7 ethoxy sulfates).
  • LAS C 11 -C 18 alkyl benz
  • exemplary surfactants useful in the paste of the invention include C 10 -C 18 alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C 10-18 glycerol ethers, the C 10 -C 18 alkyl polyglycosides and their corresponding sulfated polyglycosides, and C 12 -C 18 alpha-sulfonated fatty acid esters.
  • the conventional nonionic and amphoteric surfactants such as the C 12 -C 18 alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C 6 -C 12 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C 12 -C 18 betaines and sulfobetaines ("sultaines"), C 10 -C 18 amine oxides, and the like, can also be included in the overall compositions.
  • the C 10 -C 18 N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C 12 -C 18 N-methylglucamides. See WO 9,246,154.
  • sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C 10 -C 18 N-(3-methoxypropyl) glucamide.
  • the N-propyl through N-hexyl C 12 -C 18 glucamides can be used for low sudsing.
  • C 10 -C 20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C 10 -C 16 soaps may be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
  • the starting dry detergent material of the 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. Patent No. 4.605.509 (Procter & Gamble).
  • the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms of the 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 of the 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 Na z [(AlO 2 ) z .(SiO 2 ) y ]xH 2 O wherein z and y are integers of at least 6, the molar ratio of z to y is from about 1 to about 5 and x is from about 10 to about 264. More preferably, the aluminosilicate has the formula Na 12 [(AlO 2 ) 12 .(SiO 2 ) 12 ]xH 2 O 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.
  • aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaCO 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaCO 3 hardness/gram.
  • 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.
  • Nonlumiting examples of noncarbonate anions include those selected from the group consisting of chloride, sulfate, fluoride, 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(CO 3 ) 2 , K 2 Ca(CO 3 ) 2 , Na 2 Ca 2 (CO 3 ) 3 , NaKCa(CO 3 ) 2 , NaKCa 2 (CO 3 ) 3 , K 2 Ca 2 (CO 3 ) 3 , and combinations thereof.
  • An especially preferred material for the builder described herein is Na 2 Ca(CO 3 ) 2 in any of its crystalline modifications.
  • Suitable builders of the above-defined type are further illustrated by, and include, the natural or synthetic forms of any one or combinations of the following minerals: aceaite, Andersonite, Ashcroftine Y, Beyerite, Borcarite, Burbankite. Butschliite, Cancrinite, Carbocernaite, Carletonite.
  • the starting dry detergent material in the present process can include additional detergent ingredients and/or, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process.
  • adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressers, anti-tamish and anticorrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting 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.
  • Other builders can be generally selected from the various 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 of the above.
  • Preferred for use herein are the phosphates, carbonates, C 10-18 fatty acids, polycarboxylates, and mixtures thereof. More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate mono- and di-succinates, and mixtures thereof (see below).
  • crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity.
  • the layered sodium 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 amorphous 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 NaMSi x O 2x+ 1 .yH 2 O wherein M is sodium or hydrogen, x is from about 1.9 to about 4 and y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the formula NaMSi 2 O 5 .yH 2 O 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 orthophosphates.
  • 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.
  • nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of SiO 2 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.
  • 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.
  • polycarboxylates for use herein 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 bringing together under polymerization conditions an ester of glyoxylic acid 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, converted to the corresponding salt, and added to a detergent composition.
  • 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.
  • 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. 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 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.
  • 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.
  • 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 et al, issued May 5, 1987.
  • This Example illustrates the process of the 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 Lödige 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 of the shaft in the Lödige CB-30 mixer/densifier is about 1400 rpm and the mean residence time is about 10 seconds.
  • the contents from the Lödige CB-30 mixer/densifer are continuously fed into a Lödige 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 to control and prevent over agglomeration.
  • the detergent agglomerates are then screened with conventional screening apparatus resulting in a uniform particle size distribution.
  • composition of the detergent agglomerates exiting the fluid bed cooler is set forth in Table I below: TABLE I Component % Weight of Total Feed C 14-15 alkyl sulfate 22.5 C 12.3 linear alkylbenzene sulfonate 2.5 Aluminosilicate 35.2 Sodium carbonate 21.0 Polyethylene glycol (MW 4000) 1.5 Misc. (water, etc.) 12.3 100.0
  • Additional detergent ingredients including perfumes, enzymes, and other minors are sprayed onto the agglomerates described above in the finishing step to result in a finished detergent composition which is admixed with spray dried granules in a 60:40 weight ratio (agglomerates: spray dried granules).
  • the density of the resulting fully formulated detergent composition is 561 g/l, the median particle size is 450 microns.
  • the density of the agglomerates alone is 810 g/l.
  • Example III 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: TABLE III Component % Weight of Total Feed C 14-15 alkyl sulfate 22.7 C 12-13 linear alkylbenzene sulfonate 7.6 Aluminosilicate 34.5 Sodium carbonate 21.2 Polyethylene glycol (MW 4000) 1.5 Misc. (water, perfume, etc.) 12.5 100.0
  • Additional detergent ingredients including perfumes, brighteners and enzymes are sprayed onto the agglomerates described above in the finishing step to result in a finished detergent composition which is admixed with spray dried granules in a 60:40 weight ratio (agglomerates: spray dried granules).
  • the density of the resulting detergent composition is 560 g/l, the median particle size is 450 microns.
  • the density of the agglomerates alone is 860 g/l.

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Claims (8)

  1. Procédé pour préparer en continu une composition détergente de masse volumique élevée, caractérisé par les étapes consistant à
    (a) mélanger en continu une pâte tensioactive détergente et une matière détergente de départ sèche dans un dispositif de mélange / densification à vitesse élevée ayant un arbre avec une vitesse de rotation de 100 - 2500 tr/min pour obtenir des agglomérats détergents, dans lequel ladite pâte détergente comprend, en poids de ladite pâte tensioactive, 30 % à 95 % en poids de tensioactif détersif, 0,1 à 50 % en poids de polyéthylèneglycol ayant une température de point de fusion de 35 à 70°C et étant introduit comme du polyéthylèneglycol non aqueux, et le reste étant de l'eau,
    (b) mélanger lesdits agglomérats détergents dans un dispositif de mélange / densification à vitesse modérée fournissant 5.1010 erg/kg à 2.1012 erg/kg à un taux de 3x108 erg/kg.s à 3x109 erg/kg.s pour densifier et agglomérer davantage lesdits agglomérats détergents ; et
    (c) sécher lesdits agglomérats détergents de manière à former ladite composition détergente de masse volumique élevée.
  2. Procédé selon la revendication 1, dans lequel la pâte tensioactive comprend 60 à 95 % en poids de tensioactif détersif et 1 à 15 % en poids de polyéthylèneglycol.
  3. Procédé selon l'une quelconque des revendications précédentes, dans lequel le polyéthylèneglycol est le polyéthylèneglycol 4000.
  4. Procédé selon l'une quelconque des revendications précédentes, dans lequel ladite matière de départ sèche est un adjuvant choisi dans le groupe constitué par des aluminosilicates, des silicates lamellaires cristallins, le carbonate de sodium, Na2Ca(CO3)2, K2Ca(CO3)2, Na2Ca2(CO3)3, NaKCa(CO3)2, NaKCa2(CO3)3, K2Ca2(CO3)3, et leurs mélanges.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en outre par l'étape consistant à ajouter un agent de revêtement après ledit dispositif de mélange / densification à vitesse modérée, dans lequel ledit agent de revêtement est choisi dans le groupe constitué par des aluminosilicates, des carbonates, des silicates et leurs mélanges.
  6. Procédé selon l'une quelconque des revendications précédentes, dans lequel le temps de séjour moyen desdits agglomérats détergents dans ledit dispositif de mélange / densification à vitesse élevée est dans la plage de 2 secondes à 45 secondes.
  7. Procédé selon l'une quelconque des revendications précédentes, dans lequel le temps de séjour moyen desdits agglomérats détergents dans ledit dispositif de mélange / densification à vitesse modérée est dans la plage de 0,5 minute à 15 minutes.
  8. Procédé pour préparer en continu une composition détergente de masse volumique élevée, caractérisé par les étapes consistant à
    (a) mélanger en continu une pâte tensioactive détergente et une matière détergente de départ sèche caractérisée par un adjuvant choisi dans le groupe constitué par des aluminosilicates, des silicates lamellaires cristallins, le carbonate de sodium, Na2Ca(CO3)2, K2Ca(CO3)2, Na2Ca2(CO3)3, NaKCa(CO3)2, NaKCa2(CO3)3, K2Ca2(CO3)3, et leurs mélanges, dans un dispositif de mélange / densification à vitesse élevée ayant un arbre avec une vitesse de rotation de 100 - 2500 tr/min pour obtenir des agglomérats détergents, dans lequel ladite pâte détergente comprend, en poids de ladite pâte tensioactive, 70 % à 95 % d'un tensioactif détersif et 0,1 à 50 % de polyéthylèneglycol ayant une température de point de fusion de 35 à 70°C et étant introduit comme du polyéthylèneglycol non aqueux, et le reste étant de l'eau, le rapport en poids de ladite pâte tensioactive à ladite matière détergente sèche étant de 1 : 10 à 10 : 1 ; mélanger lesdits agglomérats détergents dans un dispositif de mélange / densification à vitesse modérée fournissant 5.1010 erg/kg à 2.1012 erg/kg à un taux de 3x108 erg/kg.s à 3x109 erg/kg.s pour densifier et agglomérer davantage lesdits agglomérats détergents,
    (b) sécher lesdits agglomérats détergents ; et
    (c) ajouter un agent de revêtement pour obtenir ladite composition détergente de masse volumique élevée ayant une masse volumique d'au moins 650 g/l.
EP96932960A 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 Expired - Lifetime EP0876473B1 (fr)

Applications Claiming Priority (3)

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US52828395A 1995-09-14 1995-09-14
US528283 1995-09-14
PCT/US1996/014279 WO1997010326A1 (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

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EP0876473B1 true EP0876473B1 (fr) 2006-06-28

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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)
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GB9805193D0 (en) * 1998-03-10 1998-05-06 Unilever Plc Process for preparing granular detergent compositions
US6906022B1 (en) 1998-09-25 2005-06-14 The Procter & Gamble Company Granular detergent compositions having homogenous particles and process for producing same
DE69941983D1 (de) * 1998-09-25 2010-03-18 Procter & Gamble Körnige waschmittelzusammensetzungen mit homogenen teilchen sowie verfahren zu ihrer herstellung
DE19959915A1 (de) * 1999-12-11 2001-07-05 Henkel Kgaa Niotensidgranulate durch Prillen
EP2451930A1 (fr) * 2009-07-09 2012-05-16 The Procter & Gamble Company Procédé continu de fabrication d'une composition de détergent pour le linge

Citations (1)

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Publication number Priority date Publication date Assignee Title
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

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DE69332270T3 (de) * 1992-06-15 2006-08-17 The Procter & Gamble Company, Cincinnati Verfahren zum herstellen von kompakten waschmittelzusammensetzungen
US5486303A (en) * 1993-08-27 1996-01-23 The Procter & Gamble Company Process for making high density detergent agglomerates using an anhydrous powder additive
CN1136824A (zh) * 1993-10-15 1996-11-27 普罗格特-甘布尔公司 制造高密度洗涤剂颗粒的连续方法
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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JPH11512473A (ja) 1999-10-26
ATE331780T1 (de) 2006-07-15
CN1202198A (zh) 1998-12-16
EP0876473A1 (fr) 1998-11-11
CN1126811C (zh) 2003-11-05
CA2232071C (fr) 2001-10-30
DE69636309D1 (de) 2006-08-10
BR9610548A (pt) 1999-07-06
WO1997010326A1 (fr) 1997-03-20
AR003570A1 (es) 1998-08-05
DE69636309T2 (de) 2007-05-31
MX9802022A (es) 1998-08-30
ES2263162T3 (es) 2006-12-01
CA2232071A1 (fr) 1997-03-20

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