EP0915959B1 - Preparation of low density detergent agglomerates containing silica - Google Patents

Preparation of low density detergent agglomerates containing silica Download PDF

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Publication number
EP0915959B1
EP0915959B1 EP97934909A EP97934909A EP0915959B1 EP 0915959 B1 EP0915959 B1 EP 0915959B1 EP 97934909 A EP97934909 A EP 97934909A EP 97934909 A EP97934909 A EP 97934909A EP 0915959 B1 EP0915959 B1 EP 0915959B1
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Prior art keywords
detergent
agglomerates
silica
density
process according
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EP97934909A
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German (de)
English (en)
French (fr)
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EP0915959A1 (en
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Steven Barrett Rogers
Paul Amaat France
James Peyton Hutchins
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Procter and Gamble Co
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Procter and Gamble Co
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    • 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
    • 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

Definitions

  • the present invention generally relates to a process for producing a low density detergent composition. More particularly, the invention is directed to a process during which low density detergent agglomerates are produced by feeding a liquid acid precursor of a surfactant and dry starting detergent material including a silica material and a neutralizing agent into a high speed mixer followed by a drying apparatus. The process produces a free flowing, low density detergent composition which can be commercially sold as a conventional non-compact detergent composition or used as an admix in a low dosage, "compact" detergent product.
  • 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, shape, 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, flexibility in the substantial bulk density can only be achieved by additional processing steps which lead to lower densities of the detergent granules.
  • the present invention meets the aforementioned needs in the art by providing a process which produces a low density (less than 500 g/l) detergent composition directly from starting ingredients such as a liquid acid precursor of a surfactant and dry detergent ingredients.
  • the dry ingredients include a silica material which ultimately is agglomerated such that it forms part of or is in the agglomerate particles themselves rather than "coated" on the outer surface of the agglomerates.
  • this provides a low density agglomerate composition having improved physical properties.
  • the process does not use the conventional spray drying towers currently used and is therefore more efficient, economical and flexible with regard to the variety of detergent compositions which can be produced in the process.
  • the process is more amenable to environmental concerns in that it does not use spray drying towers which typically emit particulates and volatile organic compounds into the atmosphere.
  • agglomerates refers to particles formed by agglomerating detergent granules or particles which typically have a smaller mean particle size than the formed agglomerates. All percentages used herein are expressed as “percent-by-weight” unless indicated otherwise. All viscosities described herein are measured at 70°C and at shear rates between about 10 to 50 sec -1 , preferably at 25 sec -1 .
  • a process for preparing low density detergent agglomerates having a density of below 500 g/l comprises the steps of: (a) agglomerating a liquid acid precursor of a detergent surfactant and dry starting detergent material in a high speed mixer to obtain detergent agglomerates, wherein the dry starting detergent material includes a silica material and an alkaline inorganic material; and (b) drying the detergent agglomerates so as to form the detergent composition having a density of less than 500 g/l.
  • another process for preparing low density detergent agglomerates having a density of below 500 g/l comprises the steps of: (a) agglomerating a liquid acid precursor of a detergent surfactant and dry starting detergent material in a high speed mixer to obtain detergent agglomerates, wherein the dry starting detergent material includes a fumed silica material and an alkaline inorganic material; (b) mixing the detergent agglomerates in a moderate speed mixer to further agglomerate the detergent agglomerates; and (c) drying the detergent agglomerates so as to form the low density detergent composition having a density of less than 500 g/l.
  • the low density detergent composition made by any of the process embodiments described herein is also provided.
  • the present invention is directed to a process which produces free flowing, low density detergent agglomerates having a density of below 500 g/l, preferably from 350 g/l to 500 g/l.
  • the process produces low density detergent agglomerates from a liquid acid precursor of a detergent surfactant, typically of an anionic surfactant.
  • a detergent surfactant typically of an anionic surfactant.
  • the present process is used in the production of normal as opposed to low dosage detergents whereby the resulting detergent agglomerates can be used as a detergent or as a detergent additive. It should be understood that the process described herein can be continuous or batch depending upon the desired application.
  • starting detergent materials are fed into a mixer for agglomeration.
  • the agglomeration step is carried forth initially in a high speed mixer after which an optional moderate speed mixer may follow if further agglomeration is desired.
  • the starting detergent materials preferably include a liquid acid precursor of a surfactant, preferably an anionic surfactant, and dry detergent material including silica and an alkaline inorganic material, the components of which are described more fully hereinafter.
  • the starting detergent materials are agglomerated in the presence of a silica material as described more fully hereinafter to produce agglomerate particles having the desired low density.
  • the instant process preferably entails mixing from 1% to 20%, more preferably from 3% to 10%, and most preferably from 3% to 5%, by weight of a silica material into the high speed mixer.
  • the alkaline inorganic material is included to serve as an in situ neutralizing agent for the acid precursor in the high speed mixer.
  • the relative amount of the alkaline material can vary since it should be present in an amount sufficient to neutralize the acid precursor.
  • the nature and composition of the entering or starting detergent materials and optional adjunct ingredients can vary as described in detail hereinafter.
  • silica in the agglomerate rather than as a coating agent, a low density agglomerate can be formed. This is contrary to expectations since using silica as a coating or dusting agent to such that it is deposited on the outer surface of agglomerate particles will raise or increase the density.
  • silica inside the agglomerate particles lowers the density as is desired for producing a low density agglomerated composition.
  • the silica when subjected agglomeration with a surfactant and subsequent drying step forms a hollow "finger-like" structure inside the individual agglomerate particles, thereby increasing the internal void space in each agglomerate particle. This, of course, results in more porous agglomerates having a relatively low density.
  • the other essential step in the process involves drying the agglomerates exiting the high speed mixer or moderate speed mixer if it is optionally used.
  • This can be completed in a wide variety of apparatus including but not limited to fluid bed dryers.
  • the drying step enhances the free flowability of the agglomerates and facilities the "fluffy” or "puffy” physical characteristics of the resulting agglomerates. Accordingly, sufficient drying must occur in order to produce the desired low density agglomerates.
  • the drying temperature used in the whichever drying apparatus will preferably be from 50 °C to 300 °C, more preferably from 80 °C to 250 °C, and most preferably, from 100 °C to 250 °C.
  • the mean residence time of the starting detergent materials in the high speed mixer is from 2 to 45 seconds while the residence time in the optional low or moderate speed mixer (e.g. Lödige Recycler KM 300 "Ploughshare" or other similar equipment) is from 0.5 to 15 minutes.
  • the detergent agglomerates produced by the process preferably have a surfactant level of from 20% to 55%, more preferably from 35% to 55% and, most preferably from 45% to 55%.
  • the particle porosity of the resulting detergent agglomerates produced according to the process of the invention is preferably in a range from 5% to 50%, more preferably at 25%.
  • an attribute of dense or densified agglomerates is the relative particle size.
  • the present process typically provides detergent agglomerates having a mean particle size of from 250 microns to 1000 microns, and more preferably from 400 microns to 600 microns.
  • the phrase "mean particle size" refers to individual agglomerates and not individual particles or detergent granules.
  • 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; (2) the coating agent may be added between the fluid bed dryer and the fluid bed cooler; (3) the coating agent may be added between the fluid bed dryer and the moderate speed mixer; and/or (4) the coating agent may be added directly to the moderate speed mixer and the fluid bed dryer.
  • 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 optional moderate speed mixer. 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 comprise the step of spraying an additional binder in one or both of the mixer or fluid bed dryers.
  • a binder is added for purposes of enhancing agglomeration by providing a "binding" or "sticking" agent for the detergent components.
  • the binder is preferably selected from the group consisting of water, anionic surfactants, nonionic surfactants, polyethylene glycol, polyvinyl pyrrolidone polyacrylates, citric acid and mixtures thereof.
  • suitable binder materials including those listed herein are described in Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble Co.).
  • optional steps contemplated by the present process include screening the oversized detergent agglomerates in a screening apparatus which can take a variety of forms including but not limited to conventional screens chosen for the desired particle size of the finished detergent product.
  • Other optional steps include conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying in the one of the aforementioned drying apparatus.
  • agglomerates exiting the moderate speed mixer can be dried in a spray drying tower as described in Capeci et al, U.S. Patent 5,496,487 (Procter & Gamble).
  • Another optional step of the instant process entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients.
  • 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 liquid acid precursor of detergent surfactant used in the process is preferably in the form of an aqueous liquid acid precursor of an anionic surfactant, although forms are also contemplated by the invention.
  • This so-called acid precursor of a surfactant paste contains at least 5% water, more preferably at least 10% water.
  • the surfactant itself ultimately formed via neutralization in situ in the high speed mixer is preferably selected from a variety of known anionics 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.
  • 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 7, preferably at least 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 benzene
  • adjunct surfactants may be optionally used in the process invention.
  • 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. Of the surfactants, anionics and cationics are preferred and anionics are most preferred.
  • exemplary surfactants useful in the invention include and 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 9,206,154.
  • 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 an alkaline inorganic material and a silica material.
  • the alkaline inorganic material is preferably selected from the group consisting of carbonates, silicates, phosphates and mixtures thereof.
  • Sodium carbonate is the most preferred alkaline inorganic material used in the process and is preferably in the form of a solid powder.
  • Silica is highly dispersed amorphous silicon dioxide that is commercially available in many forms. Most commonly, silica has a tapped density of from 50 g/l to 120 g/l.
  • the specific surface area of the particles ranges from 25 square meters per gram to 800 square meters per gram.
  • the surface of the silica particles can be chemically modified to change their behavior with respect to water.
  • silica particles may be treated with organosilanes to make the particles predominantly hydrophobic. It has been found that silicas that are hydrophobic in nature work extremely well in the current process invention; however, hydrophilic silicas are useful in the process, as well. Diatomaceous earth materials may be used in conjunction with, or as a substitute for, the silicas mentioned herein.
  • silicas are usually prepared by one of two techniques; either by precipitation (i.e. precipitated silicas) or by high temperature flame hydrolysis (i.e. fumed silicas). Both precipitated silicas and fumed silicas are useful in the current process invention. Precipitated silicas generally have an agglomerate size of from 3 micrometers to 100 micrometers, whereas fumed silicas made by flame hydrolysis usually have particles which are substantially spherical and have an average particle diameter of from 7 nm to 40 nm. Fumed silicas having an average particle size of from 7 to 25 nm are preferred in the present invention.
  • Exemplary commercially available silicas useful in the process invention include those supplied by Degussa AG (Germany) identified as AerosilTM, and particularly preferred is AerosilTM R927. Silicas which are hydrophobic, fumed and have surface areas of at least 110 square meters per gram and an average particle diameter size of 16 nm are most preferred.
  • the dry detergent material also preferably includes a detergent aluminosilicate builder which are referenced as aluminosilicate ion exchange materials.
  • 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.
  • the term "particle size diameter" as used herein 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 0.1 micron to 10 microns, more preferably from 0.5 microns to 9 microns. Most preferably, the particle size diameter is from 1 microns to 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 1 to 5 and x is from 10 to 264. More preferably, the aluminosilicate has the formula Na 12 [(AlO 2 ) 12 .(SiO 2 ) 12 ]xH 2 O wherein x is from 20 to 30, preferably 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 aluminosilicates used herein are further characterized by their ion exchange capacity which is at least 200 mg equivalent of CaCO 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from 300 to 352 mg equivalent of CaCO 3 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further characterized by their calcium ion exchange rate which is at least 2 grains Ca ++ /gallon/minute/-gram/gallon, and more preferably in a range from 2 grains Ca ++ /gallon/minute/-gram/gallon to 6 grains Ca ++ /gallon/minute/-gram/gallon.
  • An especially preferred set of dry detergent material is selected from the group consisting of aluminosilicates, crystalline layered silicates, sodium carbonate and mixtures thereof
  • 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-tarnish and anti-corrosion 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 1.9 to 4 and y is from 0 to 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 0 to 20. These and other crystalline layered sodium silicates are discussed in Corkill et al, U.S. Patent No. 4,605,509.
  • inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from 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 0.5 to 4.0, preferably from 1.0 to 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.
  • a low density agglomerated detergent composition is prepared using a lab tilt-a-pin (commercially available from Processall, Inc.) mixer.
  • the mixer is first charged with a mixture of powders, namely sodium carbonate (mean particle size of 5-40 microns made via Air Classifier Mill), light density, granular sodium tripolyphosphate (commercially supplied by FMC Corp. and referenced herein as "STPP”)), zeolite type A (commercially supplied by Ethyl Corp.
  • Example IV did not use this or any fumed silica material.
  • the liquid acid precursor of sodium alkylbenzene sulfonate (C 12 H 25 -C 6 H 4 -SO 3 -H or "HLAS" as referenced herein) surfactant is then added on top of the powder mixture while the mixer is operated for about 15 seconds at 700 rpm until discrete granules are formed in the mixer.
  • the composition of the agglomerates formed are set forth below in Table I.

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EP97934909A 1996-07-26 1997-07-16 Preparation of low density detergent agglomerates containing silica Expired - Lifetime EP0915959B1 (en)

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US2247396P 1996-07-26 1996-07-26
US22473P 1996-07-26
PCT/US1997/011988 WO1998004670A1 (en) 1996-07-26 1997-07-16 Preparation of low density detergent agglomerates containing silica

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JP2002533532A (ja) * 1998-12-22 2002-10-08 ザ、プロクター、エンド、ギャンブル、カンパニー 凝集による低かさ密度洗剤組成物の製造方法
CA2884043A1 (en) 2012-09-07 2014-03-13 Paben Proyectos Estrategicos, S.A. De C.V. Silica-based structurants and processes for making thereof
WO2014040010A2 (en) * 2012-09-10 2014-03-13 The Procter & Gamble Company Cleaning compositions comprising structured particles
US9828569B2 (en) 2013-06-13 2017-11-28 The Procter & Gamble Company Granular laundry detergent

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EP0510746A3 (en) * 1991-04-12 1993-09-08 The Procter & Gamble Company Process for preparing condensed detergent granules
JPH07179898A (ja) * 1993-12-22 1995-07-18 Lion Corp 高嵩密度粒状洗剤組成物の製造方法
AUPN535095A0 (en) * 1995-09-12 1995-10-05 Procter & Gamble Company, The Compositions comprising hydrophilic silica particulates
US5576285A (en) * 1995-10-04 1996-11-19 The Procter & Gamble Company Process for making a low density detergent composition by agglomeration with an inorganic double salt

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GR3037079T3 (en) 2002-01-31
AU3796697A (en) 1998-02-20
BR9710559A (pt) 1999-08-17
DE69709746T2 (de) 2002-07-18
AR008784A1 (es) 2000-02-23
ES2163792T3 (es) 2002-02-01
ATE209248T1 (de) 2001-12-15
WO1998004670A1 (en) 1998-02-05
DE69709746D1 (de) 2002-02-21
ZA976616B (en) 1998-02-10
CN1230981A (zh) 1999-10-06
ID17634A (id) 1998-01-15
EP0915959A1 (en) 1999-05-19
DK0915959T3 (da) 2002-05-21
CN1120229C (zh) 2003-09-03
PT915959E (pt) 2002-03-28

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