WO2000037605A1 - Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration - Google Patents

Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration Download PDF

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Publication number
WO2000037605A1
WO2000037605A1 PCT/US1998/027230 US9827230W WO0037605A1 WO 2000037605 A1 WO2000037605 A1 WO 2000037605A1 US 9827230 W US9827230 W US 9827230W WO 0037605 A1 WO0037605 A1 WO 0037605A1
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WIPO (PCT)
Prior art keywords
detergent
mixer
bulk density
source
agglomerates
Prior art date
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PCT/US1998/027230
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English (en)
Inventor
Manivannan Kandasamy
Yuji Nakamura
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 JP2000589661A priority Critical patent/JP2002533532A/ja
Priority to EP98964850A priority patent/EP1141229A1/fr
Priority to AU20082/99A priority patent/AU2008299A/en
Priority to BR9816122-9A priority patent/BR9816122A/pt
Priority to CNB988143739A priority patent/CN1183243C/zh
Priority to PCT/US1998/027230 priority patent/WO2000037605A1/fr
Priority to CA002353534A priority patent/CA2353534A1/fr
Priority to ARP990106662A priority patent/AR021975A1/es
Publication of WO2000037605A1 publication Critical patent/WO2000037605A1/fr

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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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0052—Gas evolving or heat producing 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions 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
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • 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
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2082—Polycarboxylic acids-salts thereof
    • 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
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2086—Hydroxy carboxylic acids-salts thereof
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146—Sulfuric acid esters

Definitions

  • the present invention generally relates to a process for producing a low bulk density detergent composition. More particularly, the invention is directed to a process in which low bulk density detergent agglomerates are produced by feeding a binder, such as a surfactant paste, into a mixer. The process produces a free flowing, low bulk 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.
  • a binder such as a surfactant paste
  • 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 bulk density of the resulting detergent granules are the bulk density, porosity and surface area, shape 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 density of the detergent granules.
  • Patent No. 5,486,303 Procter & Gamble
  • Capeci et al U.S. Patent No. 5,489,392 (Procter & Gamble); Hollingsworth et al, European Patent Application 351 ,937 (Unilever); and Swatling et al, U.S. Patent No. 5,205,958.
  • the following references are directed to surfactant pastes: Aouad et al, WO 93/18123 (Procter & Gamble); Aouad et al, WO 92/18602 (Procter & Gamble); Aouad et al, EP 508,543 (Procter & Gamble); Mueller et al, U.S. Patent no.
  • the present invention provides a process which produces an agglomerated low bulk density (below about 600 g/l) detergent composition directly from starting ingredients.
  • the process includes the steps of agglomerating a detergent binder, an organic acid source, and a carbonate source in a mixer to obtain detergent agglomerates, wherein the reaction of the organic acid source and the carbonate source generates gas, such as carbon dioxide gas, within the agglomerate, and drying the detergent agglomerate so as to form a detergent composition.
  • the process does not require the use of conventional spray drying towers, and therefore, is more efficient, economical and flexible with regard to the variety of detergent compositions that can be produced in the process.
  • the present invention provides a process which produces an agglomerated low bulk density (below about 600 g/l) detergent composition directly from starting ingredients.
  • the process does not use the conventional spray drying towers 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 require spray drying towers which require more energy to operate and may emit particulates and volatile organic compounds into the atmosphere if not operated properly.
  • 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 and all documents cited herein are incorporated herein by reference. 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. In accordance with one aspect of the invention, a process for producing a low bulk density detergent composition is provided.
  • the process includes the steps of agglomerating a detergent binder, an organic acid source, and a carbonate source in a mixer to obtain detergent agglomerates, wherein the reaction of the organic acid source and the carbonate source generates gas, such as carbon dioxide gas, within the agglomerate, and drying the detergent agglomerate so as to form a detergent composition.
  • gas such as carbon dioxide gas
  • 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 in a mixer wherein the starting detergent materials are agglomerated in a mixer.
  • the mixer preferably is a high speed or a low speed mixer.
  • a second mixer which can be a low, moderate, or high speed mixer, may be used for further agglomeration if necessary.
  • the nature and composition of the entering or starting detergent materials can vary as described in detail hereinafter.
  • the mean residence time of the starting detergent materials in a high speed mixer e.g.
  • L ⁇ dige Recycler CB, Schugi, or other similar equipment is from about 0.1 to 45 seconds while the residence time in a low or moderate speed mixer (e.g. Lodige Recycler KM "Ploughshare” or other similar equipment) is from about 0.5 to 15 minutes.
  • a low or moderate speed mixer e.g. Lodige Recycler KM "Ploughshare” or other similar equipment
  • the starting detergent materials preferably include (1) a detergent binder, such as a highly viscous surfactant paste, non-ionic surfactant, and other viscous binders such as polyethylene glycol, (2) an organic acid source, and (3) a carbonate source, the components of which are described more fully hereinafter.
  • a detergent binder such as a highly viscous surfactant paste, non-ionic surfactant, and other viscous binders such as polyethylene glycol
  • organic acid source such as a highly viscous surfactant paste, non-ionic surfactant, and other viscous binders such as polyethylene glycol
  • organic acid source react and generate gas, such as carbon dioxide gas, within the particle, thereby creating a void volume within the particle. This, of course, results in more porous agglomerates having a relatively low bulk density.
  • the mean residence time in the mixer is from about 5 to about 30 seconds and tip speed for the mixer is in range from about 5 m/s to about 10 m/s
  • the energy per unit mass in the mixer is from about 0.15 kj/kg to about 4.20 kj/kg
  • the mean residence time in the mixer is from about 10 to about 15 seconds and tip speed for the mixer is in range from about 6 m/s to about 8 m/s
  • the energy per unit mass for the mixer is from about 0.15 kj/kg to about 2.5 kj/kg
  • the mean residence time in the mixer is from about 10 to about 15 seconds and tip speed for the mixer is in range from about 6.5 m/s to about 7.5 m/s
  • the energy per unit mass for the mixer is from about 0.15 kj/kg to about 1.30 kj/kg.
  • the agglomerates produced preferably have a bulk density of from about 350 g/l to about 500 g/l.
  • the detergent binder and the carbonate source is first premixed, and the premixture is added to the organic acid source in the mixer.
  • the molar ratio of organic acid to carbonate source is preferably from about 1 :1 to about 1 :8, more preferably from about 1 :1 to about 1 :4. Drying may be an optional step in order to further lower the bulk density of the agglomerates.
  • the drying temperature used in any of the drying apparatus known will preferably be from about 50°C to about 300°C, more preferably from about 80°C to about 250°C, and even more preferably, from about 100°C to about 250°C.
  • the detergent agglomerates exiting the mixer contain at least about 3%, more preferably at least about 5%, and most preferably from about 5% to about 15%, by weight of water.
  • the process may include the step of spraying water in the mixer to insure that the aforementioned water levels are included in the detergent agglomerates.
  • the water embodied in the agglomerates instantaneously or very quickly evaporates upon being subjected to dielectric heating causing the agglomerates to "puff 1 into a fluffy, light, low bulk density agglomerate particle in the dryer.
  • the detergent agglomerates produced by the process preferably have a surfactant level of from about 12% to about 55%, more preferably from about 35% to about 55% and, most preferably from about 45% to about 55%.
  • the interparticle and intraparticle porosity of the resulting detergent agglomerates produced according to the process of the invention is preferably in a range from about 5% to about 60%, more preferably at about 35 to about 50%.
  • an attribute of dense or densified agglomerates is the relative particle size.
  • the present process typically provides detergent agglomerates having a median particle size of from about 250 microns to about 2000 microns, and more preferably from about 600 microns to about 850 microns.
  • the optional moderate speed mixer can be used to insure build-up to the aforementioned median particle sizes.
  • 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 bulk density values of less than 600 g/l. Such a feature is especially useful in the production of laundry detergents having varying dosage levels as well as other granular compositions such as dishwashing compositions.
  • the detergent agglomerates exiting the mixer or the moderate speed mixer are further conditioned by additional cooling or drying in a fluid bed cooler and/or drier 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 optional moderate speed mixer; and/or (4) the coating agent may be added directly to the optional 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 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 mixers or dryer.
  • 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, silicates, anionic surfactants, nonionic surfactants, polyethylene glycol, polyvinyi pyrrolidone polyacrylates, citric acid and mixtures thereof.
  • Other suitable binder materials including those listed herein are described in Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble Co.), the disclosure of which is incorporated herein by reference.
  • 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 detergent binder used in the process is preferably in the form of an aqueous viscous paste, although other forms are also contemplated by the invention.
  • This so-called viscous binder has a viscosity of from about 200 cps to about 100,000 cps, more preferably from about 10,000 cps to about 80,000 cps, and contains at least about 10% water, more typically at least about 30% by weight of water. The viscosity is measured at 70°C and at shear rates of about 10 to 100 sec. "' ' .
  • the detergent binder if used, preferably comprises a detersive surfactant as described hereinafter in the amounts specified previously and the balance water and other conventional detergent ingredients.
  • a detergent surfactant paste can be used as a detergent binder.
  • the surfactant is 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, both of which are incorporated herein by reference.
  • 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, both of which are also incorporated herein by reference.
  • anionics, cationics, zwitterionics and nonionics are preferred and anionics are most preferred.
  • Nonlimiting examples of the preferred anionic surfactants useful include the conventional C-
  • LAS C-
  • exemplary surfactants useful in the invention include and C ⁇ ⁇ rj-Ci8 alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C- ⁇ o-18 glycerol ethers, the C-10-C18 alkyl polyglycosides and their corresponding sulfated polyglycosides, and C12-C18 alpha-sulfonated fatty acid esters.
  • the conventional nonionic and amphoteric surfactants such as the C12-C18 alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C6-C12 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C12-C18 betaines and sulfobetaines (“sultaines”), C10-C18 arnine oxides, and the like, can also be included in the overall compositions.
  • AE C12-C18 alkyl ethoxylates
  • sulfobetaines especially ethoxylates and mixed ethoxy/propoxy
  • C10-C18 arnine oxides and the like
  • the C10-C18 N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C12-C 8 N-methylglucamides. See WO 9,206,154.
  • Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C10-C18 N-(3-methoxypropyl) glucamide.
  • the N- propyl through N-hexyl C-12-C18 glucamides can be used for low sudsing.
  • C-I Q- C20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C ⁇
  • Organic acid source The acid source is preferably substantially anhydrous or non-hygroscopic and the acid is preferably water-soluble. It may be preferred that the acid source is overdried.
  • Suitable acids source components include an acid or salt form of a mono or polycarboxylic acid. Such preferred acids include those selected from the group consisting of citric, malic, maleic, fumaric, aspartic, glutaric, tartaric, malonic, succinic or adipic acid, 3 chetoglutaric acid, citramalic acid, and mixtures thereof. Citric acid, maleic or malic acid are especially preferred.
  • the acid source provides acidic compounds which have an average particle size in the range of from about 10 microns to about 1180 microns, more preferably from about 70 microns to about 710 microns, calculated by sieving a sample of the source of acidity on a series of Tyler sieves.
  • the carbonate source is a carbonate and/or bicarbonate, and in particular, a carbonate/bicarbonate salt.
  • preferred carbonates are the alkaline earth and alkali metal carbonates, including sodium or potassium carbonate, bicarbonate and sesqui-carbonate and any mixtures thereof with ultra-fine calcium carbonate such as are disclosed in German Patent Application
  • Alkali metal percarbonate salts are also suitable sources of carbonate species, which may be present combined with one or more other carbonate sources.
  • the carbonate and bicarbonate preferably have an amorphous structure.
  • the carbonate and/ or bicarbonates may be coated.
  • the particles of carbonate and bicarbonate preferably have a mean particle size of about 4 ⁇ m or greater, preferably about 10 ⁇ m or greater, more preferably of about 15 ⁇ m to about 100 ⁇ m.
  • Adjunct detergent ingredients can be included in the process as well and include bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anticorrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, 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., incorporated herein by reference.
  • An alkaline inorganic salt may be used when a liquid acid precursor of a surfactant is used so as to provide a neutralizing agent in the agglomeration step.
  • Other adjunct ingredients preferably includes a detergent aluminosilicate builder 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.
  • 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 disclosure of which is incorporated herein by reference.
  • the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms of the instant aluminosilicate do not exhibit 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 [(AI0 2 )z-(Si ⁇ 2)y]xH 2 0 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
  • aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B, Zeolite P, Zeolite MAP 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 CaC ⁇ 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC ⁇ 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/gallon, and more preferably in a range from about 2 grains Ca ++ /gallon/minute/-gram/gallon to about 6 grains Ca ++ /gallon/minute/- gram/gallon .
  • 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.
  • the alkali metal especially sodium, salts of the above.
  • Preferred for use herein are the phosphates, carbonates, C-
  • 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
  • the crystalline layered sodium silicate has the formula
  • 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, all of which are incorporated herein by reference.
  • nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of Si0 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, the disclosure of which is incorporated 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 U.S.
  • 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, the disclosure of which is incorporated herein by reference. Bleaching agents and activators are described in U.S. Patent 4,412,934,
  • 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 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, both incorporated herein by reference.
  • a low bulk density detergent composition is prepared in a batch mode using a lab tilt-a-pin mixer (commercially available from Processall, Inc.). The mixer is first charged with a mixture of dry powders, namely sodium carbonate (median particle size 5-40 microns made via Air Classifier Mill), light bulk density sodium tripolyphosphate (referenced herein as "STPP" and supplied by FMC Corp.), sodium sulfate (median particle size of 5 - 40 microns made via Air Classifier Mill), sodium bicarbonate (median particle size of 5-40 microns made via Air Classifier Mill), granular citric acid monohydrate (median particle size of approximately 400 - 600 microns supplied by Wako Chemicals, Japan) and undersized finished agglomerates having a median particle size of less than 150 microns to mimic the recycling of such undersized particles during continuous large-scale modes of the current process.
  • Example I is unexpectedly low after addition of citric acid and sodium bicarbonate in the instant process invention.

Abstract

Procédé de préparation d'une composition détergente à faible masse volumique apparente (inférieure à environ 600 g/l) directement à partir d'ingrédients de départ pour détergents. Ledit procédé consiste à agglomérer un liant pour détergent, une source d'acide organique et une source de carbonate dans un mélangeur pour obtenir des agglomérats de détergent, la réaction de la source d'acide organique et de la source de carbonate produisant du gaz, tel que du dioxyde de carbone, au sein de la particule, et à sécher l'agglomérat de détergent de façon à former une composition détergente. Ledit procédé ne nécessite pas l'utilisation de tours de séchage-atomisation classiques, et par conséquent il est plus efficace, plus économique et plus souple pour ce qui est de la gamme de compositions détergentes qui peuvent être produites selon ledit procédé.
PCT/US1998/027230 1998-12-22 1998-12-22 Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration WO2000037605A1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
JP2000589661A JP2002533532A (ja) 1998-12-22 1998-12-22 凝集による低かさ密度洗剤組成物の製造方法
EP98964850A EP1141229A1 (fr) 1998-12-22 1998-12-22 Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration
AU20082/99A AU2008299A (en) 1998-12-22 1998-12-22 Process for making a low bulk density detergent composition by agglomeration
BR9816122-9A BR9816122A (pt) 1998-12-22 1998-12-22 Processo para fabricação de composição detergente de baixa densidade de volume através de aglomeração
CNB988143739A CN1183243C (zh) 1998-12-22 1998-12-22 通过附聚作用制造低堆积密度洗涤剂组合物的方法
PCT/US1998/027230 WO2000037605A1 (fr) 1998-12-22 1998-12-22 Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration
CA002353534A CA2353534A1 (fr) 1998-12-22 1998-12-22 Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration
ARP990106662A AR021975A1 (es) 1998-12-22 1999-12-22 Proceso para preparar una composicion detergente de baja densidad global por aglomeracion.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US1998/027230 WO2000037605A1 (fr) 1998-12-22 1998-12-22 Procede de preparation d'une composition detergente a faible masse volumique apparente par agglomeration

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WO2000037605A1 true WO2000037605A1 (fr) 2000-06-29

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EP (1) EP1141229A1 (fr)
JP (1) JP2002533532A (fr)
CN (1) CN1183243C (fr)
AR (1) AR021975A1 (fr)
AU (1) AU2008299A (fr)
CA (1) CA2353534A1 (fr)
WO (1) WO2000037605A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003035813A1 (fr) * 2001-10-19 2003-05-01 Unilever Plc Compositions detergentes
EP1382667A1 (fr) * 2002-07-17 2004-01-21 Unilever N.V. Procédé de production de granules détergents
US7053038B2 (en) 2001-08-13 2006-05-30 Unilever Home & Personal Care Usa Division Of Conopco, Inc. Process for the production of detergent granules
US7727947B2 (en) 2008-05-14 2010-06-01 The Procter & Gamble Company Process for the preparation of a solid laundry detergent composition comprising light density silicate salt

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO1997028246A1 (fr) * 1996-01-31 1997-08-07 Unilever Plc Procede pour la production d'une composition detergente
WO1998004661A1 (fr) * 1996-07-31 1998-02-05 The Procter & Gamble Company Compositions detergentes
WO1998004670A1 (fr) * 1996-07-26 1998-02-05 The Procter & Gamble Company Procede de fabrication d'agglomerats detergents de faible densite contenant de la silice
WO1998014550A1 (fr) * 1996-10-04 1998-04-09 The Procter & Gamble Company Procede de production d'une composition de detergent de faible densite

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO1997028246A1 (fr) * 1996-01-31 1997-08-07 Unilever Plc Procede pour la production d'une composition detergente
WO1998004670A1 (fr) * 1996-07-26 1998-02-05 The Procter & Gamble Company Procede de fabrication d'agglomerats detergents de faible densite contenant de la silice
WO1998004661A1 (fr) * 1996-07-31 1998-02-05 The Procter & Gamble Company Compositions detergentes
WO1998014550A1 (fr) * 1996-10-04 1998-04-09 The Procter & Gamble Company Procede de production d'une composition de detergent de faible densite

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7053038B2 (en) 2001-08-13 2006-05-30 Unilever Home & Personal Care Usa Division Of Conopco, Inc. Process for the production of detergent granules
WO2003035813A1 (fr) * 2001-10-19 2003-05-01 Unilever Plc Compositions detergentes
US6936577B2 (en) 2001-10-19 2005-08-30 Unilever Home Products And Care Usa, Division Of Conopco, Inc. Detergent compositions
EP1382667A1 (fr) * 2002-07-17 2004-01-21 Unilever N.V. Procédé de production de granules détergents
US7727947B2 (en) 2008-05-14 2010-06-01 The Procter & Gamble Company Process for the preparation of a solid laundry detergent composition comprising light density silicate salt
US7732394B2 (en) 2008-05-14 2010-06-08 The Procter & Gamble Company Solid laundry detergent composition comprising light density silicate salt

Also Published As

Publication number Publication date
EP1141229A1 (fr) 2001-10-10
JP2002533532A (ja) 2002-10-08
CN1183243C (zh) 2005-01-05
CA2353534A1 (fr) 2000-06-29
AU2008299A (en) 2000-07-12
AR021975A1 (es) 2002-09-04
CN1327477A (zh) 2001-12-19

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