WO2000024861A1 - Procede de preparation d'une composition detergente a ecoulement facile - Google Patents

Procede de preparation d'une composition detergente a ecoulement facile Download PDF

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Publication number
WO2000024861A1
WO2000024861A1 PCT/US1998/022896 US9822896W WO0024861A1 WO 2000024861 A1 WO2000024861 A1 WO 2000024861A1 US 9822896 W US9822896 W US 9822896W WO 0024861 A1 WO0024861 A1 WO 0024861A1
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WIPO (PCT)
Prior art keywords
materials
liquid
powder
surface area
powder materials
Prior art date
Application number
PCT/US1998/022896
Other languages
English (en)
Inventor
Mayumi Daiki
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 EP98960152A priority Critical patent/EP1124931A1/fr
Priority to PCT/US1998/022896 priority patent/WO2000024861A1/fr
Priority to CN98814282.1A priority patent/CN1214101C/zh
Priority to US09/787,445 priority patent/US6576605B1/en
Priority to BR9816061-3A priority patent/BR9816061A/pt
Priority to CA002346340A priority patent/CA2346340A1/fr
Priority to AU15819/99A priority patent/AU1581999A/en
Priority to JP2000578416A priority patent/JP2002528599A/ja
Publication of WO2000024861A1 publication Critical patent/WO2000024861A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/37—Mixtures of compounds all of which are anionic
    • 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
    • C11D11/04—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
    • 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
    • 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
    • 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
    • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds

Definitions

  • the present invention relates to a non-tower process for producing a particulate detergent composition.
  • the process produces a free flowing, detergent composition whose density can be adjusted for a wide range of consumer needs, and which can be commercially sold as a conventional 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 present invention relates to a non-tower process for preparing a granular detergent composition, the process comprising the following steps: (i) fluidising powder materials in a high-speed mixer/granulator having both a stirring action and a cutting action, the powder materials comprising: particulate solid water-soluble alkaline inorganic material in an amount in excess of that required for neutralization, optionally in admixture with one or more other particulate solids, and recycled fines, the powder materials having a total surface area; (ii) adding the liquid detersive materials to the high-speed mixer/granulator, the liquid detersive materials comprising: a liquid acid precursor, optionally in admixture with one or more other liquid materials, whereby neutralization of the acid precursor by the water-soluble alkaline inorganic material occurs; and (iii) granulating the mixture in the high-speed mixer/granulator to form detergent particles, wherein the ratio of the total surface area of the powder materials to the amount of liquid detersive materials in
  • the present invention meets the aforementioned needs in the art by providing a process which produces a detergent composition from liquid acid precursor of anionic surfactant and alkaline inorganic materials.
  • the present invention also meets the aforementioned needs in the art by providing a process which produces a granular detergent composition for flexibility in the ultimate density of the final composition from agglomeration (e.g., non-tower) process.
  • the process does not use the conventional spray drying towers currently which is limited in producing high surfactant loading compositions.
  • 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 materials with binder such as surfactants and or inorganic solutions / organic solvents and polymer solutions.
  • binder such as surfactants and or inorganic solutions / organic solvents and polymer solutions.
  • granulating refers to fluidizing agglomerates thoroughly for producing free flowing, round shape granulated-agglomerates.
  • a non-tower process for preparing detergent agglomerates comprises the following steps: (i) fluidising powder materials in a high-speed mixer/granulator having both a stirring action and a cutting action, the powder materials comprising: particulate solid water-soluble alkaline inorganic material in an amount in excess of that required for neutralization, optionally in admixture with one or more other particulate solids, and recycled fines, the powder materials having a total surface area; (ii) adding the liquid detersive materials to the highspeed mixer/granulator, the liquid detersive materials comprising: a liquid acid precursor, optionally in admixture with one or more other liquid materials, whereby neutralization of the acid precursor by the water-soluble alkaline inorganic material occurs; and (iii) granulating the mixture in the high-speed mixer/granulator to form detergent particles, wherein the ratio of the total surface
  • the present invention provides many benefits. Although not wanting to be limited by theory, it is believed that by controlling the ratio of the average surface area of the powder materials, which includes the recycled fines, to the amount of liquid detersive materials, the generation of fines can be controlled. In one typical process, fines are generated from a fluid bed cooler via a mixer, collected in a bin, and then fed back to the mixer. If more fines are generated than are fed back (or recycled back), this unbalance would cause the accumulation of fines in the bin and eventually shut down the system over time.
  • the present invention is directed to a process which produces free flowing, detergent agglomerates having wide range of density, e.g., from about 300 g/l to about 1000 g/l, especially for high dense detergent agglomerates e.g., from about 600 g/l to about 850 g/l.
  • the powder materials are first fluidised in a high-speed mixer/granulator having both a stirring action and a cutting action.
  • the powder material includes a particulate solid water-soluble alkaline inorganic material in an amount in excess of that required for neutralization.
  • other powder materials may be mixed with the alkaline inorganic material, such are recycled fines.
  • liquid detersive ingredients are added to the high-speed mixer/granulator, whereby a liquid acid precursor is added so that neutralization of the acid precursor by the water-soluble alkaline inorganic material occurs.
  • Other liquid detersive ingredients such as a neutralized anionic surfactant, e.g.
  • coco fatty alcohol sulfate, a liquid chelant, and/or a nonionic surfactant can optionally be added at this time.
  • Liquid detersive ingredients may include paste forms.
  • the mixture is subsequently granulated to form detergent particles, wherein the ratio of the total surface area of the powder materials to the liquid detersive materials is from about 0.02 to about 140.
  • the ratio is from about 0.03 to about 70; more preferably, the ratio is from about 0.04 to about 50.
  • the detergent particle is next agglomerated in a moderate speed granulator/densifier, with or without a separate powder stream, and then dried and/or cooled using for example, a fluid bed dryer/cooler, to form a particulate granular detergent composition.
  • Powder materials include particulate solid water-soluble alkaline inorganic materials.
  • inorganic materials include sodium carbonate, calcium carbonate, bicarbonates, and mixtures thereof: There should be a stoichiometric excess of particulate solid water-soluble alkaline inorganic over the liquid acid precursor.
  • powder materials include recycled fines, zeolite, phosphate, phosphonate, sulfate, silica, silicates, polymers including copolymers of maleic and acrylic acid, carboxymethyl cellulose, optical brighteners, ethylene diamine tetra acetic acid, and mixtures thereof.
  • suitable ingredients including additional surfactants, they may be handled as solids are described in detail below.
  • the starting fine powder of the present process preferably selected from the group consisting of ground soda ash, powdered sodium tripolyphosphate (STPP), hydrated tripolyphosphate, ground sodium sulphates, aluminosilicates, crystalline layered silicates, nitrilotriacetates (NTA), phosphates, precipitated silicates, polymers, citrates, powdered surfactants (such as powdered alkane sulfonic acids) and internal recycle stream of powder occurring from the process of the present invention.
  • STPP powdered sodium tripolyphosphate
  • hydrated tripolyphosphate ground sodium sulphates
  • aluminosilicates aluminosilicates
  • crystalline layered silicates nitrilotriacetates
  • phosphates precipitated silicates
  • polymers citrates
  • powdered surfactants such as powdered alkane sulfonic acids
  • internal recycle stream of powder occurring from the process of the
  • 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.
  • 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 material has the formula Na z [(Al ⁇ 2 .
  • the aluminosilicate has the formula Nai2_(Al ⁇ 2)i2- (Si ⁇ 2)i2] ⁇ H2 ⁇ wherein x is from about 20 to about 30, preferably about 27.
  • These preferred aluminosilicat.es are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X.
  • Liquid detersive materials include liquid materials which have a viscosity of from about 0 cps to about 5,000 cps, preferably from about 0 cps to about 3,000 cps and includes some paste forms.
  • liquid acid precursors examples include anionic surfactant acids, amino polyphosphates, chelating agents, such as diethylene triamine penta acetic acid, and additional anionic surfactants (as neutralized salts), nonionic, cationic, ampholytic, zwitterionic surfactants, and mixtures thereof.
  • Useful anionic surfactant acids include organic sulphuric reaction products having in their molecular structure an alkyl group containing from about 9 to about 20 carbon atoms and a sulphonic acid.
  • Examples of this group of synthetic surfactants are the alkyl benzene sulphonic acids in which the alkyl group contains from about 9 to about 15 carbon atoms in straight or branched chain configuration.
  • Especially suitable anionic surfactant acids are linear alkyl benzene sulphonates in which the alkyl group contains from about 11 to about 13 carbon atoms.
  • Other useful surfactant acids include alpha sulphonated fatty acid methyl esters, olefin sulphonates and beta alkyloxy alkane sulphonates. Mixture of the above may also be used.
  • a preferred liquid acid precursor is linear alkyl benzene sulphonic acid (HLAS).
  • a preferred liquid material is coco fatty alcohol sulfate (CFAS).
  • CFAS coco fatty alcohol sulfate
  • the ratio of CFAS:HLAS is from about 4:1 to about 8:1.
  • Other liquid detersive materials include amino polyphosphates, chelating agents, such as diethylene triamine penta acetic acid, and additional anionic surfactants (as neutralized salts), nonionic, cationic, ampholytic, and zwitterionic surfactants.
  • liquids may be sprayed into the high shear mixer including amino polyphosphates, diethylene triamine penta acetic acid and additional anionic surfactants (as neutralised salts), nonionic, cationic, ampholytic and zwitterionic surfactants.
  • Especially suitable amino polyphosphonates include diethylene triamine penta methylene phosphonic acid and ethylene diamine tetra methylene phosphonic acid.
  • Especially suitable additional anionic surfactants are water-soluble salts of the higher fatty acids.
  • Soaps can be made by direct saponification of fats and oils or by the neutralization of free fatty acids.
  • Particularly useful are the sodium and potassium salts of the mixtures of fatty acids derived from coconut oil and tallow, i.e., sodium or potassium tallow and coconut soap.
  • Useful anionic surfactants also include the water-soluble salts, preferably the alkali metal, ammonium and alkylolammonium salts, of organic sulfuric reaction products having in their molecular structure an alkyl group containing from about 10 to about 20 carbon atoms and a sulfonic acid or sulfuric acid ester group, (included in the term "alkyl” is the alkyl portion of acyl groups.)
  • alkyl is the alkyl portion of acyl groups.
  • Examples of this group of synthetic surfactants are the sodium and potassium alkyl sulfates, especially those obtained by sulfating the higher alcohols (C 8 -C 18 carbon atoms) such as those produced by reducing the glycerides of tallow or coconut oil.
  • anionic surfactants herein are the sodium or potassium salts of alkyl phenol ethylene oxide ether sulfates containing from about 1 to about 10 units of ethylene oxide per molecule and wherein the alkyl groups contain from about 8 to about 12 carbon atoms; and sodium or potassium salts of alkyl ethylene oxide ether sulfates containing from about 1 to about 10 units of ethylene oxide per molecule and wherein the alkyl group contains from about 10 to about 20 carbon atoms.
  • Water-soluble nonionic surfactants are also useful as secondary surfactant in the compositions of the invention.
  • a particularly preferred paste comprises a blend of nonionic and anionic surfactants having a ratio of from about 0.01 :1 to about 1 :1 , more preferably about 0.05:1.
  • Nonionics can be used up to an equal amount of the primary organic surfactant.
  • Such nonionic materials include compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkyl aromatic in nature. The length of the polyoxyalkylene group which is condensed with any particular hydrophobic group can be readily adjusted to yield a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.
  • Suitable nonionic surfactants include the polyethylene oxide condensates of alkyl phenols, e.g., the condensation products of alkyl phenols having an alkyl group containing from about 6 to 16 carbon atoms, in either a straight chain or branched chain configuration, with from about 4 to 25 moles of ethylene oxide per mole of alkyl phenol.
  • Preferred nonionics are the water-soluble condensation products of aliphatic alcohols containing from 8 to 22 carbon atoms, in either straight chain or branched configuration, with from 4 to 25 moles of ethylene oxide per more of alcohol. Particularly preferred are the condensation products of alcohols having an alkyl group containing from about 9 to 15 carbon atoms with from about 4 to 25 moles of ethylene oxide per mole of alcohol; and condensation products of propylene glycol with ethylene oxide.
  • Semi-polar nonionic surfactants include water-soluble amine oxides containing one alkyl moiety of from about 10 to 18 carbon atoms and 2 moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups containing from 1 to about 3 carbon atoms; water-soluble phosphine oxides containing one alkyl moiety of about 10 to 18 carbon atoms and 2 moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups containing from about 1 to 3 carbon atoms; and water-soluble sulfoxides containing one alkyl moiety of from about 10 to 18 carbon atoms and a moiety selected from the group consisting of alkyl and hydroxyalkyl moieties of from about 1 to 3 carbon atoms.
  • Ampholytic surfactants include derivatives of aliphatic or aliphatic derivatives of heterocyclic secondary and tertiary amines in which the aliphatic moiety can be either straight or branched chain and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms and at least one aliphatic substituent contains an anionic water-solubilizing group.
  • Zwitterionic surfactants include derivatives of aliphatic quaternary ammonium phosphonium, and sulfonium compounds in which one of the aliphatic substituents contains from about 8 to 18 carbon atoms.
  • Useful cationic surfactants include water-soluble quaternary ammonium compounds of the form R 4 R 5 R 6 R 7 N + X " , wherein R 4 is alkyl having from 10 to 20, preferably from 12-18 carbon atoms, and R 5 , R 6 , and R 7 are each C, to C 7 alkyl preferably methyl; X " is an anion, e.g. chloride.
  • Examples of such trimethyl ammonium compounds include C 12 . 14 alkyl trimethyl ammonium chloride and cocalkyl trimethyl ammonium methosulfate. Note that some of these components may be handled in solid form in which case they should be considered as part of the powder stream rather than liquid binders.
  • the ratio of the total surface area of the powder materials to the amount of liquid detersive materials is from about 0.02 to about 140.
  • the ratio is from about 0.03 to about 70; more preferably, the ratio is from about 0.04 to about 50.
  • the total powder material rate used for industrial manufacturing scale ranges from about 500 to about 50,000 kg/hr.
  • the liquid detersive material loading is from about 5 to about 50%, more preferably from about 10% to about 40%, and even more preferably from about 15% to about 25%. If the liquid detersive material is a linear alkyl benzene sulphonic acid (HLAS), then the ratio of the total surface area of the powder materials to HLAS is from about 0.04 to about 50.
  • HLAS linear alkyl benzene sulphonic acid
  • liquid detersive material comprises a mixture of linear alkyl benzene sulphonic acid (HLAS) and coco fatty alcohol sulfate (CFAS), and if the ratio of CFAS:HLAS is from about 4:1 to about 8:1 , then the ratio of the total surface area of the powder materials to the amount of liquid detersive materials is from about 0.04 to about 50.
  • HLAS linear alkyl benzene sulphonic acid
  • CFAS coco fatty alcohol sulfate
  • the total surface area is calculated by any conventional method known in the art.
  • One example is by Malvern, wherein the method applies the theory of laser-light-scattering by particles.
  • Another example is BET, which is a method using a carrier gas, based on the Brunauer-Emmet-Teller (BET) theory.
  • an agglomeration step is carried forth in a high speed mixer or a series of high speed mixers.
  • the examples of a high-speed mixer/granulator for the present invention can be any types of mixer known to those skilled in the art, as long as the mixer can maintain the following conditions.
  • An example can be L ⁇ dige CB Mixers manufactured by the Lodige company (Germany), e.g. L ⁇ dige Recycler CB 60.
  • the mean residence time of the starting detergent materials in the high speed mixer is preferably from about 2 to 45 seconds, more preferably from about 2 to 20 seconds.
  • the speed range of operation in the high speed mixer is preferably from 500 to 2000 rpm, more preferably from 650-850 rpm.
  • the examples of a mixer for the present invention can be combinations of any types of mixer known to those skilled in the art, as long as one of the high speed mixer used for the present invention can maintain the conditions indicated above.
  • An example can be a combination of one of L ⁇ dige CB Mixers manufactured by the L ⁇ dige company (Germany), and Flexomic Model manufactured by Schugi company (Netherlands); i.e., mixing starting detergent materials (which include an acid form of anionic surfactant, a first carbonate, and a second carbonate) are fed into a CB Mixer for agglomeration, subsequently, the resultant (agglomerate) from the CB Mixer is fed into a Flexomic Model for further agglomeration; or mixing starting detergent materials are fed into a Flexomic Model for agglomeration, subsequently, the resultant (agglomerate) from the Flexomic Model is fed into a CB Mixer for further agglomeration.
  • mixing starting detergent materials which include an acid form of anionic surfactant, a first carbonate, and a second carbonate
  • the agglomerates from process of the present invention can be subjected to further mixing process for further agglomeration of the product. This may be achieved by further mixing in a moderate speed mixer.
  • An example of such moderate speed mixer can be L ⁇ dige KM Mixers manufactured by the L ⁇ dige company (Germany).
  • the mean residence time of the moderate speed mixer may be preferably from about 1 to 20 minutes, more preferably from about 10 ⁇ 5 min.
  • 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 suppressors, antitarnish and anficorrosion 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., incorporated herein by reference.
  • Optional Process Steps include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, antitarnish and anficorrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, non-builder alkalinity sources, chelating agents, smectite clay
  • One optional step in the process is drying, if it is desired to reduce level of moisture in the agglomerates from the present process. This can be accomplished by a variety of apparatus, well known to these skilled in the art. Fluid bed apparatus is preferred, and will be referred to as the dryer in the discussion which follows.
  • the detergent agglomerates exiting the fluid bed dryer are further conditioned by additional cooling in cooling apparatus.
  • the preferred apparatus for cooling is a fluid bed.
  • 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 or dryer; (2) the coating agent may be added between the fluid bed dryer and the fluid bed cooler; and/or (3) the coating agent may be added between the fluid bed dryer and a mixer for agglomeration (i.e., the first mixer or the second mixer in the second step) which is commonly known to those skilled in the art.
  • a mixer for agglomeration i.e., the first mixer or the second mixer in the second step
  • 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 for detergent during use, but also serves to control agglomeration by preventing or minimizing over-agglomeration. 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 a mixer(s) used for the present invention or fluid bed dryers and/or fluid bed coolers.
  • 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, liquid silicates, 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.), the disclosure of which is incorporated herein by reference.
  • 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 by way of apparatus discussed previously.
  • 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.
  • surfactant paste structuring process e.g., hardening an aqueous anionic surfactant paste by incorporating a paste-hardening material by using an extruder, prior to the process of the present invention.
  • surfactant paste structuring process e.g., hardening an aqueous anionic surfactant paste by incorporating a paste-hardening material by using an extruder.
  • Example 1 The following is an example for obtaining agglomerates having high density (over 700g/l), using a L ⁇ dige CB mixer (CB-30), followed by a L ⁇ dige KM mixer (KM-600), and lastly using Fluid Bed Apparatus for drying/cooling.
  • CB-30 L ⁇ dige CB mixer
  • KM-600 L ⁇ dige KM mixer
  • 70 kg/hr of sodium aluminosilicate (mean particle size of 2.45 microns), 130 kg/hr of ground light sodium carbonate (mean particle size of 18.3 microns), 223 kg/hr of sodium tripolyphosphate (mean particle size of 22 microns), 130 kg/hr of sulfate (mean particle size of 165 microns), and 288 kg/hr recylced fines (mean particle size of 111 microns) are fluidised in a CB-30 mixer.
  • the CB's rpm is preferably 900.
  • the total surface area of all the powder materials is 1051 m 2 /kg.
  • the agglomerates from the CB-30 mixer are fed to the KM-600 mixer for further agglomeration, rounding and growing the size of the agglomerates.
  • the KM's rpm is preferably 65.
  • Choppers from the KM mixer can be used to reduce the amount of oversized agglomerates.
  • the agglomerates from the KM mixer are fed to a fluid bed drying apparatus for drying and/or cooling.
  • the resulting granules have a density of about 800 - 900 g/l.
  • the total surface area of the powder materials to the amount of liquid detersive materials is about 0.93.
  • the amount of generated fines is about 2100 kg/hr.

Abstract

L'invention concerne un procédé de préparation d'une composition détergente granuleuse sans recourir à l'utilisation d'une tour. Ce procédé consiste à i) fluidifier les matières en poudre dans un mélangeur/broyeur haute vitesse brassant et découpant les matières en poudre renfermant une matière inorganique alcaline hydrosoluble solide et particulaire dans une quantité plus importante que celle requise pour la neutralisation, éventuellement mélangées avec un ou plusieurs autres solides particulaires et des fines recyclées, les matières en poudre présentant une zone de surface totale; ii) à ajouter les matières détergentes liquides dans le mélangeur/broyeur haute vitesse, les matières détergentes liquides renfermant un précurseur acide liquide, éventuellement mélangées à une ou plusieurs autres matières liquides afin de neutraliser le précurseur acide par la matière inorganique alcaline hydrosoluble; et iii) à broyer le mélange dans le mélangeur/broyeur haute vitesse afin d'obtenir des particules détergentes. Le rapport de la zone de surface totale des matières en poudre et de la quantité de matières détergentes liquides à l'étape ii) oscille entre 0,02 et environ 140.
PCT/US1998/022896 1998-10-28 1998-10-28 Procede de preparation d'une composition detergente a ecoulement facile WO2000024861A1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
EP98960152A EP1124931A1 (fr) 1998-10-28 1998-10-28 Procede de preparation d'une composition detergente a ecoulement facile
PCT/US1998/022896 WO2000024861A1 (fr) 1998-10-28 1998-10-28 Procede de preparation d'une composition detergente a ecoulement facile
CN98814282.1A CN1214101C (zh) 1998-10-28 1998-10-28 制备自由流动洗涤剂组合物的方法
US09/787,445 US6576605B1 (en) 1998-10-28 1998-10-28 Process for making a free flowing detergent composition
BR9816061-3A BR9816061A (pt) 1998-10-28 1998-10-28 Processo para a fabricação de uma composição detergente de circulação livre
CA002346340A CA2346340A1 (fr) 1998-10-28 1998-10-28 Procede de preparation d'une composition detergente a ecoulement facile
AU15819/99A AU1581999A (en) 1998-10-28 1998-10-28 Process for making a free flowing detergent composition
JP2000578416A JP2002528599A (ja) 1998-10-28 1998-10-28 易流動性洗剤組成物の製造方法

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PCT/US1998/022896 WO2000024861A1 (fr) 1998-10-28 1998-10-28 Procede de preparation d'une composition detergente a ecoulement facile

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WO2000024861A1 true WO2000024861A1 (fr) 2000-05-04

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JP (1) JP2002528599A (fr)
CN (1) CN1214101C (fr)
AU (1) AU1581999A (fr)
BR (1) BR9816061A (fr)
CA (1) CA2346340A1 (fr)
WO (1) WO2000024861A1 (fr)

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JP5653646B2 (ja) * 2010-04-16 2015-01-14 花王株式会社 有核酵素含有造粒物の製造方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0438320A2 (fr) * 1990-01-19 1991-07-24 Unilever Plc Compositions détergentes et leur procédÀ© de préparation
WO1998020104A1 (fr) * 1996-11-06 1998-05-14 The Procter & Gamble Company Procede de neutralisation destine a la fabrication de granules agglomerees de detergent
JPH10152700A (ja) * 1996-08-26 1998-06-09 Kao Corp 高嵩密度洗剤組成物の製造方法
WO1998038279A1 (fr) * 1997-02-27 1998-09-03 The Procter & Gamble Company Procede de preparation d'une composition detergente par l'addition de cotensioactifs

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0438320A2 (fr) * 1990-01-19 1991-07-24 Unilever Plc Compositions détergentes et leur procédÀ© de préparation
JPH10152700A (ja) * 1996-08-26 1998-06-09 Kao Corp 高嵩密度洗剤組成物の製造方法
WO1998020104A1 (fr) * 1996-11-06 1998-05-14 The Procter & Gamble Company Procede de neutralisation destine a la fabrication de granules agglomerees de detergent
WO1998038279A1 (fr) * 1997-02-27 1998-09-03 The Procter & Gamble Company Procede de preparation d'une composition detergente par l'addition de cotensioactifs

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 9833, Derwent World Patents Index; Class A97, AN 98-381421, XP002107326 *

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CN1214101C (zh) 2005-08-10
EP1124931A1 (fr) 2001-08-22
AU1581999A (en) 2000-05-15
JP2002528599A (ja) 2002-09-03
CA2346340A1 (fr) 2000-05-04
BR9816061A (pt) 2001-07-10
CN1322235A (zh) 2001-11-14

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