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WO1996010070A1 - Amelioration apportee a un procede d'extrusion pour la production de detergents - Google Patents

Amelioration apportee a un procede d'extrusion pour la production de detergents Download PDF

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Publication number
WO1996010070A1
WO1996010070A1 PCT/EP1995/003668 EP9503668W WO9610070A1 WO 1996010070 A1 WO1996010070 A1 WO 1996010070A1 EP 9503668 W EP9503668 W EP 9503668W WO 9610070 A1 WO9610070 A1 WO 9610070A1
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WIPO (PCT)
Prior art keywords
weight
silicone oil
spray
surfactant
alkyl
Prior art date
Application number
PCT/EP1995/003668
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German (de)
English (en)
Inventor
Kathrin Schnepp
Monika Böcker
Manfred Greger
Dieter Jung
Norbert Kühne
Josef Markiefka
Wolfgang Seiter
Original Assignee
Henkel Kommanditgesellschaft Auf Aktien
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 Henkel Kommanditgesellschaft Auf Aktien filed Critical Henkel Kommanditgesellschaft Auf Aktien
Priority to EP95933387A priority Critical patent/EP0784668A1/fr
Publication of WO1996010070A1 publication Critical patent/WO1996010070A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
    • 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
    • C11D11/02—Preparation in the form of powder by spray drying
    • 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

Definitions

  • the invention relates to an improved method for producing granular detergents with a high bulk density.
  • Granular detergents with a high bulk density can be produced according to the process of international patent application WO 91/02047. This involves the extrusion of a homogeneous pre-mix of detergent ingredients over perforated molds, which preferably have an opening width of 0.5 mm to 5 mm, subsequent crushing of the extrudate and subsequent treatment in a rounding machine, which is largely uniform spherical products leads.
  • the compacting extrusion step gives granular particles with bulk densities of generally 700 g / 1 to 1050 g / 1.
  • These can be complete washing or cleaning agents or constituents of such agents, which are completed by admixing other components that are usually not co-extrudable, for example solid or solid bleach activators, foam regulators or enzymes.
  • the detergent ingredients provided for extrusion can usually be used in the form of solid pre-products, so-called compounds, which contain two or more customary detergent ingredients.
  • Such granular compounds can be produced by customary processes, for example spray drying an aqueous slurry.
  • An advantage of such a procedure is that under normal conditions liquid detergent ingredients, for example nonionic surfactants, are used with the aid of carrier materials which themselves belong to the usual detergent ingredients.
  • inorganic builders can be made up in solid form and, by simply mixing separately prepared compounds in different proportions, comes to very different premixes for the extrusion and thus also to very different end products.
  • the invention therefore relates to a process for the preparation of detergents or cleaning agents or their constituents with a high bulk density by extrusion in the form of holes via hole shapes and subsequent comminution of the extrudate by means of a cutting device, which is characterized in that an aqueous slurry containing surfactant , inorganic builder and silicone oil, spray-dried using hot drying gases, the spray-drying product optionally mixed with further solid and / or solid-form detergent or cleaning agent components, extruded through a perforated plate and the extrudate optionally rounded and / or powdered.
  • Suitable silicone oils which can be used in the context of the invention, that is to say liquid organopolysiloxanes, are customary alkyl and aryl polysiloxanes, their copolymers and block polymers with polyalkylene oxides and their acylation products with long-chain fatty acids. They can be used as such or in a mixture with other conventional defoaming agents, which include paraffins, long-chain fatty acid esters and finely divided silica, which can also be silanized or otherwise hydrophobized. Mixtures of this type consist of at least 50% by weight, preferably at least 90% by weight and in particular at least 98% by weight, of organopolysiloxane.
  • Organopolysiloxanes containing silicic acid, in particular diethylpolysiloxane, are preferably used.
  • the viscosity of the silicone oils used is preferably 25000 mPa.s to 38000 mPa.s at room temperature; it can be determined by customary methods, for example using a Brookfield (R) viscometer model RVT using spindle No. 5 at 10 revolutions per minute , be measured.
  • the amount of such silicones contained in the spray drying product can vary within a very wide range and is normally up to about 1% by weight.
  • the spray drying product used in the process according to the invention preferably contains 25% by weight to 65% by weight, in particular 30% by weight to 60% by weight of inorganic builder, 7.5% by weight to 40% by weight , in particular 10% by weight to 30% by weight of surfactant, in particular synthetic anionic surfactant of the sulfate and / or sulfonate type, and 0.01% by weight to 0.7% by weight, in particular 0.015% by weight to 0.4% by weight silicone oil.
  • the remainder to 100% by weight consists of the usual ingredients of spray-dried washing or cleaning agents, in particular water, preferably organic in amounts of up to 20% by weight, in particular from 8% by weight to 18% by weight
  • Cobuilders which preferably in amounts up to 8% by weight, in particular from 3% by weight to 6.5% by weight
  • discoloration inhibitors which are preferably used in spray drying products intended for the production of detergents in amounts of up to 5% by weight, in particular 1.5% by weight to 3% by weight
  • inorganic water-soluble salts for example alkali metal sulfates and / or carbonates, which preferably in amounts of up to 20% by weight, in particular of 2 wt .-% to 12 wt .-% are included.
  • the spray drying product is compacted by extrusion, alone or in a mixture with other preferably solid detergent ingredients.
  • Such further detergent ingredients which can preferably be added in amounts of up to 50% by weight, in particular 5% by weight to 25% by weight, based on the premix to be extruded, include solid bleaching agents.
  • oxygen-based agents for example alkali perborates, which can be present as so-called monohydrates or tetrahydrates, or alkali percarbonates
  • powdered bleach activators for example a tetraacetylethylenedia in granulate, prepared in solid form, in solid form, prepared by the process of European patent EP 0037026
  • Anionic surfactant compounds containing active substance for example an alkyl sulfate compound produced according to the process of international patent application WO 93/04162
  • enzymes present in granular form for example an enzyme extrudate produced according to the process of international patent application WO 91/02792 or an according to the process of German patent application DE 4339463.4
  • Customary liquid ingredients of detergents and cleaning agents for example dyes or fragrances or additional, in particular nonionic, surfactants can, if desired, be applied to the spray-drying product and / or one of the other solid detergent ingredients mentioned before the extrusion step.
  • the stated other detergent or cleaning agent constituents can also, alternatively to their processing via the premix to be extruded, be admixed with the extrudate in order to obtain a finished detergent or cleaning agent.
  • a premix is preferably made from 20% by weight to 70% by weight of the spray drying product, 3% by weight to 20% by weight of anionic surfactant compound according to WO 93/04162 with a content of more than 80% by weight, in particular more than 90% Wt .-% of alkyl sulfate with alkyl chain lengths in the range of C12 to C ⁇ Q, balance essentially inorganic salts and water, 2 wt .-% to 10 wt .-% powdered, separately added alkali carbonate, 5 wt .-% to 20 wt.
  • % powdery, separately added polycarboxylate cobuilder for example alkali citrate, and 10% by weight to 20% by weight of peroxy bleach, for example sodium perborate monohydrate, and up to 20% by weight, in particular 5% to 20% %
  • polycarboxylate cobuilder for example alkali citrate
  • peroxy bleach for example sodium perborate monohydrate
  • liquid components for example water, aqueous alkali silicate or polycarboxylate solutions and / or liquid nonionic surfactants, produced and extruded, to which further solid or solid detergent ingredients, if desired, can be added after the extrusion.
  • a solid premix is extruded which contains 20% by weight to 35% by weight of inorganic builder, in particular zeolite, 1% by weight to 13% by weight of organic cobuilder, in particular monomeric and / or polymeric polycarboxylate, 15% by weight to 25% by weight of surfactant, in particular anion and / or nonionic surfactant, up to 20% by weight of bleaching agent and 0.01% by weight to 0.3% by weight
  • a solid premix which contains 20% by weight to 35% by weight of inorganic builder, in particular zeolite, 1% by weight to 13% by weight of organic cobuilder, in particular monomeric and / or polymeric polycarboxylate, 15% by weight to 25% by weight of surfactant, in particular anion and / or nonionic surfactant, up to 20% by weight of bleaching agent and 0.01% by weight to 0.3% by weight
  • a solid premix is extruded which contains 20% by weight to 35% by weight of inorganic builder, in particular ze
  • the extrusion is carried out under conditions known in principle, preferably using an extruder, into which the spray product or a homogeneous premix containing it is fed and under a pressure in the range from preferably 30 bar to 180 bar, in particular 40 bar to 80 bar, through a perforated plate with a hole diameter of preferably 1.2 mm to 2.0 mm, in particular 1.4 mm to 1.7 mm, extruded into strands and comminuted to a length that does not differ significantly from the thickness, that is to say the hole diameter becomes.
  • the extrudate if desired with application of powdery solids as described in particular in WO 94/01526, can then be rounded and deburred in a conventional rounding device, for example a spheronizer ( R ).
  • Suitable surfactants are selected from synthetic anionic surfactants, in particular of the sulfate or sulfonate type, nonionic surfactants, cationic surfactants and / or amphoteric surfactants.
  • Anionic surfactants are preferably selected from the class of alkyl sulfates, alkyl ether sulfates, sulfofatty acid disalts, alkyl sulfofatty acid esters. salts, alkanesulfonates and / or alkylbenzenesulfonates with linear Cg to Ci5 alkyl groups on the benzene nucleus.
  • the useful surfactants of the sulfate type include in particular primary alkyl sulfates with preferably linear alkyl radicals having 10 to 20 carbon atoms, which have an alkali metal, ammonium or alkyl or hydroxyalkyl-substituted ammonium ion as the counter cation.
  • the derivatives of linear alcohols with in particular 12 to 18 carbon atoms and their branched-chain analogs, the so-called oxo alcohols, are particularly suitable. Accordingly, the sulfation products of primary fatty alcohols with linear dodecyl, tetradecyl, hexadecyl or octadecyl radicals and mixtures thereof are particularly useful. Particularly preferred alkyl sulfates contain a tallow alkyl radical, that is to say mixtures with essentially hexadecyl and octadecyl radicals.
  • the alkyl sulfates can be prepared in a known manner by reacting the corresponding alcohol component with a conventional sulfating reagent, in particular sulfur trioxide or chlorosulfonic acid, and then neutralizing with alkali, ammonium or alkyl or hydroxyalkyl-substituted ammonium bases.
  • a conventional sulfating reagent in particular sulfur trioxide or chlorosulfonic acid
  • ether sulfates can be used as the anionic surfactant component.
  • Such ether sulfates preferably contain 2 to 30, in particular 4 to 10, ethylene glycol groups per molecule.
  • Suitable anionic surfactants of the sulfonate type include, in addition to the alkylbenzenesulfonates with preferably 9 to 15 carbon atoms in the linear alkyl chain in particular, the sulfoesters obtainable by reacting fatty acid esters with sulfur trioxide and subsequent neutralization, in particular those containing fatty acids 8 to 22 C-atoms, preferably 12 to 18 C-atoms, and linear alcohols with 1 to 6 C-atoms, preferably 1 to 4 C-atoms, sulfonation products, and the sulfofatty acid disalts that can be derived from them.
  • the alkanesulfonates are substances which are obtained by sulfoxidation of hydrocarbons, which preferably contain 10 to 20 carbon atoms. This generally results in products with a statistical distribution of the sulfonic acid substituents which, if desired, can be separated in a known manner.
  • Secondary alkanesulfonates with 12 to 17 are for agents according to the invention C atoms particularly suitable. Suitable cations in all cases of the anionic surfactants mentioned are, in particular, those from the group of alkali ions, ammonium or alkyl- or hydroxyalkyl-substituted ammonium ions.
  • the nonionic surfactants in question include, in particular, alkyl glycosides, fatty acid polyhydroxy ide, for example glucamides, as are produced, for example, in international patent application WO 92/06984, and the alkoxylates, in particular the ethoxylates and / or propoxylates of alcohols, Alkylamines, vicinal diols and / or carboxylic acid amides, which have alkyl groups with 10 to 22 carbon atoms, preferably 12 to 18 carbon atoms.
  • the degree of alkoxylation of these compounds is generally between 1 and 20, preferably between 3 and 10. They can be prepared in a known manner by reaction with the corresponding alkylene oxides.
  • Products which can be prepared by alkoxylation of fatty acid alkyl esters having 1 to 4 carbon atoms in the ester part by the process of international patent application WO 90/13533 are also suitable.
  • Preferred among the carboxamide derivatives are the ethanolamide derivatives of alkanoic acids with 8 to 22 carbon atoms, preferably 12 to 16 carbon atoms.
  • the alcohol alkoxylates in question include the ethoxylates and / or propoxylates of linear or branched chain alcohols having 10 to 22 carbon atoms, preferably 12 to 18 carbon atoms.
  • the derivatives of fatty alcohols are particularly suitable, although their branched-chain isomers can also be used for the preparation of usable alkoxylates.
  • the ethoxylates of primary alcohols with linear dodecyl, tetradecyl, hexadecyl or octadecyl radicals and mixtures thereof are particularly useful. It is also possible to use corresponding alkoxylates of mono- or polyunsaturated fatty alcohols, which include, for example, oleyl alcohol, elaidyl alcohol, linoleyl alcohol, linolenyl alcohol, gadoleyl alcohol and erucalcohol.
  • alkyl glycosides suitable as nonionic surfactant components for agents according to the invention and their preparation are described, for example, in European patent applications EP 92355, EP 301 298, EP 357 969 and EP 362671 or the US Pat. No. 3,547,828.
  • the glycoside components of such alkyl glycosides are oligo- or polymers from naturally occurring aldose or ketose monomers, which include in particular glucose, mannose, fructose, galactose, talose, gulose, altrose, allos, idose, ribose, arabinose, xylose and lyxose.
  • the oligomers consisting of such glycosidically linked monomers are characterized not only by the type of sugar they contain, but also by their number, the so-called degree of oligomerization, which, as an analytically determinable variable, can also assume fractional numerical values and generally between 1 and 10, in the alkyl glycosides preferably used is below a value of 1.5, in particular between 1.2 and 1.4.
  • the preferred monomer building block is glucose because of its good availability.
  • the alkyl part of such alkyl glycosides preferably also comes from easily accessible derivatives of renewable raw materials, in particular from the above-mentioned fatty alcohols, although their branched-chain isomers, in particular so-called oxo alcohols, can also be used to produce usable alkyl glycosides.
  • the primary alcohols with linear octyl, decyl, dodecyl, tetradecyl, hexadecyl or octadecyl radicals and mixtures thereof are particularly useful.
  • Particularly suitable alkyl glycosides contain a coconut fatty alkyl radical, that is to say mixtures with essentially dodecyl and tetradecyl radicals.
  • an agent according to the invention is to contain cationic surfactants, these are preferably selected from the quaternary ammonium compounds having at least one long-chain alkyl group having 10 to 22 carbon atoms.
  • these substances with two long-chain and two short-chain alkyl chains each having 1 to 4 carbon atoms on the nitrogen atom are particularly preferred because of their known textile-softening properties.
  • cationic surfactants usually have a halide anion, in particular chloride or bromide, or a sulfuric acid semi-ester anion, in particular methosulfate or ethosulfate, although quaternary ammonium compounds with anions which correspond to the synthetic anionic surfactants mentioned above can also be used.
  • Amphoteric surfactants are preferably selected from the derivatives of tertiary or quaternary aliphatic amines, the aliphatic radicals of which can be straight-chain or branched and one of which carries a carboxy, sulfo, phosphono, sulfato or phosphato group.
  • the agents according to the invention can contain soap, that is to say an alkali or ammonium salt of a CQ to C22 carboxylic acid.
  • Conventional water-soluble or water-insoluble, inorganic and / or organic builder materials can be used as builder components in detergents according to the invention.
  • Zeolites and silicates are preferred among the inorganic builder substances.
  • the finely crystalline, synthetic and bound water-containing zeolite is preferably A-type zeolite in detergent quality.
  • Mixtures of zeolite NaA and NaX are also suitable, the proportion of zeolite NaX in such mixtures advantageously being less than 30%. They normally have no particles larger than 30 ⁇ m and preferably consist at least 80% of particles smaller than 10 ⁇ m.
  • Suitable zeolites have an average particle size of less than 10 ⁇ m (measurement method: Eisenhofer diffraction; mean volume distribution), preferably between 1.5 and 4.5 ⁇ m, in particular between 2.0 and 4.0 ⁇ m.
  • Their calcium binding capacity which can be determined according to the information in German patent application 24 12837, is in the range from 100 to 200 mg CaO / g.
  • the content of finely divided, in particular crystalline, hydrated zeolite in the compositions is preferably 30 to 65% by weight and in particular 32 to 45% by weight, based on anhydrous active substance.
  • the zeolite generally has a water content of 17 to 25% by weight, in particular 20 to 22% by weight.
  • Alkali silicates which can be used additionally or instead can be amorphous or crystalline.
  • Preferred alkali silicates are the sodium silicates, in particular the amorphous sodium silicates, with a Na2O: SiO2 molar ratio of 1: 2 to 1: 2.8.
  • Such amorphous alkali silicates are commercially available, for example, under the name Portil ( R ).
  • Such crystalline layered silicates are described, for example, in European patent application 164 514.
  • both ⁇ - and S-sodium disilicate a2Si2 ⁇ 5 * yH2 ⁇ are preferred, whereby ⁇ -sodium disilicate can be obtained, for example, by the process described in international patent application WO91 / 08171.
  • the content of alkali silicates in the compositions is preferably 1 to 15% by weight and in particular 2 to 8% by weight, based on the anhydrous active substance.
  • the weight ratio of zeolite to amorphous silicate, based in each case on anhydrous active substance is preferably 4: 1 to 10: 1.
  • the crystalline layered silicates are preferably used in amounts of 1 to 15% by weight and in particular 2 to 7% by weight, the weight ratio of zeolite to crystalline layered silicate, in each case based on anhydrous active substance, preferably being at least 5: 1.
  • the weight ratio of amorphous alkali silicate to crystalline alkali silicate is preferably 1: 2 to 2: 1 and in particular 1: 1 to 2: 1.
  • Suitable organic builder components are polymeric carboxylates or polymeric carboxylic acids with a relative molecular weight of at least 350 in the form of their water-soluble salts, in particular in the form of the sodium and / or potassium salts, such as oxidized polysaccharides according to international patent application WO 93 / 08251, polyacrylates, polyhydroxyacrylates, polymethacrylates, polymaleates and in particular copolymers of acrylic acid with maleic acid or maleic anhydride, preferably such from 50 to 70% acrylic acid and 50 to 10% maleic acid.
  • the relative molecular weight of the homopolymers is generally between 1000 and 100000, that of the copolymers between 2000 and 200000, preferably 50,000 to 120,000, based on free acid.
  • a particularly preferred acrylic acid-maleic acid copolymer has a relative molecular weight of 50,000 to 100,000.
  • Suitable, albeit less preferred, compounds of this class are copolymers of acrylic acid or methacrylic acid with vinyl ethers, such as vinyl ethyl ethers, vinyl esters, ethylene, propylene and styrene, in which the proportion of the acid is at least 50% by weight.
  • Terpolymers can also be used as the polymeric carboxylates or carboxylic acids, the two carboxylic acids and / or their salts as monomers, and the third Monomer vinyl alcohol and / or a vinyl alcohol derivative or a carbohydrate contain.
  • the first acidic monomer or its salt is derived from a monoethylenically unsaturated C3-C ⁇ -carboxylic acid and preferably from a C3-C4-monocarboxylic acid, in particular from (meth) acrylic acid.
  • the second acidic monomer or its salt can be a derivative of a C / j-C ⁇ -dicarboxylic acid, preferably an f ⁇ -C ⁇ -dicarboxylic acid, maleic acid being preferred.
  • the third monomeric unit is formed from vinyl alcohol and / or preferably an esterified vinyl alcohol.
  • vinyl alcohol derivatives are preferred which are an ester of short-chain carboxylic acids, for example C 1 -C 4 -carboxylic acids, with vinyl alcohol.
  • Preferred terpolymers contain 60 to 95% by weight, in particular 70 to 90% by weight of (meth) acrylic acid or (meth) acrylate, particularly preferably acrylic acid or acrylate, and maleic acid or maleate and 5 to 40% by weight. %, preferably 10 to 30% by weight of vinyl alcohol and / or vinyl acetate.
  • Terpolymers in which the weight ratio (meth) acrylic acid or (meth) acrylate to maleic acid or maleate is between 1: 1 and 4: 1, preferably between 2: 1 and 3: 1 and in particular 2.1 and 2.5: 1.
  • the second acidic monomer or its salt can also be a derivative of an allylsulfonic acid which is in the 2-position with an alkyl radical, preferably with a C 1 -C 4 -alkyl radical, or an aromatic radical which is preferably derived from benzene or benzene derivatives derives, is substituted.
  • Preferred terpolymers contain 40 to 60% by weight, in particular 45 to 55% by weight of (meth) acrylic acid or (meth) acrylate, particularly preferably acrylic acid or acrylate, 10 to 30% by weight, preferably 15 to 25% by weight of methyl sulfonic acid or methylene sulfonate and as a third monomer 15 to 40% by weight, preferably 20 to 40% by weight of a carbohydrate.
  • This carbohydrate can be, for example, a mono-, di-, oligo- or polysaccharide, mono-, di- or oligosaccharides being preferred, saccharose being particularly preferred.
  • predetermined breaking points are built into the polymer, which are responsible for the degradability of the polymer.
  • sodium perborate tetrahydrate NaBÜ2 * H2O2 • 3 H2O
  • monohydrate NaB ⁇ 2 • H2O2
  • borates which provide H2O2 can also be used, for example the Perborax Na2B4Ü7 • 4 H2O2.
  • These compounds can be partially or completely by other active oxygen carriers, in particular by peroxyhydrates, such as peroxycarbonates (Na2C ⁇ 3 • 1.5 H2O2), peroxypyrophosphates, citrate perhydrates, urea-H2 ⁇ 2 or melamine-H2 ⁇ 2 compounds as well as by peracidic salts or peracids, such as perbenzoates , Peroxyphthalates, diperazelaic acid or diperdodecanedioic acid can be replaced.
  • peroxyhydrates such as peroxycarbonates (Na2C ⁇ 3 • 1.5 H2O2), peroxypyrophosphates, citrate perhydrates, urea-H2 ⁇ 2 or melamine-H2 ⁇ 2 compounds as well as by peracidic salts or peracids, such as perbenzoates , Peroxyphthalates, diperazelaic acid or diperdodecanedioic acid can be replaced.
  • bleach activators can be incorporated into the bleach-containing preparations.
  • these are N-acyl or O-acyl compounds which form organic peracids with H2O, preferably N, N'-tetraacylated diamines, such as NNN '.N'-tetraacetyl-ethylenediamine, furthermore carboxylic acid anhydrides, such as benzoic anhydride and phthalic anhydride, and esters of polyols such as glucose pentaacetate.
  • the bleach activator can be coated with coating substances in a known manner or, if necessary, be granulated using granulating aids and, if desired, contain further additives, for example dye.
  • Carboxymethyl cellulose is used for particulate detergents loose granulated tetraacetylethylenediamine (TAED) as can be prepared by the process described in European patent EP 037026, particularly preferred.
  • aqueous slurries were produced which contained 40 to 44% by weight of water, were heated to temperatures of about 60 ° C. to 80 ° C. and were sprayed under a pressure of 30 bar in a drying tower, where hot air (temperature 160 ° C to 220 ° C) was conducted in countercurrent.
  • the spray drying products S1 and S2 characterized in Table 1 by their composition were obtained, which had bulk densities of about 350 grams per liter.

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Abstract

L'invention concerne la fabrication d'agents de lavage et de nettoyage par compression d'un prémélange homogène de constituants de détergents sous forme de boudins, au moyen de moules perforés, puis par broyage de la matière extrudée qui est ensuite arrondie dans un appareil prévu à cet effet. Ceci permet d'obtenir des produits sphériques largement homogènes présentant une masse volumique apparente comprise généralement entre 700 g/l et 1050 g/l. L'invention vise à améliorer l'homogénéité du prémélange conçu pour l'extrusion ainsi que le lissé de la surface du granulé d'extrusion en évitant des différences de longueur. A cet effet, on sèche par pulvérisation une précipitation aqueuse renfermant un tensioactif, un adjuvant inorganique et de l'huile de silicone, au moyen de gaz de séchage chauds. Le produit de séchage par pulvérisation est mélangé le cas échéant avec d'autres constituants d'agents de lavage ou de nettoyage solides et/ou constituants préparés sous forme solide, extrudé à travers une plaque perforée, et la matière extrudée est éventuellement arrondie et/ou poudrée.
PCT/EP1995/003668 1994-09-27 1995-09-18 Amelioration apportee a un procede d'extrusion pour la production de detergents WO1996010070A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP95933387A EP0784668A1 (fr) 1994-09-27 1995-09-18 Amelioration apportee a un procede d'extrusion pour la production de detergents

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP4434500.3 1994-09-27
DE19944434500 DE4434500A1 (de) 1994-09-27 1994-09-27 Verbessertes Extrusionsverfahren zur Herstellung von Waschmitteln

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WO1996010070A1 true WO1996010070A1 (fr) 1996-04-04

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WO (1) WO1996010070A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6069124A (en) * 1997-05-30 2000-05-30 Lever Brothers Company Division Of Conopco, Inc. Granular detergent compositions and their production
EP0840780B1 (fr) * 1995-07-12 2000-11-15 Henkel Kommanditgesellschaft auf Aktien Produit granule de lavage ou de nettoyage a masse volumique apparente elevee
US6191095B1 (en) 1997-05-30 2001-02-20 Lever Brothers Company, A Division Of Conopco, Inc. Detergent compositions
US6221831B1 (en) 1997-05-30 2001-04-24 Lever Brothers Company, Division Of Conopco, Inc. Free flowing detergent composition containing high levels of surfactant
US6303558B1 (en) 1997-05-30 2001-10-16 Lever Brothers Co., Division Of Conopco Detergent composition containing at least two granular components
US9228157B2 (en) 2009-04-24 2016-01-05 Conopco, Inc. Manufacture of high active detergent particles

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6169899A (ja) * 1984-09-14 1986-04-10 花王株式会社 流動性の改良された高密度の粒状洗剤の製法
WO1991002047A1 (fr) * 1989-08-09 1991-02-21 Henkel Kommanditgesellschaft Auf Aktien Fabrication de granules comprimes pour produits de lavage
WO1994001526A1 (fr) * 1992-07-02 1994-01-20 Henkel Kommanditgesellschaft Auf Aktien Preparation detergente solide ayant un meilleur comportement au rinçage
DE4235646A1 (de) * 1992-10-22 1994-04-28 Henkel Kgaa Verfahren zur Herstellung wasch- und reinigungsaktiver Extrudate

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Cited By (6)

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EP0840780B1 (fr) * 1995-07-12 2000-11-15 Henkel Kommanditgesellschaft auf Aktien Produit granule de lavage ou de nettoyage a masse volumique apparente elevee
US6069124A (en) * 1997-05-30 2000-05-30 Lever Brothers Company Division Of Conopco, Inc. Granular detergent compositions and their production
US6191095B1 (en) 1997-05-30 2001-02-20 Lever Brothers Company, A Division Of Conopco, Inc. Detergent compositions
US6221831B1 (en) 1997-05-30 2001-04-24 Lever Brothers Company, Division Of Conopco, Inc. Free flowing detergent composition containing high levels of surfactant
US6303558B1 (en) 1997-05-30 2001-10-16 Lever Brothers Co., Division Of Conopco Detergent composition containing at least two granular components
US9228157B2 (en) 2009-04-24 2016-01-05 Conopco, Inc. Manufacture of high active detergent particles

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DE4434500A1 (de) 1996-03-28

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