EP0971999A1

EP0971999A1 - Granulated detergents

Info

Publication number: EP0971999A1
Application number: EP98912430A
Authority: EP
Inventors: Thomas Holderbaum; Thomas Merz; Edgar Köppelmann
Original assignee: Henkel Ecolab GmbH and Co KG
Current assignee: Ecolab GmbH and Co OHG
Priority date: 1997-03-12
Filing date: 1998-03-03
Publication date: 2000-01-19
Also published as: DE19710156A1; WO1998040454A1

Abstract

The invention relates to a very simple and economical method for producing flowable detergents for use in the commercial sector. Said detergents are highly stable during storage and easy to handle. This is basically accomplished by granulating a mixture comprising at least 8 wt. % silicate and at least 12 wt. % of an at least partially liquid non-ionic surfactant, in relation to the finished detergent, with optionally additional common, particularly non-surfactant, detergent constituents e.g. zeolite or sodium carbonate.

Description

Granulated detergent

The present invention relates to a commercial detergent and a method for producing particulate detergents for the commercial laundry sector.

Probably the simplest method for producing particulate detergents is to mix powdery individual components, for example sodium carbonate, sodium tripolyphosphate and sodium perborate. Since some of these solid inorganic detergent ingredients are sufficiently porous and absorbent, liquid ingredients, which include surfactant substances in particular, can be sprayed onto the mixed product or one or more of the powdery individual components and thus also find their way into the detergent in a simple manner. This approach quickly reaches its limits if, on the one hand, increased demands are placed on the chemical stability of the detergent ingredients, which can be impaired by contact with one another, and on the other hand on the physical stability of the detergent. This includes the requirement for minimizing segregation processes, which can occur due to different particle sizes of the ingredients, during storage and transportation of the detergent, as well as that for consistently good handling over long periods of time, which is determined by the debris and free-flowing properties of the detergent . A widely used solution to these tasks results from the known spray drying of heat-resistant detergent ingredients and separate admixing of the thermally sensitive constituents, which generally have to be pre-assembled in particle form. However, such a method means that the manufacturing process is considerably more expensive when compared to the simple mixing process. While this price increase is accepted because of the above-mentioned associated immense advantages in the applicability of detergents for use in household laundry, it is higher for detergents for use in commercial laundries Meaning too. There, in extreme cases, one would even be prepared to meter out the individual components or storage-stable premixes from them separately, because of the lower complexity of the detergent compositions, if this would save costs. However, such a procedure is relatively labor-intensive, leads to poor washing results if the metering adjustment is incorrect, and cannot be used easily on commercial washing machines which have automatic metering devices, since these cannot be adapted indefinitely to the metering of a wide variety of active ingredients.

The invention, with which the problems addressed are to be solved, is a process for the production of free-flowing detergents for commercial use by granulating solid and liquid components, which is characterized in that a mixture of, in each case based on the finished detergent, at least 8% by weight of silicate (calculated as anhydrous) and at least 12% by weight of at least partially liquid nonionic surfactant, optionally granulated with further, in particular non-surfactant, detergent ingredients, such as zeolite or sodium carbonate.

The invention further relates to a particulate detergent which contains at least 12% by weight, preferably more than 12% by weight, of nonionic surfactant and at least 8% by weight, preferably more than 8% by weight of alkali silicate, preferably alkali metal silicate, and values of over 70% achieved in the trickle test described below.

To carry out the trickle test, 1000 ml of the substance to be tested are placed in a round funnel made of plastic, e.g. PVC (diameter of the upper funnel opening 80.5 mm, diameter of the lower funnel opening 10 mm, inclination 15 °, straight lower outlet pipe with a length of 30 mm and Diameter 10 mm), which is provided at its upper opening with an open top attachment of the same inner diameter and was attached to a tripod. During filling, the lower opening of the outlet pipe is closed and then opened so that the substance to be tested can run out. The time until the test material completely runs out is measured and compared with the time it takes for a dry standard sand to run out under these conditions. A sand whose run-out time is below the specified is usable as standard sand Conditions is 50 seconds ± 10 seconds. Its expiry time is set to 100%. This time is divided by the run-off time of the detergent sample to get the trickle test result of the detergent. Agents according to the invention have a trickle test value of over 70%, preferably of at least 80%.

As part of the manufacturing process according to the invention, it is possible to carry out the granulation in a mixer / granulator or in a plurality of mixers / granulators connected in series, which may have different mixing and granulating speeds. In a preferred embodiment of the invention, the granulation is carried out in two mixers / granulators connected in series. It is advantageous if a pre-granulate is first created in a high-speed mixer and then - if necessary with the addition of further solid and liquid constituents, in particular with the addition of up to 50% by weight, based on the finished, but still undried, granulate to solid to powdery components - the actual granulation and compaction takes place in a slower running mixer / granulator. The residence time in the high-speed mixer is usually less than 1 minute, in particular significantly less than 1 minute, while the residence times in the preferably continuously operating slower granulators can be up to several minutes, for example between 1 and 10 minutes.

In particular, however, a process control is preferred which, according to the teaching of international patent application WO 93/23523, also uses two consecutive mixers / granulators, but first the slower-running mixer / granulator and then the high-speed mixer are used.

The solid and liquid components can be added in any order. In a preferred embodiment, however, the solid constituents are initially introduced and then the liquid components, with the mixing tools running, to which, in the context of this invention, also those at the respective processing temperature, which are normally between 30 ° C. and 70 ° C. is in particular between 40 ° C and 60 ° C, belong to pumpable components, added. Nonionic surfactants are preferably used as liquid constituents used which are completely liquid at room temperature or flowable at the respective processing temperature.

In addition to nonionic surfactants, water and, for example, also anionic surfactant acids, anionic surfactant pastes, aqueous alkali metal hydroxide solutions, in particular sodium hydroxide solution, polycarboxylate solutions and / or phosphonate solutions can be used as liquid constituents or pumpable at the respective processing temperature. If desired, silicones and paraffins can also be used in minor amounts. However, it is particularly preferred that aqueous solutions and or aqueous dispersions are used in this process step, with surfactant-containing solutions and / or dispersions also being suitable at this point in the process.

The granulation is continued until the desired particle size distribution, that is to say the desired granule structure, has been reached. The total mixing and granulating time is preferably between 1 and 10 minutes, in particular between 2 and 8 minutes, with mixing and granulating times between 3 and 5 minutes being particularly advantageous. Mixing times that are too long may result in undesirably high coarse grain fractions. Granules produced according to the invention preferably have an average particle size in the range from 0.2 mm to 1.2 mm, in particular from 0.4 mm to 1.0 mm. It is preferably free of particles larger than 2 mm in size.

The granules can be treated with an aqueous solution or an aqueous dispersion of one or more non-surfactant ingredients of detergents or cleaning agents before or during drying. Of course, it is also possible for the aftertreatment to be carried out with several solutions and / or dispersions, but this is generally not preferred. This treatment must take place in such a way that the surface of the granules is covered, but further granulation in the sense of progressive build-up granulation is largely avoided. Water-soluble inorganic salts, such as amorphous silicates, carbonates are preferred as non-surfactant ingredients of detergents. Sulfates, and / or organic salts such as phosphonates, polycarboxylates, especially citrate, and polymeric polycarboxylates are used. Are particularly preferred aqueous solutions of sodium silicates and / or polymeric polycarboxylates. The aqueous solutions contain the non-surfactant detergent ingredient (s) preferably in concentrations of 25 to 50% by weight and in particular in amounts of 30 to 40% by weight. The aqueous solution or dispersion or the aqueous solutions or dispersions are preferably used in amounts of 1 to 15% by weight and in particular in amounts of 2 to 8% by weight, based on the untreated granules.

Any drying process that follows the granulation can be carried out in all conventional drying devices. However, drying in the fluidized bed is preferred. If desired, a finely divided powder with an average particle size of less than 40 μm, preferably of at most 10 μm, can be added during or after the drying step, preferably during the drying in the fluidized bed. Such finely divided powders are, for example, hydrophobic or hydrophilic silicas, calcium or magnesium stearates, calcium or magnesium carbonates, aluminum silicates, in particular zeolite A and / or zeolite P, and titanium dioxide. Mixtures of finely divided powders can also be used. As is known, this measure allows the bulk density of the granules to be increased.

The process according to the invention can be carried out continuously, both batchwise and advantageously. Free-flowing and storage-stable granules are obtained which have bulk densities of preferably above 700 g / 1, in particular in the range from 850 g / 1 to 1000 g / 1. The content of the finished, finally dried granules of nonionic surfactants is over 12% by weight.

All known detergent ingredients can advantageously be used in the commercial laundry in the process according to the invention. Such agents are preferably highly alkaline detergents which, in aqueous solution, have a pH in the range from 10 to 13, in particular from 10 to 12, at a concentration of 1% by weight. The solid ingredients can preferably be introduced into the process as powder, but if desired also as prefabricated granules. To adjust the required alkaline pH in the wash liquor, the agent produced according to the invention contains larger amounts of alkalizing agents, which include, in particular, alkali metal silicates and alkali carbonates, but also the alkali metal hydroxides. Such alkalizing agents are present in the agents according to the invention preferably in amounts of 20% by weight to 85% by weight, in particular 30% by weight to 50% by weight, mixtures of anhydrous alkali metasilicate, in particular sodium metasilicate, and alkali carbonate, especially sodium carbonate, from 8: 1 to 1: 2 are preferred.

An agent produced according to the invention also contains nonionic surfactant, in particular in an amount in the range from 12% by weight to 25% by weight. preferably from 15% to 22% by weight. The nonionic surfactants in question include the alkoxylates, in particular the ethoxylates and / or propoxylates of saturated or mono- to polyunsaturated linear or branched chain alcohols having 10 to 22 carbon atoms, preferably 12 to 18 carbon atoms. The degree of alkoxylation of the alcohols is generally in the range from 1 to 20, preferably from 3 and 14. They can be prepared in a known manner by reacting the corresponding alcohols with the corresponding alkylene oxides. The derivatives of fatty alcohols are particularly suitable, although their branched chain isomers, in particular so-called oxo alcohols, can also be used to prepare alkoxylates which can be used. Accordingly, the alkoxylates, in particular the ethoxylates, of primary alcohols with linear, in particular dodecyl, tetra-decyl, hexadecyl or octadecyl radicals, and mixtures thereof, can be used. In addition, 1 to 20 times, in particular 3 to 10 times, alkoxylation products of alkylamines, vicinal diols and carboxamides, which correspond to the alcohols mentioned with regard to the alkyl part, can be used. In addition, there are the ethylene oxide and / or propylene oxide insertion products of fatty acid alkyl esters, as can be prepared in accordance with the process specified in international patent application WO 90/13533, and fatty acid polyhydroxyamides, as are, for example, in accordance with the processes of the US patent specifications US 1 985 424, US 2 016 962 and US 2 703 798 and international patent application WO 92/06984 can be considered. So-called alkyl polyglycosides suitable for incorporation into the agents according to the invention are compounds of general formula (G) _p -OR, in which R is an alkyl or alkenyl radical having 8 to 22 carbon atoms, G is a glycose unit and p is a number between 1 and 10. Such compounds and their preparation are described, for example, in European patent applications EP 92 355, EP 301 298, EP 357 969 and EP 362 671 or US Pat. No. 3,547,828. The glycoside component (G) _p is oligomers or polymers from naturally occurring aldose or ketose monomers, in particular glucose, mannose, fructose, galactose, talose, gulose, altrose, allose, idose, ribose, arabinose, Xylose and Lyxose belong to. 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. The degree of oligomerization p generally takes fractional numerical values as the quantity to be determined analytically; it is between 1 and 10, for the glycosides preferably used below 1.5, in particular between 1.2 and 1.4. The preferred monomer building block is glucose because of its good availability. The alkyl or alkenyl part R of the glycosides preferably also originates from easily accessible derivatives of renewable raw materials, in particular from fatty alcohols, although their branched-chain isomers, in particular so-called oxo alcohols, can also be used to produce usable glycosides. Accordingly, the primary alcohols with linear octyl, decyl, dodecyl, tetradecyl, hexadecyl or octadecyl radicals and mixtures thereof are particularly useful. Particularly preferred alkyl glycosides contain a coconut fatty alkyl radical, ie mixtures with essentially R = dodecyl and R = tetradecyl.

Agents according to the invention or produced by the method according to the invention can additionally contain further surfactants, in particular synthetic anionic surfactants of the sulfate or sulfonate type, in amounts of preferably not more than 10% by weight, in particular from 0.1% by weight to 5% by weight, in each case based on the total mean. Synthetic anionic surfactants which are particularly suitable for use in such compositions are the alkyl and / or alkenyl sulfates having 8 to 22 carbon atoms and carrying an alkali metal, ammonium or alkyl or hydroxyalkyl-substituted ammonium ion as countercation. The derivatives of fatty alcohols having in particular 12 to 18 carbon atoms are preferred and their branched chain analogs, the so-called oxo alcohols. The alkyl and alkenyl 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. In addition to the alkylbenzenesulfonates, suitable anionic surfactants of the sulfonate type include the .alpha.-sulfoesters obtainable by reacting fatty acid esters with sulfur trioxide and subsequent neutralization, in particular those derived from fatty acids having 8 to 22 carbon atoms, preferably 12 to 18 carbon atoms, and linear Alcohols with 1 to 6 carbon atoms, preferably 1 to 4 carbon atoms, derived sulfonation products, as well as the sulfofatty acids resulting from these by formal saponification.

Soaps can be considered as further optional surfactant ingredients, whereby saturated fatty acid soaps, such as the salts of lauric acid, myristic acid, palmitic acid or stearic acid, as well as soaps derived from natural fatty acid mixtures, for example coconut, palm kernel or tallow fatty acids, are suitable. Soap mixtures are particularly preferred which are composed of 50% by weight to 100% by weight of saturated C ₁₂ -C ₁₈ fatty acid soaps and up to 50% by weight of oleic acid soap. Soap is preferably contained in amounts of up to 15% by weight, in particular from 2% by weight to 8% by weight.

An agent according to the invention or produced by the method according to the invention can be water-soluble and / or water-insoluble builders, in particular selected from alkali alumosilicate, alkali tripolyphosphate, crystalline alkali silicate with a modulus above 1, monomeric polycarboxylate, polymeric polycarboxylate and mixtures thereof, preferably in amounts in the range from 10% by weight. % to 50 wt .-%, in particular from 15 wt .-% to 40 wt .-%, contain. In addition to monomeric polycarboxylic acids such as citric acid or salts thereof, organic builders are suitable from the class of the aminopolycarboxylic acids and polyphosphonic acids. The aminopolycarboxylic acids include nitrilotriacetic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid and their higher homologues, preference being given to using N, N-bis (carboxymethyl) aspartic acid becomes. Suitable polyphosphonic acids are l-hydroxyethane-l, l-diphosphonic acid. A inotri (methylenephosphonic acid), ethylenediaminetetra (methylenephosphonic acid) and their higher homologues, such as, for example, diethylenetetraminetetra (methylenephosphonic acid). The water-soluble organic builder substances from the class of the polymeric polycarboxylic acids include, in particular, the polycarboxylates of the international patent application WO 93/16110 which are accessible by oxidation of polysaccharides, and polymeric acrylic acids, methacrylic acids, maleic acids and mixed polymers from these, which also contain small amounts of polymerizable substances may contain copolymerized without carboxylic acid functionality. The relative molecular weight of the homopolymers of unsaturated carboxylic acids is generally between 5000 and 200000, 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 methyl ether, vinyl esters, ethylene, propylene and styrene, in which the proportion of acid is at least 50% by weight. Terpolymers which contain two unsaturated acids and / or their salts as monomers and vinyl alcohol and / or a vinyl alcohol derivative or a carbohydrate as the third monomer can also be used as water-soluble organic builder substances. The use of the third monomer presumably creates predetermined breaking points in the polymer, which are responsible for the good biodegradability of the polymer. These terpolymers can be produced in particular by processes which are described in German patent specification DE 42 21 381 and German patent application DE 43 00 772 and generally have a relative molecular mass between 1000 and 200000, preferably between 200 and 50,000 and in particular between 3000 and 10,000. They can be used in the form of aqueous solutions, preferably in the form of 30 to 50 percent by weight aqueous solutions. All of the polycarboxylic acids mentioned are generally used in the form of their water-soluble salts, in particular their alkali metal salts.

In particular, crystalline or amorphous alkali alumosilicates, in amounts of up to 50% by weight, are provided as water-insoluble, water-dispersible inorganic builder materials. preferably not more than 40% by weight. Among them, the crystalline aluminosilicates in detergent quality, in particular zeolite A, zeolite P and optionally zeolite X, alone or in mixtures, are preferred. Suitable aluminosilicates in particular have no particles with a grain size above 30 μm and preferably consist of at least 80% by weight of particles with a size below 10 μm. Their calcium binding capacity, which can be determined according to the information in German patent DE 24 12 837, is generally in the range from 100 to 200 mg CaO per gram. Suitable substitutes or partial substitutes for the aluminosilicate mentioned are certain crystalline or amorphous alkali silicates, which can be present alone or in a mixture with one another. The alkali silicates which can be used as builders in the agents according to the invention have a molar ratio of alkali oxide to SiO ₂ below 0.95, in particular from 1: 1.1 to 1:12. Alkali silicates preferred as builder substances are the sodium silicates, in particular the amorphous sodium silicates, with a Na ₂ O: SiO ₂ molar ratio of 1: 2 to 1: 2.8, as can be prepared, for example, by the process of European patent application EP 0 425 427 . Silicates which can be used as builders are also described, for example, in European patent application EP 0 164 514.

In addition to the inorganic builder mentioned and the alkalizing agent, further water-soluble or water-insoluble inorganic solid substances can be used in the agents produced according to the invention. In this context, the alkali chlorides, alkali hydrogen carbonates and alkali sulfates and mixtures thereof are suitable. Such additional inorganic filler material can be present in amounts up to 40% by weight, but is preferably absent entirely.

In addition, the agents can contain further constituents customary in washing and cleaning agents. These optional components include in particular enzymes, so-called soil release polymers, for example copolyesters, the dicarboxylic acid units. Alkylene glycol units and polyalkylene glycol units contain complexing agents for heavy metals, for example aminopolycarboxylic acids, aminohydroxypolycarboxylic acids, polyphosphonic acids, hydroxypolyphosphonic acids and / or aminopolyphosphonic acids. Anti-graying gates, color transfer inhibitors, for example polyvinyl pyrrolidone or polyvinyl pyridine-N-oxide, foam inhibitors, for example fatty alcohol phosphoric acid esters. Organopolysiloxanes or paraffins, and optical brighteners, for example stilbene disulfonic acid derivatives. Preferably up to 1% by weight, in particular 0.01% by weight to 0.5% by weight, of optical brighteners, in particular compounds from the class of the substituted 4,4'-bis- (2nd , 4,6-triamino-s-triazinyl) -stilbene-2,2'-disulfonic acids, up to 5% by weight, in particular 0.1% by weight to 2% by weight, of complexing agents for heavy metals, in particular hydroxyalkylenephosphonic acids and their salts, and up to 2% by weight, in particular 0.05% by weight to 1% by weight, of foam inhibitors, the proportions by weight referred to in each case based on the total agent.

Any enzyme present are preferably selected from the group comprising protease, amylase, lipase, cellulase, hemicellulase, oxidase, peroxidase or mixtures of these. Protease obtained from microorganisms, such as bacteria or fungi, is primarily suitable. It can be obtained in a known manner by fermentation processes from suitable microorganisms, which are described, for example, in German Offenlegungsschriften DE 19 40 488, DE 20 44 161, DE 21 01 803 and DE 21 21 397, and US Pat. Nos. 3,623 957 and US 4,264,738, European patent application EP 006 638 and international patent application WO 91/02792. Proteases are commercially available, for example, under the names BLAP®, Savinase®, Esperase®, Maxatase®, Optimase®, Alcalase®, Durazym® or Maxapem®. The lipase which can be used can be obtained from Humicola lanuginosa, as described, for example, in European patent applications EP 258 068, EP 305 216 and EP 341 947, from Bacillus species, as described, for example, in international patent application WO 91/16422 or European patent application EP 384 717 , from Pseudomonas species, for example in European patent applications EP 468 102, EP 385 401, EP 375 102, EP 334462, EP 331 376, EP 330 641, EP 214 761, EP 218 272 or EP 204 284 or the international patent application WO 90/10695 described, from Fusarium species, as described for example in European patent application EP 130 064, from Rhizopus species, as described for example in European patent application EP 117 553, or from Aspergillus species, as described, for example, in European patent application EP 167 309. Suitable lipases are commercially available, for example, under the names Lipolase®, Lipozym®, Lipomax®, Amano® lipase, Toyo-Jozo® lipase, Meito® lipase and Diosynth® lipase. Suitable amylases are commercially available, for example, under the names Maxamyl®, Termamyl® and Duramyl®. The cellulase which can be used can be an enzyme which can be obtained from bacteria or fungi and which has a pH optimum, preferably in the weakly acidic to weakly alkaline range from 6 to 9.5. Such cellulases are known, for example, from German published applications DE 31 17 250, DE 32 07 825, DE 32 07 847, DE 33 22 950 or European patent applications EP 265 832, EP 269 977, EP 270 974, EP 273 125 and EP 339 550 known.

Suitable foam inhibitors include phosphoric acid mono- and difatty alkyl esters, long-chain soaps, in particular beef soap, fatty acid amides, paraffins, waxes, microcrystalline waxes, organopolysiloxanes and mixtures thereof, which may additionally contain microfine, optionally silanized or otherwise hydrophobized silica. Such foam inhibitors are preferably bound to granular, water-soluble carrier substances, as described, for example, in German Offenlegungsschrift DE 34 36 194, European patent applications EP 262 588, EP 301 414, EP 309 931 or European patent EP 150 386.

In a preferred embodiment, an agent according to the invention or manufactured according to the method according to the invention contains up to 6% by weight, in particular 2% by weight to 5% by weight, of synthetic anionic surfactant from the group comprising alkylbenzenesulfonate and alkylsulfate, up to 10% by weight .-%, in particular 3 wt .-% to 8 wt .-% soap, 12 wt .-% to 25 wt .-%, in particular 15 wt .-% to 22 wt .-% nonionic surfactant in the form of alkoxylated fatty alcohols, in particular an approximately 2: 1 to 1: 1 mixture of low ethoxylated fatty alcohol, for example 3-fold ethoxylated C _12.18 fatty alcohol, with higher ethoxylated fatty alcohol, for example 7-fold ethoxylated C _16/18 fatty alcohol, 10% by weight % to 50% by weight of alkali metal silicate, 4% by weight to 50% by weight of alkali carbonate, up to 2% by weight, in particular 0.1% by weight to 2% by weight of complexing agents from the class of the phosphonic acids , up to 30% by weight of water-soluble inorganic builders, in particular sodium tripolyphosphate, up to 6% by weight, in particular up to 4% by weight of organic cobuilders, up to 0.5% by weight of optical brighteners and up to 2% by weight. -%, in particular 0.4 wt .-% to 1.5 wt .-% soil release polymer.

A detergent produced according to the invention can be metered into a commercial washing machine with ease using a conventional, controlled powder metering device, such as is known, for example, from European Patent EP 0 297 371. Preferably, more than 1000 g of a detergent according to the invention can be metered within 30 seconds using such a powder metering device.

Examples

example 1

In a ploughshare mixer (manufacturer Drais) 3.04 kg of zeolite Na-A (Wessalith® P, manufacturer Degussa AG), 0.08 kg powdered sodium polycarboxylate (Sokalan® CP 5, manufacturer BASF AG), 1.17 kg coated sodium carbonate and 0.95 kg sodium metasilicate submitted. These solid components are granulated after adding 0.97 kg of water, 0.56 kg of 7-fold ethoxylated fatty alcohol (Dehydol® LT 7, manufacturer Henkel KGaA) and 0.82 kg of 3-fold ethoxylated fatty alcohol (Dehydol® LS 3, manufacturer Henkel KGaA). After drying in a fluidized bed dryer and sieving the coarse particles with a diameter of over 1.6 mm, granules Ml with good flowability were obtained, which had a bulk density of 900 g / 1 and a value in the trickle test in the range from 80% to 88%. With the aid of the powder metering device known from European patent EP 0 297 371, 1600 g of this agent could be metered in within 30 seconds.

Example 2

A comparative product VI, which contained the same ingredients as Ml according to Example 1, was obtained by simply mixing the components in a Forberg mixer, in which the zeolite and the polycarboxylate were combined in the form of a spray-dried powder and this was applied to the other components. The agent obtained in this way could not be metered using the powder metering device known from European Patent EP 0 297 371. The trickle test gave a value of 0%, which means that due to the formation of bridges, no powder ran out of the funnel opening.

Claims

claims

1. Particulate detergent which contains at least 12% by weight of nonionic surfactant and at least 8% by weight of alkali silicate, in particular alkali metasilicate, and reaches a value of over 70% in the trickle test.

2. Composition according to claim 1, characterized in that it reaches a value of at least 80% in the trickle test.

3. Composition according to claim 1 or 2, characterized in that there are up to 6 wt .-%, in particular 2 wt .-% to 5 wt .-% synthetic anionic surfactant from the group comprising alkylbenzenesulfonate and alkyl sulfate, up to 10 wt .-% %, in particular 3% by weight to 8% by weight of soap, 12% by weight to 25% by weight, in particular 15% by weight to 22% by weight of nonionic surfactant in the form of alkoxylated fatty alcohols, in particular approximately one 2: 1 to 1: 1 mixture of low ethoxylated fatty alcohol with higher ethoxylated fatty alcohol, 10% by weight to 50% by weight of alkali metal silicate, 4% by weight to 50% by weight of alkali carbonate. up to 2% by weight, in particular 0.1% by weight to 2% by weight of complexing agents from the class of the phosphonic acids, up to 30% by weight of water-soluble inorganic builders, in particular sodium tripolyphosphate, up to 6% by weight , in particular up to 4% by weight of organic cobuilder, up to 0.5% by weight of optical brightener and up to 2% by weight, in particular 0.4% by weight to 1.5% by weight, of dirt-releasing polymer contains.

4. Composition according to one of claims 1 to 3, characterized in that it has a pH in the range from 10 to 13 at a concentration of 1 wt .-% in aqueous solution.

5. A process for the preparation of free-flowing detergents for commercial use by granulating solid and liquid components, characterized in that a mixture of, based in each case on the finished detergent, at least 8% by weight of silicate (calculated as anhydrous) and at least 12% by weight .-% at least partially liquid nonionic surfactant granulated with, if appropriate, further customary, in particular non-surfactant, detergent components.

6. The method according to claim 5, characterized in that the liquid constituents used are nonionic surfactants which are completely liquid at room temperature or flowable at the respective processing temperature.

7. The method according to claim 5 or 6, characterized in that the granulation is carried out in two consecutive mixers / granulators.

8. The method according to any one of claims 5 to 7, characterized in that water-soluble inorganic salts such as amorphous silicates as non-surfactant detergent ingredients. Carbonates or sulfates, and / or organic salts such as phosphonates, polycarboxylates, especially citrate, and polymeric polycarboxylates are used.

9. The method according to any one of claims 5 to 8, characterized in that the processing temperature is between 30 and 70 ° C, in particular between 40 and 60 ° C.

10. The method according to any one of claims 5 to 9, characterized in that the total mixing and granulation time is between 1 and 10 minutes, in particular between 2 and 8 minutes.

11. The method according to any one of claims 5 to 10, characterized in that the granules produced have an average particle size in the range from 0.2 mm to 1.2 mm, in particular from 0.4 mm to 1.0 mm.