DK154828B - PROCEDURE FOR THE PREPARATION OF A DUMPER DETERGENT - Google Patents

Abstract

1. A process for the production of a low-lather detergent consisting of several powder-form to particulate components, one of the powder components consisting of a polysiloxane defoamer and the remaining powder components consisting of spray-dried or granulated detergents of the usual composition and, optionally, bleaching agents, characterised in that, to produce the powder component containing the polysiloxane defoamer, an aqueous suspension which contains from 40 to 75% by weight (expressed as anhydrous compound) of at least one compound from the class of polymer phosphates, silicates, carbonates and sulfates of sodium and which is free from surfactants and contains no more than 0.3%, based on anhydrous salt, of polysiloxane defoamer is spray-dried in known manner using gases heated to between 120 and 300 degrees C and the particulate spray-dried product thus obtained which contains from 80 to 95% by weight of anhydrous salts is treated with 3 to 10% by weight, based on anhydrous salt, of polysiloxane defoamer consisting of a liquid mixture of polysiloxane and finely particulate silica in a ratio by weight of from 50:1 to 5:1, after which the particulate adsorbate obtained is mixed with the other powder components in such ratios by weight that the detergent contains from 0.01 to 0.5% by weight of silica-containing polysiloxane defoamer.

Description

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As is well known, the undesirable strong foaming of detergents can be suppressed by the addition of antifoaming mixtures of polydimethylsiloxane and finely divided silicic acid. Furthermore, it is known that the distribution state of the siloxanes in the detergent plays a significant role in the effect.

If the siloxanes are added to the slurry prior to the spray drying, a homogeneous distribution state is obtained, in which there is also no deterioration of the washing performance, but at the same time the anti-foaming effect is partially reversed.

In DE publication 23 38 468, a detergent is disclosed wherein the mixture of polysiloxane and silicic acid is incorporated in a carrier which is impermeable to the detergents. The purpose of this measure is to prevent an interaction between the detergents and the polysiloxane contained in the detergent and thus a decrease in the effect during mixing and storage. For this purpose, the mixture of polysiloxane and silicic acid is adsorbed on a solid support consisting of sodium carbonate, sodium silicate, sodium tripolyphosphate, clay, silica gher 20 or fuller soil or of starch, polyglycols, high ethoxylated fatty alcohols, gelatin or other gelling materials. The granular adsorbates are prepared by spray drying, spray cooling, or fluidization of liquid or molten mixtures of polysiloxane antifoam and carrier material. The produced grains or prills, respectively, are then coated with a coating material which may consist of the compounds used as the carrier material. The coating should counteract the adhesion of the grains and prevent interactions with other detergent ingredients, especially surfactants. The present disclosure recommends one method by which the polysiloxane components are sprayed onto a granular support, for example sodium tripolyphosphate, and in this form incorporated into the detergent as an unfavorable foam profile is obtained.

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It has now been found that the method of manufacture described does not lead to optimal results. When spray drying or spray cooling the melts or liquid mixtures, part of the irihibitor effect is lost. The grains often exhibit an insufficient wetting and dissolving ability, so that residue formation can occur due to undissolved constituents. In addition, a state of distribution of the poly siloxane is formed which, when using the detergent, results in poor washing results. This is particularly pronounced in a strong gray, especially of polyester-containing tavern laundry.

The object of the present invention is to overcome the disadvantages described. BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a process for producing a foam-dampened detergent consisting of several powdery to granular components, wherein one of the powder components consists of a poly-siloxane antifoam adsorbed on a carrier and the other powder components consist of spray-dried and granulated detergents of The present invention is characterized in that, for the preparation of the powder component containing the polysiloxane foam damper using 120 to 300 ° C hot gases, in a known manner, spray-drying an aqueous slurry containing 40-75% by weight. (calculated as anhydrous compound) of at least one compound of the class of polymer phosphates, silicates, carbonates and and sulfates of sodium, which slurry is free of surfactants and does not contain more than 0.3% by weight of anhydrous salt of polysiloxane antifoam, and treating the resulting granular spray product containing 80-95 wt% va non-anhydrous salts of 3 - 10% by weight (calculated on anhydrous salt) polysiloxane antifoam consisting of a liquid mixture of polysiloxane and finely divided silica in a weight ratio of 50: 1 to 6: 1 to which the adsorbate thus obtained is mixed. known per se with the other powder components in such weight ratios that the content of the detergent of silicic acid-containing polysiloxane antifoam is 0.01 to 0.5% by weight.

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The compounds useful in preparing the carrier are pentane sodium tripolyphosphate, sodium silicates of the composition Na 2 O: SiO 2 = 1: 1.5 to 1: 3, sodium carbonate and sodium sulfate. Preferably, salt mixtures containing at least two of the aforementioned salts are used. Such salt mixtures are spray dried by an aqueous slurry containing 50-70% by weight of anhydrous salt. The spray drying can take place in conventional spray drying systems, for example in so-called spray towers, in which the slurry is sprayed by means of nozzles and dried by means of heated gases, especially air or air-mixed combustion gases in co-flow or preferably countercurrent. The inlet temperature of the drying air is 120 - 300 ° C, preferably 150 - 250 ° C, and the outlet temperature is generally 75 - 95 ° C.

Particularly suitable have been found salt compositions whose content of sodium silicate is 3 - 75% by weight, especially 5-15% by weight based on anhydrous salt. Such salt mixtures provide a particularly abrasion-resistant and at the same time well-soluble grained carrier substance. Preferably, the sodium silicate used in the aforementioned weight ratio 20 has a 1: 1 ratio.

A further improvement of the grain structure is obtained if a salt mixture is used which, in addition to the aforementioned sodium silicate, also contains sodium tripolyphosphate and sodium sulfate in a weight ratio of 10: 1 to 1:10, especially 25: 5: 1 to 1: 5, based on anhydrous tripolyphosphate and water free sodium sulfate. The sodium tripolyphosphate is hereby preferably used as hexahydrate irrespective of the calculation ratio stated.

Therefore, the carrier preferably has the following composition 30 (calculated as anhydrous salt): 4

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5-15 wt% Na 2 O: SiO 2 = 1: 2 15 - 65 wt% Na 2 P ^ O ^ 65 - 15 wt% Na 2 SO 4 5-20 wt% water 5 Carriers with high tripolyphosphate content have a higher water content (10 - 20% ) and those with a high sodium sulfate lower water content (5 - 8%). When mixing ratio poly = phosphate: sulfate in the range 2: 1 to 1: 2, the water content is approx.

8 - 12%. ......

Further, in a particularly preferred mode of operation, the aqueous slurry based on anhydrous salts can be mixed with up to 0.3% by weight, preferably 0.05 to 0.2% by weight, of the polysiloxane and silicic acid mixture. This component added before the spray-drying, as previously stated, loses some of its antifoaming effect, but this loss can be taken into account, as it relates only to a small percentage of the total polysiloxane antifoam used. This addition, on the other hand, significantly improves the spray-drying performance of the concentrates, the grain structure of the carrier grains as far as better absorbency of poly-siloxanes is concerned, and in particular the wettability of the powder components loaded with additional poly-siloxane antifoam for later use. washing bath. On the contrary, if the total amount of polysiloxane silicic acid mixture is incorporated into the concentrate and spray dried together as proposed in the prior art, the wettability in the wash bath is degraded and residual formation can occur due to undissolved particles. In addition, the overall antifoaming effect is reduced.

The carrier must be surfactant free as surfactants also attenuate the antifoaming effect. In addition, it must be free of water-insoluble or heavily-soluble compounds such as the clays, silica-guhr, full-soil and cellulose recommended in the literature, as these substances also

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5 leads to a loss of effect, which may be due to the partial separation of the polysiloxane from the silicic acid.

The carrier prepared in the manner indicated has a grainy nature and has a grain spectrum of 0.05 to 2.5 mm, preferably 0.1 to 1.6 mm, with a mean grain size of 0.2 to 0.8 mm. It is characterized by a good absorption capacity of the polysiloxane silicic acid component on the one hand and a fast and complete dissolution in the wash bath, even at low wash temperatures.

In order to prepare the antifoam powder components, the granular carrier is mixed with conventional poly (siloxane-silicic acid mixtures), the weight ratio of carrier (calculated as anhydrous salt) to polysiloxane-silicic acid mixture being 50: 1 to 6: 1, preferably 25: 1 to 15. 8: 1. Suitable compounds such as dimethyl, diethyl, dipropyl, dibutyl, methylethyl, methylphenyl, methylcyclohexyl and hydroxyalkyl polysiloxanes are suitable as polysiloxanes. Furthermore, cross-linked polysiloxanes (so-called silicone resins) are suitable. The polysiloxanes are used in admixture 20 with finely divided silicic acid, for example aerosil, with silane silicic acid available as well. by reacting hydroxy.l group-containing silicic acid with chlorosilanes. The weight ratio of polysiloxane to silicic acid is 50: 1 to 5: 1, preferably 25: 1 to 7: 1.

The mixing of the granular support with the polysiloxane-silicic acid mixture can take place in conventional mixers, with both a discontinuous and a continuous operation being possible. Suitable for example are drum mixers, spray mixers, cascade mixers or mixers consisting of a vertical drop pipe with an axially arranged rotating shaft equipped with mixing tools (so-called Schugi mixers).

The spray-dried carrier material is thus provided that 6

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independently. The pore structure of the support grain leads to an optimal distribution state of the foam damper. This optimum is expressed by the following properties: 1. The pore structure is such that upon absorption no separation of the polysiloxane from the silicic acid occurs.

Such separation, which can be observed, for example, by the use of other carriers (for example, clay, silica-guhr) leads to extensive loss of effect.

2. The grain is free flowing and does not grease / i.v.s. that the poly = 10 siloxane does not creep over to other powder components and does not break through a cardboard package.

3. The polysiloxane-absorbed polysiloxane is widely protected against interactions with other detergent components, especially alkalis and surfactants. Even without additional enveloping layers to be applied with similar hassle, no effect loss ·· on the storage.

4. The polysiloxane silica treated grain is well wettable and easily soluble. Therefore, no problems occur with the injection of the powder into washing machines.

20 Remaining formation on the laundry due to undissolved particles is avoided.

5. When dissolved in the wash liquor, a favorable distribution state is formed of the polysiloxane antifoam, which is such that, on the one hand, effective foaming dampening is already obtained in low quantities and on the other hand no coatings which promote the graying of the laundry and grease rubber components in washing machines.

The carrier loaded with polysiloxane-silica mixture (hereinafter called powder component A) has a weight load of 30 450 to 700, preferably 500 to 650 g / kg. liter. It is therefore of the same order of magnitude as the weight of 7

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cannot be intermixed during transport and storage.

The powder component A is mixed in a manner known per se with other powdery to granular detergent components, the amount ratios being measured so that, depending on the strength of the desired effect, 0.01 to 0.5, preferably 0.05 to 0.2 weight, is found. % polysiloxane silica mixture in the detergent.

The detergent component containing surfactants and builder salts (hereinafter called powder component B) should have a grain size of 0.05 to 2.5 mm, preferably 0.1 to 1.6 mm. It contains at least one anionic, nonionic or zwitterionic surfactant, builder salts and other non-bleaching detergent constituents, including detergent alkali, graying inhibitors, optical brighteners, stabilizers, neutral salts and dyes, but not per-compounds or bleaches containing active chlorine , bleach activators and enzymes that are not durable under the conditions of hot spray drying.

Anionic surfactants suitable for the preparation of component B 20 are those of the sulfonate or sulfate type, in particular alkyl benzene sulfonates, olefin sulfonates, alkyl sulfonates and α-sulfo fatty acid esters, primary alkyl sulfates, and the sulfates of ethoxylated higher alcohols containing 2-3 glycol ether groups. In addition, alkaline soaps of fatty acids of natural or synthetic origin may be used, for example, the sodium soaps of coconut fatty acid, palm kernel fatty acid or tallow fatty acid. The anionic surfactants are preferably in the form of sodium salts. Provided that said anionic and zwitterionic compounds have an aliphatic hydrocarbon residue, it should preferably be straight chain and have 8-22, preferably 12-18 carbon atoms. In the compounds of an araliphatic hydrocarbon, they preferably contain unbranched alkyl chains 6-16, especially 10-14, carbon atoms.

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Suitable nonionic surfactants are especially ethoxylation products of saturated or single unsaturated aliphatic primary alcohols having 12-24, preferably 12-18, carbon atoms and 3-20, especially 4-15, ethylene glycol ether groups. Suitable alcohols from which the present ethoxylation products are derived are, for example, those of natural origin such as coconut or tallow fatty alcohols and oleyl alcohol, respectively; furthermore oxo = alcohols or synthesis alcohols obtained by ethylene polymerization. ....

Other suitable nonionic surfactants are ethoxylation products of secondary alcohols, vicinal diols and amino alcohols having each 12-18 carbon atoms as well as of alkyl phenols having 6-12 carbon atoms in the alkyl residue, the number of glycol ether groups being also 3-20, preferably 4-15 15. The aforementioned ethoxylated alcohols, amino alcohols and alkyl phenols may also be wholly or partially replaced by those whose preparation contains 0.5 to 3 moles of propylene oxide per liter. mole of starting compound and only in the second step is the intended amount of ethylene = 20 oxide.

Optionally, such nonionic surfactants may also be present which are derived from the aforementioned compounds and which have ethylene glycol and propylene glycol ether groups in second order, for example alcohols having 10-30 ethylene glycol = 25 ether groups and 3-30 propylene glycol ether groups; than ethoxylation products of mercaptans, fatty acid amides and fatty acids. Also useful are the water-soluble polyethylene oxide adducts for polypropylene glycol containing 20 - 250 ethylene glycol ether groups and 10 - 100 propylene glycol ether groups, ethylenediaminopolypropylene glycol and alkyl polypropylene glycol having 1-10 carbon atoms in the alkyl chain. The said compounds usually contain per. propylene glycol unit 1-5 ethylene glycol units. Also non-ionic compounds of the type of amine oxides and sulfoxides, which may also be ethoxylated, are useful.

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Suitable builder substances are polymeric phosphates, carbonates, silicates and sulphates of potassium and especially of sodium, the silicates having a ratio of SiO 2 to Na 2 O of 1: 1 to 3.5: 1. In particular, polymeric phosphate may be pentane sodium = 5 umphosphate, which may be in admixture with its hydro lysis products, the mono- and diphosphates, as well as higher condensed phosphates, for example the tetraphosphates. Also useful are cation exchange suitable aqueous alumosilicates of potassium or especially of sodium of the general formula (Na 2 O) x, Al 2 O 3, (SiO 2) y, (H 2 O) z, where x = 0.9 to 1.5, y = 1.3 to 4.0, and z = 1 to 6.

These aluminosilicates generally have a grain size of 0.1 to 20 µm and are preferably crystalline.

Furthermore, the builder salts include salts of complexed aminopolycarboxylic acids, especially alkali salts of nitrilotriacetic acid and ethylenediaminotetraacetic acid. Also suitable are the higher homologues of said aminopolycarboxylic acids. Also salts of nitrogen-free polycarboxylic acids which form complex salts with calcium ions, which also include carboxyl group-containing polymerisates, are suitable. Examples are citric acid, tartaric acid, benzene hexacarboxylic acid and tetrahydrofuran = tetracarboxylic acid. Also polycarboxylic acids containing carboxymethyl ether groups are useful such as 2,2'-oxydiracetic acid and with glycolic acid partially or completely etherified polyhydric alcohols or hydroxycarboxylic acids, for example tris-carboxymethylglycerine, biscarboxymethyl glyceric acid, carboxymethyl-oxyacetic acid or carboxylic acid or carboxylic acid and carboxylic acid Furthermore, the polymeric carboxylic acids having a molecular weight of at least 350 in the form of water-soluble sodium or potassium salts such as polyacrylic acid, polymethacrylic acid, poly-α-hydroxyacrylic acid, polymaleic acid, polyitaconic acid, polymesaconic acid, polybutene = tricarboxylic acid, and copolymeric acids of the corresponding or with ethylenically unsaturated compounds such as ethylene, propylene, isobutylene, vinyl methyl ether or furan.

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Furthermore, complexing polyphosphonic acid salts may be present, for example, the alkali salts of aminopolyphosphonic acids, especially aminotri (methylphosphonic acid), 1-hydroxyethane-1,1-diphosphonic acid, phenylhydroxymethane diphosphonic acid, methylene diphosphonic acid, and salts of the higher homologous acids. Mixtures of the aforementioned complexing agents are also useful.

The other constituents which may be contained in component B include washing alkalis, neutral salts, gray inhibitors, optical brighteners, stabilizers such as magnesium silicate, antifouling agents and dyes; in addition, additives which improve the spray-drying ability, for example, alkali salts of toluene, xylol or cumol sulfonic acid.

Suitable washing alkalis are alkali carbonates, bicarbonates, borates and silicates having a Na 2 O: SiO 2 ratio of 1: 1 to 1: 3.5. As neutral salts, there may be sodium sulfate and sodium chloride.

As a graying inhibitor, carboxymethyl cellulose 20 as well as cellulose blend ethers containing alternating amounts of carboxymethyl, methyl and / or hydroxyethyl, hydroxypropyl and hydroxybutyl groups, in particular methylhydroxy propylcellulose and methylhydroxybutylcellulose, are particularly suitable; further, polymers that are colloidal soluble in water respectively 25 copolymers of vinyl alcohol, vinylpyrrolidone, acrylamide and acrylonitrile.

Suitable optical clarifiers are alkali salts of 4,4-bis (-2 "-anilino-4" -morpholino-1,3,5-triazinyl-6 "-amino) -style-2,2'-disulfonic acid or compounds built up in a similar manner which, instead of the morpholino group, carries a diethanolamine group, a methylamino group or a 3-methoxy-oxyethylamino group, moreover, as diaryl = 11 type diuretics can be used.

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chlorophenyl) -Δ-pyrazoline and compounds similarly constructed which carry the carboxymethyl or acetylamino group instead of the sulfonamido group. Also useful are substituted amino coumarins, for example 4-methyl-7-dimethylamino or 4-methyl-7-diethylaminocoumarin.

Further, as polyamide clarifiers, the compounds 1- (2-benzimidazolyl) -2- (1-hydroxyethyl-2-benzimide = azolyl) -ethylene and 1-ethyl ~ 3-phenyl-7-diethylamino-carbostyryl can be used. As the clarifying agent for polyester taverns and polyamide taverns, the compounds are suitable 2,5-di- (2-benzoxazolyl) -thio = phen, 2- (2-benzoxazolyl) -naphtho- [2,3-b] -thiophene and 1 , 2-di (5-methyl-2-benzoxazolyl) ethylene. Furthermore, substituents of the type of substituted diphenyl styrenes may be present. Mixtures of the aforementioned clarifiers 15 may also be used.

Preferably, any additional powder component (C) present contains a per-compound, for example, sodium percarbonate, but especially sodium perborate tetrahydrate.

Furthermore, additional powder components may be present, which may contain, for example, enzymes or bleach activators. For protection against decomposition or interactions with the other powder constituents of the detergent, the enzymes and bleach activators may be coated with water-soluble or dispersible wrap substances. The powder component .B is preferably prepared by spray drying in a known manner by an aqueous slurry. Such spray powders usually have a liter weight of 300 to 600 g and, after mixing with the component A prepared by spray drying, are not prone to mixing during filling and transport. Optionally, component B may also be prepared by known granulation.

The compound of the various powder components occurs at 12

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work continuously or according to the principle of the free faid.

Before or during the mixing process, additional ingredients, for example fragrances, may also be introduced into one of the powder components or powder mixture. Finally, one of the powder components B or C, but in particular the sodium = perborate (component C), as described in patent applications DE-OSS 27 48 970 and 27 53 680, may also be treated with nonionic surfactants to improve the rinsing conditions of the washing powder. .

The powdered detergents prepared in the manner indicated are characterized by a favorable foam ratio. It is an advantage that the antifoaming effect of the siloxanes in the process of the invention or during storage does not suffer any appreciable damage, but that, on the other hand, by the means, no graying of the fabrics or any loading of the washing machine parts by a only difficult removable siloxane film.

Therefore, the detergents prepared according to the process described can have the following composition: 20 A) 1 part by weight of a granular powder component containing 1-15% by weight of a mixture of polysiloxane and finely divided silica in a ratio of 50: 1 to 6: 1 which is adsorbed on a spray-dried product containing 25% to 15% by weight of sodium silicate of the composition

Na 2 O: SiO 2 = 1: 1.5 to 1: 3, especially 1: 2, 30-80 wt% pentane sodium tripolyphosphate and / or sodium sulfate and / or sodium carbonate, 5-20 wt% water (including crystal water),

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13 B) 5 to 80 parts by weight of a granular powder component containing 10 to 40% by weight of at least one anionic, nonionic or zwitterionic surfactant, 5 to 40% to 80% by weight of at least one builder salt, 10 to 50% by weight of other non-bleaching detergent stocks parts, C) 0 to 30 parts by weight of a granular powder component containing, an oxidative-acting bleach, 10 wherein the mixing ratio of the individual powder components is metered such that the agent contains a total of 0.01 to 0.5% by weight of polysiloxane.

EXAMPLES

To prepare the carrier, slurries containing 35% by weight water of the salt mixtures listed in Table 1 were spray dried (indications by weight% anhydrous salt). The spray drying was carried out in a spray tower equipped with three spray nozzles, in which the drying air heated to 240 ° C was fed countercurrently. The 20 grain size distribution of the spray-dried products determined by sieve analysis is also given in Table 1.

Very favorable grain spectra exhibit the products of Examples 4, 5 and in particular 6. Grain components over 1.6 mm in diameter were sieved prior to further processing.

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TABLE 1

Ingredients __ Example __ (% by weight) 123 4 5 6

Na5P3 ° 10 70.0 "40/0 31/4 33.0 33 '°

Na 2 SO 4 - 83.0 35.0 47.8 45.0 44.8

Na20.2 SiO2 10.2 12.0 13.0 10.4 11.0 11.0 H2 O 13.8 5.0 12.0 10.4 11.0 11.0

Polysiloxane - - - - - 0.2

Grain size (parts by weight%)> 1.6 mm 2.0 0.1 0.1 0.1 0.2 0.1> 0.8 mm 2.4 0.2 0.2 0.2 0.4 0.1> 0.4 mm 26.5 7.1 6.5 5.6 5.8 5.9> 0.2 mm 64.7 60.8 66.9 72.3 68.4 73.7> 0.1 mm 4.0 28.6 24.3 20.0 23.2 19.2 <0.1 mm 0.4 3.2 2.0 1.8 2.0 1.0

The spray-dried products (temperature 20 ° C) in a drum mixer were incrementally mixed with a homogeneous mixture of 6 parts by weight of polydimethylsiloxane and 1 part by weight of silanized silicic acid heated to 50 ° C. The viscosity of the polysiloxane silicic acid mixture was 1,300 cP at 20 ° C and 750 cP at 50 ° C. In Examples 1, 2, 4 and 5, 5 parts by weight of polysiloxane-silica were used for 95 parts by weight of carrier. In Example 3, this ratio was 10:90 and in Example 6 (0.2% by weight polysiloxane-containing spray-dried product) was 4.8 to 95.2 parts by weight.

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The spray-dried products (temperature 20 ° C) in a drum mixer were incrementally mixed with a homogeneous mixture of 6 parts by weight of polydimethylsiloxane and 1 part by weight of silanized silicic acid heated to 50 ° C. The viscosity of the polysiloxane-silica mixture was 1,300 cP at 20 ° C and 750 cP at 50 ° C. In Examples 1, 2, 4 and 5, 5 parts by weight of polysiloxane silicic acid mixture were used for 95 parts by weight of carrier, in Example 3 this ratio was 10-90 and in Example 6 (0.2% by weight poly = siloxane-containing spray-dried product) 95.2 parts by weight.

After a total mixing time of 5 minutes, the polysiloxane-silica mixture was completely absorbed by the carrier. The impregnated granule was found to be dry, rice-resistant, non-sticky and non-greasy. The liter weight of the granulate was between 560 and 590 g / l.

The composition of the spray-dried detergent (component B) was (by weight%): 10.0 n-dodecylbenzene sulfonate 4.2 soap (talc coconut = 9: 1)

2.0 tallow alcohol + 5 EO

1.9 tallow alcohol +14 EO

50.0 tripolyphosphate 3.0 sodium silicate (Na 2 O: SiO 2 = 1: 3)

2.1 magnesium silicate 0.3 EDTA

0.9 Carboxymethyl Cellulose 0.3 Optical Clarifier 17.1 Sodium Sulfate Residual Water

The powder components A and B were mixed with the addition of 30 sodium perborate tetrahydrate (component C) in the mixing conditions listed in Table 2. The foam conditions were tested after 10 days of storage of the mixture in a commercially available horizontal drum washer at temperatures of 30, 60 and 95 ° C. For this purpose, the machine was filled with 16

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was 7.5 g and the water hardness was 16 ° dH. The foam height was checked in each case through the front sight glass and assessed as follows:

No foam = 0 5 1/4 of the sight glass height = 1 1/2 of the sight glass height = 2 3/4 of the sight glass height = 3 4/4 of the sight glass height = 4 Overcast = 5 10 The results are summarized in Table 2.

TABLE 2

Components Siloxane Foam height

Ex. A,% B, S C, S% 30 ° C 60 C 95 ° C

1 2.0 A ± 75 23 0.1 0.5 0.5 2.0 15 2 2.0 A2 75 23 0.1 0.0 0.5 1.5 3 0.5 A3 75.5 23 0 , 05 1.0 1.5 2.5 4 2.0 A4 75 23 0.1 0.0 0.5 1.0 5 2.0 A5 75 23 0.1 0.0 0.5 1.0 6 2.0 A6 75 23 0.1 0.0 0.5 1.5 20 Comparative Experiment 5 weight polydimethylsiloxane was mixed in the manner described in DE-OS 23 38 468, Example 1 with 5 weight silicic acid and 40 weight ethoxylated tallow alcohol (25 E0) at 50 ° C and sprayed onto a fluidized bed of 50 weight sodium sulfate.

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Comparative Experiment V2

Comparative Experiment V1 was repeated with the change that instead of sodium sulfate, a crystalline powdered sodium aluminum silicate of the composition 0.9 ^ 20, A ^ O ^ / 2 S1O2, 3 1 15 µ.

The dissolution ratio of the siloxane-containing powder component was carried out as follows: 3 In a beaker (500 cm volume), 200 ml of a 1 to 22 ° C tempered solution of 1 g sodium dodecylbenzene sulfonate in 1 liter of water is stirred by means of a motor stirrer. is equipped with 4 at an angle of 30 ° downwardly bent blade with a constant speed of 700 rpm. minute. The blades distance from the bottom of the container is 2.5 cm. 1 g of the sample is gently shaken while avoiding lump formation in the resulting stirring cone. After 90 seconds, the solution is poured through a tarred sieve with a mesh width of 0.1 mm and a diameter of 7 cm and aspirated by means of a suction bottle. Substances left in the beaker are transferred to the sieve by means of at least 20 injected water. After a drying time of 24 hours in the air, the screen is weighed back. Results of 10 trials are obtained.

The residual amounts were (by weight% of the material used):

Example 1 6.62%

Example 2 4.25% Example 3 3.31%

Example 4 3.90%

Example 5 3.75%

Example 6 1.01%

Comparative Experiment V · 22.1% 30 Comparative Experiment V2 48.8%

Claims (8)

A process for preparing a foam-dampened detergent consisting of several powdery to granular components, wherein one of the powder components consists of a polysiloxane antifoam adsorbed on a carrier and wherein the other 15 powder components consist of spray-dried and granular detergents, respectively, of conventional composition and , characterized in that a dry slurry containing 40-75% by weight (calculated as anhydrous compound) of at least one compound of the class of polymer phosphates, silicates, carbonates and sulphates is spray-dried to produce the powder component containing the poly = siloxane foam damper of sodium which slurry is free of surfactants and contains no more than 0.3% by weight (calculated on anhydrous salt) of polysiloxane antifoam 25 o using 120-300 C hot gases in a manner known per se and thus processes it obtained granular spray product containing 80-96 wt.% anhydrous salts with 3-10 wt.% (based on anhydrous salt) polysiloxane antifoam, which consists of a liquid mixture of polysiloxane and finely divided silica in a weight ratio of 50: 1 to 5: 1, then mixing the resulting granular adsorbate in a manner known per se with the other powder components in such weight ratios that the content of the detergent silica-containing polysiloxane antifoam is 0.01 - 0.5% by weight. DK 154828 B Process according to claim 1, characterized in that a slurry containing 50-70% by weight of anhydrous salts is spray dried, which slurry contains at least two compounds of the class tripolyphosphates, silicates, carbonates and sulfates in the form of sodium salts. Process according to claims 1 and 2, characterized in that a silicate having a ratio of Na 2 O: SiO 2 = 1: 1.5 to 1: 3, preferably 1: 2, 10 is used. Process according to claims 1-3, characterized in that a salt mixture is used, of which 3-75 wt.%, Preferably 7-12 wt.%, Consists of sodium silicate. Process according to claims 1-4, characterized in that a salt mixture is used which, in addition to sodium = silicate, also contains sodium tripolyphosphate and sodium sulfate in a weight ratio of 10: 1 to 1:10, preferably 5: 1 to 1: 5. 20 Process according to claims 1-5, characterized in that a slurry is dried in a slurry in which the sodium tri = polyphosphate is essentially present as hexahydrate. Process according to claims 1-6, characterized in that 0.05 - 0.2% by weight of polysiloxane foam damper, based on anhydrous salt, is added to the aqueous slurry. Process according to claims 1-7, characterized in that the spray drying is carried out in a spray tower using hot gases with an inlet temperature of 150 - 250 ° C and an outlet temperature of 75 - 95 ° C. 35