JPH06509128A - Detergent active formulation exhibiting delayed dissolution behavior and method for producing the same - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] A detersive active preparation exhibiting delayed dissolution behavior and its manufacturing method Process for treating existing detergent-active solid formulations with liquid reactive polynoloxanes and It relates to formulations exhibiting delayed dissolution behavior obtained by this method.

In the present invention, cleaning active formulations generally include laundry formulations, dishwashing formulations and creams. surfactant-containing precursor products or compounds thereof. It is understood that Products of this type especially contain relatively large amounts of nonionic surfactants. If water is added, a gel-like phase may form on the surface during the dissolution or dispersion process. The powder particles tend to stick to each other. some kind of house with special design Under undesirable conditions, such as those occurring in garden washers, bulk High residue deposits may form and therefore the product cannot be used for the desired application. do not have. As will be explained later, the problem to be solved by the present invention is to use detergent for household laundry. Under the conditions in which the detergent powder is fed into the machine, the water flow separates individual grains of detergent powder faster than clumps form. Cleaning formulations by special treatment of particle surfaces so that particles are separated from each other The goal is to retard the dissolution or decomposition of

Many proposals for improving the dispensing behavior of detergents are described in the patent literature. for example, German patent no. Detergent precursor products or detergent ingredients are listed. Described in this patent document In the method, for example, in a cation exchanger (builder) consisting of zeolite NaA, Polycarboxylic acids and nonionic surfactants are used with specified soaps to Average particle size and bulk density are defined within certain ranges. Furthermore, the nonionic interface Mixing the activator with a water-soluble or substantially water-soluble compound having a water-repellent group is proposed. Water-repellent compounds of this type include, for example, tallow fatty acid partial glycerin is a mixture of tallow fatty acid amide and hydroxyethylethylenediamide. .

It is not possible to produce detergents with good distribution (feeding) behavior according to the teachings of the above patents. However, the obvious drawback is that the teachings described are prescription specific. Ru. Therefore, other formulations of detersive active preparations that are desirable for other reasons may be significantly influenced by the composition of the formulation. cannot be improved by post-processing without adverse effects.

The same applies to the improved version described in German Published Patent No. 3822479. This also applies to detergent additives that exhibit distributional behavior. This patent document describes granular porous a water-soluble or water-dispersible carrier material and a water-soluble or water-dispersible carrier material adsorbed on the carrier material. Associated with granular detergent additives consisting of dispersible nonionic surfactants, which are Nonionic surfactants exist as a homogeneous mixture with hydrophobic substances that have polar groups. However, the weight ratio of the nonionic surfactant to the hydrophobic substance is 99.1 to 6040. There is. The hydrophobic substance is preferably a CU-U fatty acid.

[Baysilon-01] Bayer entitled MH15J Bayer AG's manual states that all substituents R in the formula shown below are methyl. polymethylhydrodienesiloxane group, X is hydrogen, and n is about 40 Sun is listed. Regarding the possible uses of such compounds, Bisilon E. MH15 can be used to prevent agglomeration and improve flowability of particulate inorganic materials. It is stated that it can be done. This refers to the flowability and agglomeration of the powder.

The instructions contain water-swelling cleaning active preparations with delayed dissolution of correspondingly treated substances. There is no mention of agglomeration.

Against this background of prior art, the problem that the present invention seeks to solve is that when adding water, Post-treatments that reduce the tendency of powder to agglomerate, almost regardless of its composition, The aim is to modify powder or granular detergent active preparations.

Another problem that the present invention seeks to solve is to provide improved dispensing properties in washing machines. The objective is to provide detergents that Yet another problem to be solved by the present invention is that It is an object of the present invention to provide a detergent precursor product that can produce such detergents.

The particular problem that the present invention aims to address is that the weight per volume is large and the improved An object of the present invention is to provide a detergent that exhibits a unique distribution behavior, and a method for producing the same.

That is, the present invention provides for the production of powdered or granular detergent active formulations that exhibit delayed dissolution behavior. A method of creating The preformed powder or granules are mixed with a liquid polysiloxane that is reactive with acidic hydrogen. sun component, At a temperature of 10-120°C, In the presence of a catalyst if necessary, Adjust the weight ratio of detergent active agent to polysiloxane component to 25 = 1 to 2000 21 It relates to a manufacturing method characterized by mixing, contacting, and reacting.

The manufacturing method of the present invention can be implemented relatively easily. Starting materials have dissolution behavior Certain cleaning active preparations that should be delayed, i.e. detergents, detergent precursors, dishwashing detergents or is a detergent or other solid surfactant formulation present in powder or granular form. Ru.

The detergent active formulation is contacted with the polysiloxane component at a temperature in the range of 10 to 120°C. Ru. Allows the polysiloxane component to react quickly and when the material is not affected by heat. higher temperature can be selected. Polysiloxane components and cleaning active formulations The reaction with is preferably carried out while mixing. Mixing the detergent active formulation with the polysiloxane component The mixing ratio ranges from 251 to 2000:1.

Polysiloxane components suitable for the process of the present invention have reactive groups and are compatible with the following general formula: The corresponding polysiloxane is: ■ In the above general formula, R is an alkyl group containing 1 to 4 carbon atoms, X is an alkyl group R1 water base, chlorine, alkyl-substituted amine group or hydroxyalkyl group Alkyl substituents contain 1 to 4 carbon atoms. ), and the number of substituents X per molecule is At least one is not an alkyl group. Polysiloxane used in the present invention The chain length of the components is defined by n, which is a number from 1 to 50, and is the same or different alkyl It may have a group.

Preferred substances for the production method of the present invention are those in which the substituent R is a methyl group and the substituent X is a methyl group. either hydrogen or methyl groups, on average at least one per molecule is a compound in which X is hydrogen and not a methyl group. Such polymethyl Drodiene siloxanes are commercially available. The equivalent amount of 5t-H groups is gram polysiloxane Preference is given to between 2 and 20 mmol per xane.

In the production method of the present invention, the reaction between the polysiloxane component and the detergent active agent is promoted. Sometimes it is preferable. To do this, the temperature must be set to 120℃ within the above temperature range. The temperature can be increased or even higher. However, adding catalyst You may. Suitable catalysts are, for example, amino-sensitive silanes and polysiloxanes. It is used in an amount of 2 to 50% by weight based on the amount of water. Catalyst after addition of polysiloxane in a separate step or at the same time as the reactive siloxane, using a separate nozzle if necessary. It is best to add it through.

Although the process of the present invention can be carried out quickly and safely at relatively high temperatures, the siloxane at room temperature, more preferably the temperature at which the detergent active formulation is present at the end of the process. The addition is preferably carried out at a temperature in the range of 20 to 50°C, particularly preferably.

The manufacturing method of the present invention uses a powder or granular detergent having a bulk density of 400 to 1000 g/I. It has a particularly remarkable effect in the case of pharmaceutical preparations. Therefore, one preferred method of the present invention is In embodiments, a detersive active formulation having this bulk density range is used as a starting material.

Suitable starting materials are, for example, detergents produced by spray drying and subsequent compression. Precursor, or its mixing with other detergent ingredients that cannot be spray dried to produce a detergent It is a thing. Such high densities are particularly suitable as starting materials for use in the process of the invention. The preparation of detersive active formulations is described in the patent literature.

That is, the product manufactured by the method of German patent application No. 3803966 is The method provides a particularly favorable improvement in its distribution behavior. This kind of product is less Spray-dried powder with a bulk density of 350 g/l is placed horizontally or slightly Produced by continuous feeding into a cylindrical mixing drum with a sloped and smooth inner wall. will be built. This mixing drum has an intermediate shaft with a length of 80 to 98% of the inner diameter of the drum. A shaft with radially arranged beating tools having a diameter (measured from The rotational speed of the shaft is set so that the powder stays in the drum. It is adjusted so that the time is 10 to 60 seconds and the output is constant, and the Froude number is 5. It ranges from 0 to 1200.

Particularly preferred preformed detersive active formulations as starting materials in the process of the invention are This is a product manufactured by the method described in International Patent Publication WO91/2047. this The seed product is a detergent or detergent precursor product, optionally in the presence of a plasticizer, Strand the homogeneous premix from a die with holes of 0.5 to 5 cm. Extrusion, the size of the extrudate is reduced by a cutting device, and then processed by a spheroidizing machine It can also be prepared in a mixture with other detergent ingredients in the method of the invention. It can also be used as

Furthermore, the production method of the present invention is carried out by the method described in German Patent Publication No. 3812530. Particularly good results are given when using the manufactured cleaning active formulations. this kind of The formulation is 4 to 30% by weight of at least one anionic surfactant, at least one nonionic surfactant, and at least one nonionic surfactant. 2-20% by weight of surfactant, 20-50% by weight of at least one builder, Rinse alkali 3-25% by weight, Contains up to 30% by weight of other spray-drying detergent ingredients, more preferably 3-25% by weight. , the spray-dried product is a spray-dried powder having a bulk density of at least 350 g/l. A cylindrical mixing drum with a smooth inner wall placed horizontally or slightly inclined Manufactured by a method of continuously supplying. This mixing drum has the inner diameter of the drum a radially arranged beating tool having a length of 80 to 98% of (measured from the intermediate shaft) a shaft is mounted for rotation, and the rotational speed of the shaft is The residence time of the powder in the drum is 10 to 60 seconds, and the output is constant. The Froude number ranges from 50 to 1200. at least half and not more than 5% (of the formulation) of anionic surfactant in the spray-dried powder. The remaining nonionic surfactant is introduced into the mixer in liquid form.

The method of the invention has a high bulk density as described in U.S. Pat. No. 4,639,326. It is particularly advantageous and suitable for improving the distribution behavior of detergent active formulations. this usa The patent involves spray-drying a carrier powder that already contains a portion of a nonionic surfactant; Add nonionic surfactant on top until half of the weight of nonionic surfactant is consumed. spray and then add the remaining nonionic surfactant granulated together with the carrier, The resulting mixture is then added to a base powder that is substantially free of sodium sulfate. with a nonionic surfactant content of 5-15% and 600 g/ It relates to a powdered detergent having a bulk density of 1 or more.

One advantage of the process of the invention is that the process can only be applied to the final cleaning active formulation. If the detergent is made up of different types of powders and the dissolution behavior of only one of them is not altered, It can be applied selectively to various powder components when necessary. .

The manufacturing method of the present invention can be applied to the surface of the polysiloxane component or the component of the detergent active preparation. Strictly speaking, it is the polysiloxane component that has reacted with the formulation components on the externally accessible surface area. A powdered or granular detersive active preparation is provided containing the reaction product of 10 minutes.

The macrodissolution or minute content of virtually any powdered or granular detergent active preparation The present invention also improves dispersion behavior by retarding the solubility of individual particles. The method can be used to improve laundry detergents, dishwashing detergents or other surfactant-containing formulations. However, a preferred embodiment of the present invention is produced by the production method of the present invention.

anionic surfactant 5-30% by weight, 1 to 15% by weight of nonionic surfactant, Builder 10-65% by weight, Alkaline component up to 35% by weight, more preferably 5-30% by weight, cobuilder 5 weight % by weight, more preferably from 0.5 to 4% by weight, more preferably up to 40% by weight bleach. preferably from 6 to 30% by weight, up to 15% by weight bleach activator, more preferably from 1 to 8% by weight. %, up to 25% by weight of alkali silicates, especially sodium silicates, more preferably 2 ~18% by weight, Select from foam inhibitors, foaming agents, fabric softeners, anti-redeposition agents, optical brighteners, dyes, and fillers. 0.1-10% by weight of at least one selected component, and 1-20% by weight of water. A granulated solid detergent containing a polysiloxane component and/or a granulated solid detergent. Or, the reaction product between it and a detergent component is added in an amount of 25 to 2000 parts by weight of the granulated detergent. It is a detergent contained on the particle surface in an amount of 1 part by weight (based on polysiloxane component).

Particularly preferred are solid granulated detergents improved according to the invention having the following composition: Lukylbenzene sulfonate, fatty alcohol sulfate, fatty alcohol ester -tersulfate, α-olefin sulfonate and/or fatty acid alkyl anionic surfactants 5 to 28 selected from the group consisting of ester sulfates; weight%, Alkyl polyethylene glycol ether, nonylphenol polyethylene glycol selected from the group consisting of coal ethers and/or alkyl polyglycosides; nonionic surfactant 1 to 11% by weight, foam suppressor 0.1 to 3.5% by weight, Zeolite NaA 20-50% by weight, Up to 10% by weight of sodium carbonate, more preferably 1-8% by weight, polycarboxylic acid up to 10% by weight, more preferably 0.5-8% by weight, bleach 13-25% by weight, bleach activator 0.2-10% by weight, Up to 6% by weight of sodium silicate, more preferably 1 to 5% by weight, fabric softener, recycled Group consisting of anti-deposition agents, enzymes, optical brighteners, dyes, fragrances, formulation aids and fillers 1 to 3% by weight of one or more components selected from; 1-15% by weight of water.

According to the invention, starting from a detergent having a weight per volume of 400 to 1000 g/] Preferably, it is used as a substance. This kind of detergent is a compressed detergent or It may be a detergent manufactured from the beginning by a granulation method. In this case, the detergent is Preferably, it is produced by wet granulation and subsequent drying, especially fluid bed drying. compression washing It goes without saying that agents can also be improved by the present invention.

In the manufacturing method of the present invention, only surfactant-containing ingredients other than the final detergent itself are removed from polysiloxane. It can also be successfully employed when processing by component. For example, produced by spray drying The prepared detergent precursor can be used as is or after compaction. . Such precursor products produced by spraying methods are usually not affected by heat. Contains all detergent ingredients. Precursor products may therefore be e.g. bleach or It does not contain enzymes, but it does contain builders and surfactants.

Corresponding detergent precursor products have the following composition: 5 to 15 parts anionic surfactant. amount%, 1 to 10% by weight of nonionic surfactant, Soap 0.5-2% by weight, Up to 30% by weight of sodium carbonate, preferably 10-27% by weight, zeolite Na A20-50% by weight, Up to 10% by weight of polycarboxylic acid, preferably from 0.5 to 8% by weight, resistant to spray drying up to 10% by weight of other detergent ingredients, preferably from 0.1 to 5% by weight, The balance water (1-20% by weight).

The individual components of the above basic formulation will be explained below.

Anionic surfactants are generally surfactants of the sulfonate or sulfate type. It is a drug. Surfactants with sulfonate groups are preferred; Honate, α-sulfofatty acid ester salt and α-sulfofatty acid ester unit salt Particularly preferred. Anionic surfactants generally exist in the form of sodium salts.

Its proportion is 2 to 15% by weight, preferably 5 to 12% by weight, based on the total detergent. be.

Suitable nonionic surfactants are selected from alcohols and alkylphenols. 1 mole of a compound essentially having 10 to 20 carbon atoms and 2 to 20 moles of ethylene oxide , preferably 3 to 15 moles of adduct. Of particular importance is the 7-15 mole tyrene oxide and a primary alcohol such as coconut oil or tallow alcohol, Oleyl alcohol, oxo alcohol, carbon number 8-18, preferably 12-1 8 secondary alcohol, monoalkyl alcohol having 6 to 14 carbon atoms in the alkyl group or an adduct with dialkylphenol. These water-soluble nonionic surfactants in addition to 2 to 6 ethylene glycol ether residues in the molecule. Polyglycol ethers that are water-soluble or substantially water-insoluble are especially suitable for water-soluble nonions or or anionic surfactants. Other suitable nonions The surfactant has an alkyl group of 8 to 18, preferably 10 to 16 carbon atoms. These are alkyl glycosides and alkyl polyglycosides. Nonion in detergent The content of surfactants or mixtures thereof is preferably 3 to 10% by weight, more Preferably it is 3 to 7% by weight.

Besides carbon sodium, builders are generally zeolites, especially NaA type zeolites. and polycarboxylic acids. (measured according to German patent 2224837) , te) Microcrystalline synthetic hydrated N with calcium binding capacity of 100 to 200 mgCaO/g AA type zeolite is preferred. The particle size typically ranges from 1 to 10u It is in.

Suitable (co)polymeric polycarboxylic acid esters include polyacrylates, polymethacrylates, acrylic acid, especially copolymers of acrylic acid and maleic acid (preferably acrylic 50-90% by weight of acid and 50-10% by weight of maleic acid). homopolymer molecule The amount generally ranges from 1000 to 100,000, and the molecular weight of the copolymer is Generally in the range of 2000 to 200.000, preferably 50.000 to 120.000. It is surrounded by Particularly preferred acrylic acid/maleic acid copolymers are 50.000 to 1 It has a molecular weight of 0o, ooo.

Suitable but less preferred compounds of this class contain a small proportion of acid. At least 50% acrylic or methacrylic acid and a vinyl ether (e.g. , vinyl methyl ether). For example, U.S. Patent No. 414422 Also polyacetal carboxylic acids of the type described in No. 6 and No. 4146595 It is suitable for polymerization of glycolic acid, introduction of stable end groups, and produced by saponification to form um or potassium salts. Polymerization of acrolein and polymers obtained by Kanitzaro disproportionation of polymers with strong alkalis. Acids are also suitable. These are essentially acrylic acid units and vinyl alcohol or It consists of acrolein units.

A suitable alkali metal component is an alkali silicate, especially a Na02:SiOz composition ratio. sodium silicate in a ratio of 1:1 to 1:3.5, preferably 1:2 to 1:3.35. It is mu. Another suitable alkali metal component is sodium carbonate.

The detergents of the invention contain phosphonic acids, such as aminoalkane phosphoric acids, as co-builders. may contain phosphoric acid. A preferred aminoalkanephosphonic acid is ethylene diamide Tetramethylene phosphonate (EDTMP), diethylenetriamine penta methylene phosphonate (DTPMP), and higher homologs thereof. child They are preferably neutral reactive sodium salts, such as hexanatrium of EDTMP. It is used in the form of hebuta- and octa-sodium salts or DTPMP. wash Their content in the agent is preferably up to 1% by weight, more preferably up to 1% by weight in terms of free acid. Preferably it is 0.1 to 0.5% by weight. A suitable phosphonic acid is 1-hydroxy siethane-1,1-diphosphonic acid, and the disodium salt or tetra of this acid It is a sodium salt.

Furthermore, the detergent of the present invention preferably contains a bleaching agent. Acts as a bleaching agent in water Among the compounds that generate H2O2, sodium perborate tetrahydrate (NaBOz・ H2O2・3HzO) and -hydrate (NaBO2・HzOz) are particularly important. Ru. However, other H2O2-generating borates, such as Varborac 7, (Na2B 40t.4HtO2) is also suitable. These compounds may be completely or partially , other active oxygen carriers, especially peroxyhydrates, e.g. carbonate (Na2CO3・1゜5H202), peroxypyrophosphate, cylindrical Trate parts 1 Idrate, urea/) (202, or melamine/H□02 compounds, and persalts or peracids such as perbenzoates, peroxyphthalates , ciba-azelaic acid or dino-dodecanoic acid.

In order to increase the bleaching effect at washing temperatures below 80℃, especially from 40 to 60℃, bleaching activity is added. Sex agents may also be incorporated into the formulation. An example of a bleach activator is H2O2 and an organic peracid. N-acyl or O-acyl compounds formed, preferably N,N'-tetrayl Cetylated diamines, such as N,N,N',N'-tetraacylethylenediamine : carboxylic acid anhydrides such as benzoic anhydride and phthalic anhydride; and polyols. esters such as glucose pentaacetate.

Detergents are used as cotton optical brighteners, especially derivatives of diaminostilbendisulfonic acid. or an alkali metal salt thereof. Suitable optical brighteners of this type are e.g. For example, 4,4′-bis-(2-anilino-4-morpholino-1,3,5-tria Zin-6-ylamino)-stilbene-2,2°-nesulfonic acid salt or moiety ethanolamino group, methylamino group or 2-metho group instead of ruphorino group It is a compound with a similar structure that has a xyethylamino group. Suitable for polyamide fibers Optical brighteners are of the 1,3-diaryl-2-pyrazoline type, such as 1-(p -sulfamoylphenyl)-3-(p-chlorophenyl)-2-pyrazoline be.

Substituted 4.4′-bis-(4-chloro-3-sulfostyryl)-diphenyl type fluorophore Photobrighteners are also suitable. Mixtures of the optical brighteners mentioned above can also be used.

Suitable enzymes are proteases, lipases and amylases or mixtures thereof. selected from. Bacteria or fungi, such as Bacillus subtilis illus 5ubtilis), Bacillus licheniformis (liche Streptomyces griseus (S treptom) Enzyme preparations produced from P. yces griseus are particularly suitable. The enzyme is , adsorbed on carriers and/or encapsulated in shell-forming materials to Can be protected from decomposition.

Suitably the foam suppressor is an organopolysiloxane, even if silanized therewith. Good mixture with fine silica, paraffin, wax, microcrystalline wax, and this It is a mixture of these and silanized silica. Cl2-2゜fatty acid and C7-, diamide or from CI 2-2゜alkylamine and C2-6 dicarboxylic acid. Derivative bis-acylamides are also suitable. Mixtures of different foam suppressants, e.g. mixtures of silicone and paraffin or wax, and bis-anuramide; Mixtures with paraffin or wax can also be used advantageously. Foam suppressant is granulated water Preferably, it is immobilized on a soluble or water-dispersible carrier.

Suitable fabric softeners include bentonites and smectites, such as those described in German Patent No. 2 334899 and those described in European Patent 026529 It is a layered silicate. Other suitable fabric softeners include strips corresponding to the formula: M is a synthetic fine-grain layered silicate with a mectite-type crystalline phase and reduced swelling power. gO(M2O)-(AhOs)b(SiOz)c(HzO)-[wherein M is nat] Lithium, sometimes containing lithium, but with a small molar ratio of sodium to lithium Both are 2, a is 0.05-0.4, b is 0-0.3, C is 1.2-2, n is 0.　 3-3, (H2O)n represents bound water in the crystalline phase. ].

Other suitable fabric softeners are less than 0.6 when suspended in water (166 dH 1 room temperature) , preferably a swelling power of less than 0.4 Vs/V [pretreated with excess soda solution] , washed carefully and suspended in 9 parts by weight water/1 part by weight layered silicate for 20 hours. A synthetic layered silicate having a ratio of sedimentation volume (Vs)/total volume (V), and has a mixed crystal structure, with irregularly intercalated crystalline alkali metal polysilicate. Synthesis containing structures that determine a savonite-like and/or hectorite-like crystalline phase. It is a stratified silicate. Such layered silicates are described in German patent 35264 It is described in detail in 05. The content of layered silicate is, for example, 5 to 20% by weight % range.

Detergents can be made stable by conventional methods, e.g. spray drying conditions, by spray drying the ingredients and heating. By later adding sensitive ingredients such as bleach, enzymes, fragrances and suds suppressants, can be manufactured. Another suitable method consists of granulating the ingredients; In the case of granulation of water, salt solution, polymer solution and/or nonionic surfactant May be used as a liquid. Of particular importance is that despite the presence of zeolite, The content of potassium metal silicates can be increased from 2.5 to 3% by weight without the risk of increased ash formation. can increase particle strength and injectability of fine granular powder. This means that

Granular detergent D1 having the following composition was prepared and tested. 1st to 9th components and Mix the bulk of the sodium sulfate to obtain an aqueous slurry and transport it through a laboratory-scale tower. and spray dried. Perborate, bleach activator and granules into the spray dried product Mixed. All amounts are in weight percent.

7.0 Sodium dodecylbenzene sulfonate 1.5 Sodium tallow soap 6, 5 Crt-In fatty alcohol + 3-5 EO250 zeolite NaA 10.0 Sodium carbonate 2.5 Na silicate (Na20: 5iO2=1: 3.3) 0.8 cellulose ether 0.2 Fluorescent brightener 5.0 Phosphonate/copolymer/Na sulfonate mixture 25.0 Perborate Sodium acid tetrahydrate 2.0 Tetraacetylethylenediamine 05 Granular enzyme 0.2 Granular silicone foam inhibitor Remainder: Sodium sulfate, water The product obtained was compressed in the manner described in German patent 3812520. generation washing Agent D1 had a bulk density of 688 g/]. The following formula for 1g per 1kg of Dl Polymethylhydrodiene siloxane corresponding to The products are commercially available as Bisilon (registered trademark) to Ale MH15.

After introduction, the detergent was stored at room temperature for 5 days.

The distribution behavior simulates the conditions in the distribution chamber of a domestic washing machine operating at limit conditions. I rated it and decided. 100g of the product was placed in a test dispenser (Zanussi (Z dispensing torof) and after 1 minute drain 10 liters of tap water. The tuttle was poured over 90 seconds. Detergent remaining after flushing 10 liters The residue was reweighed wet and 30% of the weight was subtracted as water weight. below Scores were given for distribution behavior. Ratings A and B are very good or practically satisfactory. This is an acceptable level. A rating of C means poor distribution behavior.

A = fully distributed (the number is the number of liters of water required) B = less than 10g C = 10g or more of residue (the number is the number of grams of residue) The number of grams of residue. ) The distribution behavior of detergent D1 can be changed according to the invention from the original C20. It has been improved from A5 to A5.

Example 2 24% by weight surfactant (mixture of anionic and nonionic surfactants) ), 21% by weight zeolite NaA.

17.5% by weight sodium perborate-hydrate, 12.5% by weight sodium carbonate Um, 6% by weight of polycarpoxylate (Sokalano registered trademark) C F2), 4% by weight sodium sulfate, 7.5% water by weight; Foam suppressant, soap at 100% by weight Extruded detergent D2 (bulk) containing The distribution behavior with a density of 795 g/I) was determined by the application of 0.3% by weight of reactive polysiloxane. As in Example 1, it was improved from C26 to B2.

When 0.6% by weight of reactive polysiloxane was applied, the rating was AIO.

international search report Continuation of front page (72) Inventor Schulz, Rüdeiger Federal Republic of Germany Day-4019 Monheim, Fuichtestraasse No. 18

Claims (12)

[Claims] 1. A method for producing powdered or granular detergent active formulations that exhibit delayed dissolution behavior. hand, The preformed powder or granules are mixed with a liquid polysiloxane that is reactive with acidic hydrogen. sun component, At a temperature of 10-120°C, In the presence of a catalyst if necessary, The weight ratio of detergent active formulation to polysiloxane component is adjusted from 25:1 to 2000:1. A manufacturing method characterized by mixing, contacting, and reacting. 2. The polysiloxane component has the general formula: ▲There are mathematical formulas, chemical formulas, tables, etc.▼(I) [In the formula, R is a C1-4 alkyl group, represents hydrogen, chlorine, NR2 or OR, or an alkyl group R. However, 1 minute At least one of the substituents X per child is not an alkyl group. n is an integer from 1 to 50 It is. ] The manufacturing method according to claim 1, wherein the compound is a compound represented by: 3. Bulk density of 400-1000 g/l as powdered or granular detersive active formulation The manufacturing method according to claim 1 or 2, wherein a detergent having the following is used. 4. As a detergent active formulation, by spray drying and subsequent compression or as wet granules Detergent precursors or other detergents produced by oxidation and subsequent drying Claims 1 to 3 using ingredients, in particular mixtures with other detergent ingredients that cannot be spray-dried. 3. The manufacturing method according to any one of 3. 5. Optionally in the presence of a plasticizer, the duct preferably has pores of 0.5 to 5 mm in diameter. Extrude the homogeneous premix into strands from the chair and cut the extrudate to size. Detergents or detergents produced by compacting them using a device and then processing them using a spheronizer. It is a precursor product and can also be used as a mixture with other detergent ingredients if required. Claims 1 to 3 in which a detergent or detergent precursor product is used as a detergent active formulation. The manufacturing method described in any of the above. 6. X is hydrogen or a C1-4 alkyl group, and the equivalent amount of Si-H groups is 2 to 20 mmol of the compound of formula (I) per siloxane is added to the polysiloxane composition. The manufacturing method according to any one of claims 1 to 5, wherein the method is used as a liquid. 6. Claims for spraying polysiloxane ingredients together with other liquid ingredients, especially with fragrances The manufacturing method according to any one of ranges 1 to 6. 7. As a catalyst, amino-sensitive silane is used in an amount of 2 to 50% by weight relative to polysiloxane. 7. The manufacturing method according to any one of claims 1 to 6, wherein the method is used in an amount of %. 8. The polysiloxane component is added by heating the mixture at a temperature in the range of 20 to 50°C. 8. The manufacturing method according to any one of claims 1 to 7, which is applied without limitation. 9. An anion field produced by the production method according to any one of claims 1 to 8. 5-30% by weight of surfactant, 1 to 15% by weight of nonionic surfactant, Builder 10-65% by weight, Alkaline component up to 35% by weight, more preferably 5-30% by weight, cobuilder 5 weight % by weight, more preferably from 0.5 to 4% by weight, more preferably up to 40% by weight bleach. preferably from 6 to 30% by weight, up to 15% by weight bleach activator, more preferably from 1 to 8% by weight. %, up to 25% by weight of alkali silicates, especially sodium silicates, more preferably 2 ~18% by weight, Select from foam inhibitors, foaming agents, fabric softeners, anti-redeposition agents, optical brighteners, dyes, and fillers. 0.1-10% by weight of at least one selected component, and 1-20% by weight of water. A granular solid detergent containing a polysiloxane component and/or a polysiloxane component. 1 weight per 25 to 2000 parts by weight of granulated detergent % (in terms of polysiloxane component) Solid detergent. 10. Alkylbenzene sulfonates, fatty alcohol sulfates, fatty alcohols Cole ether sulfates, α-olefin sulfonates and/or fats anionic surfactant selected from the group consisting of acid alkyl ester sulfates; 5-28% by weight, Alkyl polyethylene glycol ether, nonylphenol polyethylene glycol selected from the group consisting of coal ethers and/or alkyl polyglycosides; nonionic surfactant 1 to 11% by weight, foam suppressor 0.1 to 3.5% by weight, Zeolite NaA 20-50% by weight Up to 10% by weight of sodium carbonate, more preferably 1-8% by weight of polycarboxylic acid 1 up to 0% by weight, more preferably 0.5-8% by weight, bleach 13-25% by weight, bleach activator 0.2-10% by weight, Up to 6% by weight of sodium silicate, more preferably 1 to 5% by weight, fabric softener, recycled Group consisting of anti-deposition agents, enzymes, optical brighteners, dyes, fragrances, formulation aids and fillers 1 to 3% by weight of one or more components selected from; Water 1-15% by weight The granular solid detergent according to claim 9, comprising: 11. Claim 9 or 10 having a bulk density of 400 to 1000 g/l Granular detergent. 12. An anion produced by the production method according to any one of claims 1 to 8. surfactant 5-15% by weight, 1 to 10% by weight of nonionic surfactant, Soap 0.5-2% by weight, Up to 30% by weight of sodium carbonate, preferably 10-27% by weight, zeolite Na A20-50% by weight, Up to 10% by weight of polycarboxylic acid, preferably from 0.5 to 8% by weight, resistant to spray drying up to 10% by weight of other detergent ingredients, preferably from 0.1 to 5% by weight, Water 1-20% by weight A detergent precursor product containing a polysiloxane component and/or a detergent component with it. 1 part by weight (polysiloxane) per 25 to 2000 parts by weight of granulated detergent A precursor product characterized by containing on the particle surface an amount of xane component equivalent).