SK108593A3 - Agglomeration of high active pastes to form surfactant granules useful in detergent compositions - Google Patents

Abstract

The present invention relates to a process for making a free flowing granular detergent comprising: mixing an effective amount of an aqueous surfactant paste having a detergency activity of at least 40 % and an effective amount of a dry detergency powder, said surfactant paste active and builder or powder having a ratio of 0.05:1 to 19:1 to form a mix; rapidly forming a uniform mixture from said mix at a temperature of from about 0 DEG C to about 80 DEG C; granulating said mixture into discrete detergent granules using a high speed mixing at a tip speed of about 5-50 m/sec; and wherein said surfactant paste is comprised of at least one anionic surfactant, and wherein said mixing and granulating are conducted simultaneously, or immediately sequentially. The nil-surfactant components of the finished granular detergent other than the granulated active paste, comprise a (relatively small) part of the total amount of builder, another part of the builder having been used for granulation. The nil active components can be spray-dried to form a powder having good color, frangibility, dissolution properties and desirable density and size characteristics for direct dry mixing with other ingredients of the finished granular detergent.

Description

Technical field

The invention relates to a process for preparing compositions comprising condensed detergent granules.

BACKGROUND OF THE INVENTION

Granular detergent compositions have hitherto been prepared mainly by spray drying. In this process, detergent ingredients such as surfactants and other ingredients are mixed with 35 to 50% water to form a slurry. The resulting slurry is heated and spray dried, which is expensive. However, a good agglomeration process could be less costly.

Spray drying requires 30-40% water removal. Spray drying equipment is expensive. The obtained granules have good solubility but low apparent weight, so that the packed volume is large. Also, the flowability of the spray-dried granules is adversely affected by large surface irregularities and therefore my granulate has a poor appearance. There are other known disadvantages in the preparation of granular detergents by spray drying.

There are many known non-spray drying processes for the production of detergent granules, but there are also drawbacks. They usually require more than one mixer and a special grinding procedure. Others require the use of an acid form of a surfactant to be carried out. Some others require high temperatures that degrade the starting materials. High surfactant pastes are not used in these processes due to n? their stickiness.

EP-A-0 345 090, published December 6, 1989, discloses a process for the production of particulate / married / detergent compositions, wherein the detergent acid is contacted with neutralizing agents and the particulates / granules / are obtained by contacting the detergent acid with the detergent acid. a particulate neutralizing agent or a detectable salt with a carrier in the absorption zone.

EP-A-0 349 201, published January 3, 1990, discloses a process for preparing condensed detergent granules by finely dispersing dry detergent ingredients and a highly active surfactant added as a uniform dough, which is then cooled and granulated using a fine dispersion, resulting in flowing granular particles.

EP-0 390 251, published Oct. 3, 1990, discloses a process for continuous granular detergent or composition comprising the following processing steps: first, the particulate starting material consisting of the detergent surfactant and the other ingredients is processed at high speed. mixers, then in a variable speed granulator / densifier, and finally in a drying / cooling device, adding powder in the second stage or between the first and second stages to reduce the amount of oversized particles.

A. Lavidsohn and B.I.ildildwidsky, Sviettheticsetergents, John Wiley and Sons, 6th Edition 1976, deal with general detergent knowledge, including the manufacture of finished detergent products.

High-shear and cold mixing processes are known per se, but require a special grinding step or other precautions. For example, in some DCs, they use dry neutralization techniques to mix the acid form of the surfactant with sodium carbonate. See U.S. Pat. pst. no. No. 4,515,707, Brooks, issued May 7, 1985; Japanese Laid-Open Application No. 183540/1983, Kao Sosp Co., Lt., filed September 30. 1983 8 Japanese Sho. Cion, K.K., June 5, 1986. Typically, here, an excess of carbonate (2 to 20 moles) is required to achieve an adequate conversion of the surfactant acids. Excess carbonate raises the alkaline range in the wash water, which may be undesirable, especially for some low phosphate kits.

The use of a surfactant acid usually requires direct use or storage at a cooling temperature. Highly reactive acids, such as alkyl sulphate acids, are exposed to de-gradation if they. do not cool, they tend to undergo hydrolysis during storage, the formation of sulfuric acid and alcohol. From a practical point of view, the known processes require close joining of surface production

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of active acid with granulation, which requires a greater capital investment.

A second route, well known in the art and described in the patent *. iterature, is the neutralization of the in-situ anionic surfactant by caustic solutions / nspr. MaOl '(or Keustic powders) e.g. NsjCO · ^ / ihnec! before or during the granulation step is ¹ · about. In these situations, caution should be taken to ensure complete neutralization of the acid and to avoid adverse effects on the rest of the surfactant matrix during storage or washing. The resulting particles are very dense granules that can be added to granular detergents.

Because this second route imposes lower temperatures and less drastic shear conditions than crutching and spray drying, it has many limitations. On the one hand, it is necessary to carry out a chemical reaction (neutralization) during or prior to the granulation step, thereby appreciably limiting the range of process conditions that can be used (temperature, chemicals, etc.). The very low surface area of the anionic surfactant prevents the use of chemicals sensitive to these acidic conditions. But above all, in the case of such anionic surfactants ^- 'which are not chemically stable in acid form or physically unstable, this process requires the close coupling of sulfuryl ATAC j / j sulfone.čne unit with neutralization / granulation step. These significant limitations in logistics and / or sketching of difficulties for these procedures, as well as the important increase in the complexity and difficulties of control systems, are the consequence.

The essence of climbing

The present invention brings about the above-mentioned problems of solution and provides a more acceptable and versatile guidance for the manufacture of granular detergents. The invention is based on an agglomeration / granulation step which is not bound to the sulfation / sulfonation process. The invention is based on the introduction of the anionic surfactant in an aqueous, highly concentrated solution of its salt, most preferably its sodium salt. These highly active / low moisture / surfactant pastes have a high viscosity but are pumpable at temperatures at which the surfactants are stable. This ensures the possibility of transporting and transferring chemicals from the production rooms to the granulation sites and allows for adequate storage prior to particle production. In such cases, when both sulfation and sulfonation and immediately preceding the granulation step, the invention allows to install temporary buffer t ^r nky that simplify the overall control unit. In the case of certain enionic surfactants or brick mixtures where highly viscous liquid crystalline phases are formed, this technology requires either the possibility of forming lower viscous phases (e.g. nuclear phase / or the use of some viscosity modifiers / e.g. hydrotropes /.

An important object of the invention is a process for producing a dense, concentrated detergent granular product by an agglomeration process as opposed to spray drying.

It is another object of the present invention to provide a granulated, ergonomic product with improved solubility and good dispersing properties and improved disrergency in the washing machine.

Other objects of the invention will become apparent from the following description.

The invention relates to an economical process for producing a dense, concentrated detergent granular product, and in particular to compositions comprising highly active condensed detergent granules.

Referring to Figure 1, a shear rate viscosity graph for a / non-surfactant / nile surfactant containing a relatively small amount of zeolite, b / a similar, typically detergent slurry containing a surfactant and a relatively large proportion of zeolite and c / surface an inactive slurry containing no zeolite at all.

Figure 2 shows the solubility of spray dried surfactant powder containing a relatively small amount of zeolite compared to the solubility of powder made of surfactant containing slurry.

The invention relates to a process for the manufacture of a free-flowing granular detergent in which an effective amount of an aqueous surfactant paste having a detergency efficiency of at least 40% is admixed with an effective amount of a dry detergent powder. The ratio of surfactant paste as active ingredient and base to powder is 0.05: 1 to 19: 1. From this mixture, a uniform mixture is rapidly formed at a temperature of about 0 to 80 ° C, which is then granulated into separate detergent granules using high speed mixing with a peripheral speed of about 5 to 50 m / sec. The surfactant paste consists of at least one anionic surfactant (s) and some other surfactants which, if present, are selected from the group of anionic, nonionic, zwitterionic, ampholvtic and cationic surfactants and the feelings of mixtures, The mixing and granulation is performed simultaneously or immediately laterally.

The invention is based on agd. a mercurial / granulation step that is not bound to the sulfation / sulfonation process. In one embodiment of the invention, an anionic surfactant is used in an aqueous concentrated solution of a salt thereof, preferably a sodium salt. These highly active (and preferably low moisture / surfactant pastes) have a high viscosity, but can be pumped at temperatures at which the surfactants are stable. In other administrations, the invention requires anionic surfactants or mixtures thereof containing at least one anionic surfactant to form highly viscous liquid crystalline phases because less viscous phases have formed or some viscosity modifiers are used.

It is another object of the present invention to provide a process for producing a free-flowing detergent composition, wherein the granular surfactants are mixed with the remainder of the detergent ingredients, which are typically spray dried onto an inflated powder. The stream preferably contains 15 to 55% by weight of the base component, wherein the spray dried slurry is mixed with the agglomerated surfactant. It has been found that the viscosity of the non-surfactant slurries containing ηΐΡ ^ό ó amounts of the main component (detersive powder), preferably zeolite, is to the same range as the viscosity of the surfactant-containing aqueous slurries at the same moisture content and within the appropriate shear rate range. It is therefore possible to spray-dry a non-surfactant slurry using pressure punches under normal conditions. The advantage of small amounts of powdered ingredients in surfactant slurry ineffective is that it can be obseihnuté viscosity-increasing compo those, such as polymers or substances ⁱⁿ ine men. By using relatively small amounts of the powder component in the ineffective slurry, where the main honor of the total amount of powder component is used to agglomerate the active grazing, there is the possibility for other impregnants such as layered silicate or citrate.

A spray-dried powder resulting from a non-surface effect slurry, which contains relatively small amounts of the basic component, is well soluble in comparison with. detersive mixtures formed by the spraying of dried slurry containing a surfactant. by mixing the spray-dried, non-surface-effect powder with granulated active paste and other ingredients such as bleaching agents, bleach activators, antifoams, enzymes and stabilizers, a finished product is obtained with good dispensing and dispersing properties in the laundry scatter. Pozstrekovým drying the aqueous slurry of inert surface, kto'-A comprises a portion of the total quantity of basic components, a powder is obtained with improved absorption cf. ^c it with a basic component in the raw state. Thus, a larger amount of nonionic surfactant can be sprayed onto the spray dried inactive slurry.

In accordance with the present invention, suitable pastes of salts of anionic surfactants of sionic surfactants are suitable. In a particularly preferred sodium salt, the concentration and surfactant are as large as possible (i.e. with the least possible humidity, at which liquidity is still possible, so that it can be transported by the pump at temperatures at which it remains stable while granulating. the use of various pure or mixed surfactants is known to be of practical importance for the industrial use of the invention. It occurs in particles with adequate physical properties that are added to the granular deterrents. The anionic surfactant per substance must be included in the paste at a concentration of 10%, preferably

It is preferred that the moisture content of the surfactant aqueous paste is as small as possible, but to maintain the fluidity of the paste, although low moisture results in a higher surfactant concentration in the final particle. Preferably it contains pa

paste before entering the applicator, hassle free and very

abv minimizes the total water level in the system during mixing, pelleting and drying. The lower active surfactant ratio of water allows the base component, e.g.

1: 1, (2) higher levels of other liquids in the assembly without ebv giving rise to dough or grains, (3) less cooling due to higher permissible granulation temperatures and (4) less need for drying the granules, and the final moisture limit was reached.

Two important parameters of the surfactant pastes that may affect the mixing and granulating stages are temperature and viscosity of the paste. The viscosity is, inter alia, a function of concentration and temperature, with a range of 3,000 to 10,000,000 cps in the present invention. Preferably, the viscosity of the paste entering the assembly is about 20,000 to 100,000 cps, and more preferably about 30,000 to 70,000 cps. The viscosity of the paste according to the invention is measured at a temperature of 7 ° C.

The paste may be introduced into a mixer at an initial temperature between its maknutis point (usually in the range of 40-60 ° C) and its decomposition temperature (degrsdation), which depends on the chemical nature of the paste. "Apr. alkyl sulfate pastes have the tendency to degrade not 7? to < 8 ° C. High temperatures reduce the viscosity, which simplifies pasting the paste, but results in less active agglomerates. Use of moisture reduction steps / e.g. scattering deflecting the drying / vvžaduje However, the use of higher temperatures / 100 of ³ C /. In the process according to the invention, the activity of the isomerates is maintained. high degree due to moisture removal.

The introduction of the paste into the mixer can be carried out in a number of ways, from simple pouring to high pressure pumping through narrow openings at the end of the pipe through the inlet of the mixer. Although all of these processes are suitable for the manufacture of agglomerates with good physical properties, it has been found that in a preferred embodiment of the invention, the paste injection molding results in a better distribution in the mixer, which allows to obtain particles of the desired size. Using high 'erpscích pressures for' entrance in the mixer results in increase of activity in the final, and ^r lom.erátoch. by combining both effects and placing the paste through the holes (extrusion) that are. sufficiently small, the desired flow rate is achieved, but with? maintains the maximum possible pumping pressure in the system, thus achieving very disadvantageous results.

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The activity of the aqueous surfactant paste is at least 30% ^{and can be} as high as about 95, with preferred activities being 50 to 50% X and 65 to 75% X. The balance / equilibrium / paste is mainly water but can also be processing aids, such as a nonionic surfactant. At higher active concentrations, no basic constituents or only a small amount of brick are required for granulating the grazing in the cold. The resulting concentrated surfactant granules may be added to the basic ingredients or powders, or may be used in conventional agglomeration operations. The aqueous active paste comprises an organic surfactant selected from the group consisting of anionic, zwitterionic, ampholytic and cationic surfactants and mixtures thereof. Antenna surfactants are preferred.

Eionic surfactants are used as secondary surfactants or processing aids and do not fall within the scope of the surfactant, the surfactants used are disclosed in U.S. Pat. pat. no. 3 664 961, Morris, who came out? May 197, U.S. Pat. pst. no. No. 3,919, 67c, Laughlin et al., Issued December 39, 1975. Among useful cationic surfactants are those? those described in U.S. Pat. ; -At. no. No. 4,222,995, Cockrell, issued September 16, 1989; and in U.ä. pst. no. No. 4,239,659, Murrh, issued December 15, 1989. However, cationic surfactants are usually less compatible with aluminosilic materials than are disclosed herein, and are therefore preferably used in small amounts or not used in the compositions of the invention at all. representative examples of surfactants in the compositions of the invention.

Water-soluble salts of higher fatty acids, e.g. soaps are useful anionic surfactants in the compositions herein. These include alkali metal soaps, such as sodium, potassium and alkylammonium εο ^Ί šší ^šší mast ^mast mast ^mast ktoré ^šší šší ^šší šší ^šší šší ^šší šší ^šší šší ^šší šší ^šší šší ^šší šší ^šší šší ^šší šší ^šší .

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i.a., the depot was prepared by direct saponification fats and olefins or by neutralization of free fatty acids. Particularly preferred are the sodium and potassium salts of mixtures of fatty acids derived from coconut oil and tallow, i. sodium or potassium tallow and coconut soap.

Useful enionic surfactants also contain water-soluble salts, preferably alkali metal, ammonium, and ^1- ammonium salts of organic sulfuric reaction orolts having in their molecular structure an alkyl group of about 10 to 20 carbon atoms and an ester group of sulfonic acid. or sulfuric. (The alkyl portion of the acyl groups) is included in the term alkyl. Examples of such a group of synthetic surfactants are sodium and potassium alkyl sulfates, particularly obtained by sulfating higher alcohols (with carbon atoms) and reducing tallow and coconut oil glycerides such as sodium and potassium alkylbenzene sulfonates in which the alkyl group contains about 9 to 15 carbon atoms in straight or branched chain configuration, eg * of the type described in U.3. P ^ t. no. Of particular interest are linear straight chain alkylbenzene sulfonates in which the average number of carbon atoms in the alkyl group is about 11 to 13, denoted by C1-4 LAS.

other suitable anionic surfactants for use herein are sodium alkyl glyceryl ether sulfonates, especially the higher alcohol ethers derived from. tallow and coconut oil; coconut fatty acid sodium monoglyceride sulfonates as well as the corresponding sulfates; sodium or potassium salts of alkylphenolethylene oxide ether sulfenes containing 1 to 19 units of ethylene oxide per. a molecule and wherein the alkyl groups contain from about 1 to about 12 carbon atoms; and sodium or potassium salts of alkylethyleneside sulfates containing about 1 to 10 units of ethyl oxide per molecule and wherein the alkyl group contains about 10 to 20 carbon atoms.

Useful anionic surfactants known herein are the water-soluble salts of o-esters of alpha-6-fatty acids containing about 6 to 20 carbon atoms in the fatty acid group of about 1 to 10 carbon atoms in the c-sulfur group; water-soluble salts of 2-acvloxy-alkane-1-sulfonic acids containing about 2 to 9 carbon atoms in the acyl group and about 9 to 23 carbon atoms in the skeletal residue; Alkyl ether sulfates containing about 10 to 20 carbon atoms in the alkyl group and about 1 to 30 moles of ethylene oxide; water-soluble salts of olefinic sulfonates containing from about 12 to 24 carbon atoms; and beta-alkyloxyalkene-1-phonates containing about 1 to 3 carbon atoms in the alkyl group and about 5 to 20 carbon atoms in the pancreatic residue. Although acid salts are typically mentioned and used herein, acid neutralization can be performed as part of the finely dispersing step.

Preferred enionic surfactant pastes are mixtures of linear or branched alkylbenzenes of C 10 -C 16 alkyls and C 10 -C 16 alkyl sulfates. These pastes are usually prepared by reacting a liquid organic substance with sulfur trioxide to form a sulfone or sulfuric acid, which is then neutralized to its salt. Sol is a surfactant paste which is the subject of this entire patent. The sodium salt is preferred due to the advantages of the final conversion and the cost of NaOH over other neutralizing agents, but is not necessary since other agents can be used, e.g.

KOH.

Water-soluble nonionic surfactants are also useful as secondary surfactants in the compositions of the invention. However, anionic / nonionic mixtures are used in preferred processes. A particularly preferred paste comprises a mixture of nonionic and anionic surfactants in a ratio of about 0.01: 1 to 1: 1, more preferably about 0.05: 1. The cationic substances can be used up to an amount in which primarily organic surfactants are present. Such nonionic materials include compounds produced by condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkylaromatic in nature. The polyoxyalkylene moiety that condenses with a hydrophobic group can be readily treated to provide a water-soluble compound with the desired degree of equilibrium between hydrophilic and hydrophobic elements.

Suitable nonionic surfactants include the polyethylene oxide condensates of alkylphenols, e.g. condensation products of alkylphenols having an alkyl group of about 6 to 16 carbon atoms, in a straight or branched chain configuration, with about 4 to 25 moles of ethylene oxide per mole of alkyl phenol.

Preferred nonionic components are the water-soluble condensation products of C 6 to C 22 aliphatic alcohols in a straight chain or branched configuration with from 4 to 25 moles of ethylene oxide n? 1 mole of alcohol. Particularly preferred are the condensation products of alcohols containing an alkyl group of about 9 to 15 carbon atoms with about 4 to 25 moles of ethylene oxide per mole of alcohol and the condensation products of propylene glycol with ethylene oxide.

Semi-polar nonionic surfactants include water-soluble amine oxides containing one alkyl moiety of about 10 to 18 carbon atoms and 2 moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups of 1 to about 3 carbon atoms; water-soluble phosphine oxides containing one alkyl moiety of about 10 to 18 carbon atoms and 2 moieties selected from the group consisting of alkyl and hydroxyalkyl groups of about 1 to 3 carbon atoms; and water-soluble sulfoxides containing one alkyl moiety of about 10 to 18 carbon atoms and a moiety selected from the group consisting of alkyl and hydroxyalkyl moieties of about 1 to 3 carbon atoms.

L'e ^': zi zwitterionic surfactants include derivatives of aliphatic or aliphatic derivatives of the compounds heterocyklickýc} secondary and tertiary amines in which the aliphatic radical sorry bu3 be straight or branched chain and wherein existing in 12 day of the aliphatic substituents contains from about O to about 18 carbon atoms, and at least one aliphatic substituent contains an anionic water-soluble group.

Zwitterionic surfactants include derivatives of aliphatic quaternary ammonium phosphorus and sulfonium compounds in which one of the aliphatic substituents contains about 6 to 18 carbon atoms.

Particularly preferred surfactants herein include linear alkylbenzenesulfonates containing from about 11 to 14 carbon atoms in the alkyl group; tallow alkyl sulfates; cocosalyl glyceryl ether sulfonates; alkyl ether sulfates wherein the alkyl moiety contains about 14 to 18 carbon atoms and the average degree of ethoxylation is about 1 to 4; olefinic or paraffinic sulfonates containing from about 14 to 16 carbon atoms; alkyldimethylamine oxides in which the alkyl group contains about 11 to 16 carbon atoms; alkyldimethyl ammonio propane sulfonates and alkyldimethylammonium hydroxy propane sulfonates in which the allyl group contains about 14 to 18 carbon atoms; higher fatty acid soaps containing from about 12 to 18 carbon atoms; condensed products of C8-alcohols with about 3 to 8 moles of ethylene oxide and mixtures of said compounds.

Useful cationic surfactants are water-soluble quaternary ammonium compounds of the formula R RR RRgRgRyNX ”wherein R ^ is alkyl of 10 to 20, preferably 12 to 18 carbon atoms, and R-, Rg and Ry are each C ^yy88, preferably methyl,

X is an anion, e.g. chloride. Examples of such trimethyl ammonium compounds include C 1-4 alkyl-trimethylammonium chloride and cocyl trimethyl ammonium tosulfate.

Particularly preferred surfactants used herein include sodium linear C 1-6 alkylbenzenesulfonate; olefin sulfonates; tertiammonium-C 1-6 alkyl-benzenesulfonate; alkylsulfonates / tallow, coconut, palm, of synthetic origin, e.g. CM-, etc. /; sodium alk 1 sulfates; MRS; sodium coconut alkyl glycervether ether sulfonate; a sodium salt of a sulphated tallow alcohol condensation product with about 4 moles of ethylene oxide; a coconut fatty alcohol condensation product with about 6 moles of ethylene oxide; a tallow fatty alcohol condensation product of about 11 moles of ethylene 13-xide; a condensation product of a fatty alcohol containing about 14 to 1? about 7 moles of ethylene oxide; a condensation product of a fatty C 1-4 alcohol with about 3 moles of ethylene oxide; 3- (N, Ed-methyl-N-cocosalkylammonio) -2-hydroxypropane-1-sulfonate; 3- (N, Nóimetvl-to-coconutalkylammonio) -propane-l-sulfonate; 6- (A-dodecylbenzyl-N, N-dimethylammonio) hexanoate; dodecyl dimethyl amine oxide; kokosalkyldiemtylamínoxid; and water-soluble sodium and potassium salts of coconut and tallow fatty acids.

As used herein, the term "surfactant" or surfactant refers to nonionic surfactants unless otherwise indicated. The surfactant (excluding the nonionic agent) and the dry, thermosetting ingredient or powder are in the range of 0.005: 1 to 19: 1, preferably 0.05: 1 to 10: 1, and more preferably 0.1: 1 to 5: first Even more preferably, the surfactant to detergent component ratios are 0.15: 1 to 1: 1 and 0.2: 1 to 0.5: 1.

Although an anionic surfactant in the form of the above-described pastes is used in a suitable embodiment of the process of the invention, a certain amount can be supplied in the form of a powder, for example a blown powder. In these embodiments, care must be taken to ensure that the tackiness and moisture of the flowing powder is as low as possible, thereby avoiding increased loading / loading of the anionic surfactant and thereby producing a sinter with a very high concentration of surfactant. In a preferred agglomeration process, a liquid stream may also be used to introduce other surfactants and / or polymers. This can be done by premixing the surfactant into a single liquid stream, or alternatively by bringing the various streams into a fracture. In these two embodiments of the process, there may be differences in the properties of the final particles ( _in- feed, gelling, dissolution rate, etc.), especially if the mixed surfactants are allowed to form before the particle formation. These differences can then be utilized as the advantages of the intended application for a particular preferred process.

Ss which also observes that using now described technological gie 14 is m ^ft žu add larger amounts of certain chemicals / example. of non-ionic, lemons:, acid (in final composition compared to other known processes, besides ab · ”, there were deleterious effects on some key matrix properties (sintering, squeezing, etc.).

As used herein, the term fine dispersion mixing and / or granulation means mixing and / or gronifying the mixture in a finely dispersing mixer at a blade speed of about 5 m / s to 50 m / s, unless otherwise specified. The total mixing and granulating time is preferably on the order of 0.1 to 10 minutes, more preferably 0.1 to 5 minutes, and most preferably 0.2 to 4 minutes. More preferably, the mixing and granulating speeds are about 10 to 45 m / s and about 15 to 40 m / s.

Ka carrying out the method of the Invention ss m ^ft žu use various devices and units which are suitable for processing surfactants. Suitable devices include, for example, falling layer sulfoixing reactors, digestion tanks, esterification reactors, etc. Any of a number of mixers / agglomerators may be used for mixing / agglomeration. In one preferred embodiment, the method according to the invention is carried out continuously. Particularly preferred are the Fukae® FS-G mixers manufactured by Fukae Powtech Kogvo Co., Sp. the apparatus is substantially in the form of a cup-shaped container accessible upwardly through the door and provided near the bottom with a stirrer substantially with a vertical axis and a cutting mechanism disposed on the side wall, i.e. a stirrer. and the cutting mechanism may be actuated independently of one another and at particularly variable speeds. The container may be provided with a cooling jacket or, if necessary, a cryogenic unit.

Other similar mixers suitable for use in the process of the invention are the Diosna (R) V series from Lierks und Sohne, Germany, and Pharma Liatrix from the former T Kielder Ltd., England. Other blenders you can think of. that are suitable for use in the method of the invention, Fuji's VG-C series is Fuji Sangyo Co.,

R

Japosko, and Po's from Zanchetta and Co srl. Italy.

Other suitable St. Firich equipment, PV series, manufactured by Gustau Fardh.eim, Germany; L-o-.ige '-ζ · F-series; for batch mixing, of the Iaud KI series; for continuous mixing / agglomeration, manufactured by Lolige Maschinenbau GmbH, Paderberg, Germany; Grais T16G series, manufactured by rais Werke GmbH, Lünnheiin, Germany; and Winkworth®

RT 25 series, manufactured by Winkworth Hachtnery Ltd., Bershire, England.

left examples of suitable blenders of St Littleford. mixer, model jf FI.1-13O-L-12, with internal cutting blades, and Food Processor, model U PCX-Plus, with 19.7 cm blades. Other mixers with fine dispersion mixing and granulating ability with a residence time of the order of 0.1 to 10 minutes can also be used. A DC impeller with a turbine-type impeller having several blades on a rotating axis is preferred. The invention may be practiced in batches or as a continuous process.

The preferred operating temperatures should be as low as possible, since this results in a higher concentration of surfactants in the final particles. It is preferred that the temperature during the agglomeration is less than 50 ° C, more preferably 0 to 70 ° C, even more preferably 10 to 60 ° C, and most preferably 20 to 50 ° C. The lower operating temperatures of the process of the invention can be achieved by various methods known in the art, such as nitrogen cooling, water cooling in the jacket of the apparatus, by adding a solid ⁵ po <3; preferred process is the cooling of the solid CO2, and the most preferred method for j _much nitrogen cooling.

A highly attractive process in a preferred embodiment of the invention to further increase the surfactant concentration in the final particles is accomplished by adding to the liquid stream containing the anionic surfactant and / or other surfactant to increase viscosity and / or the melting point and / or reduces the tackiness of the paste. In a preferred embodiment of the process according to the invention, the addition of these elements can be carried out in a line as the paste is pumped into the agglomerator. Examples of such elements include various powders, which will be described in more detail below.

The process of the invention produces high-density granules for use in detergent compositions. A preferred granular detergent granulate composition comprises a high concentration of surfactant. By increasing the concentration of the surfactant, it is achieved that the particles / agglomerates in the product are more suitable for many different formulations. These highly surfactant-containing particulate agglomerates require less finishing than the final agglomerates. This avoids the use of large amounts of opaque processing agents (inorganic powders, cents), which can be used in other stages of the overall production process of ¹ ether; (spray drying, dedusting, etc.)

The granules produced by the process according to the invention are large, small and dusty. freely flowing. Preferably, they have a bulk density of about 0.5 to 1.0, more preferably about 0.6 to 0.8 g / ml. The average particle size g / according to the invention is about 200 to 1000 microns. Preferred particles (granules) so produced have a size in the range of 200 to 2000 microns. More preferably, the granulation temperatures are in the range of about 10 to 60 ° C, and most preferably about 20 to 50 ° C.

The desired free-flowing granule content of the invention can be adjusted to the levels required for the intended application by drying in a conventional powder-drying apparatus, such as a fluid bed dryer. If a fluid bed hot-air drier is used, care must be taken to avoid degradation / degradation / heat-sensitive granule components. It is also desirable to incorporate a cooling stage prior to bulk storage. This step can also be carried out in a conventional fluidized bed by introducing c lad fine air. The drying / agglomeration of the agglomerates can also be carried out in any other powder-drying apparatus such as rotary dryers.

For detergent applications, it is necessary to keep the final moisture of the agglomerate below the values at which the agglomerates can be stored and transported in bulk. The exact amounts of moisture depend on the composition of the agglomerate, but are typically found at levels of 1 to 1.5% of free water (i. % water which is not bound to any crystalline species in the aplomerate (a) more preferably at 2 to 4%.

- 17 In the process of the invention and the compositions obtained from the following Z, E m ^E using any of a reagent Compatible dete ^ ingredient or combination of ingredients or a powder.

Here the described detergent composition m / ND 8luminosilikctový iói.ovýmenný containing crystalline material of formula I, and ₂ t (.A10 _{2) z.} (Si0 _{2) y] 2} 0 .xl emanations which are at least about 6, the mole ratio zky ssi 1.0 to 0.4 and is about 10 to 264. The amorphous hydrated sluminosilicate materials herein are empirical ^; _from C ^ AIO. wherein K is sodium, potassium, ammonium or substituted ammonium, z is about 0.5 to 2 µm is 1, said materials having a magnesium ion exchange rate of at least 50 milligrams of carbonate (CaCO 2) hardness per gram of anhydrous aluminosilicate. Hydrated sodium Zeolite A having a particle size of about 1 to 10 microns is preferred.

The aluminosilicate ion exchange component materials used herein are in hydrated form and contain about 10 to 28% by weight, if crystalline, and optionally larger amounts of water, if amorphous. Highly preferred crystalline spherosilicone ion exchange materials contain about 18-22% water in their crystalline lattice. These materials have a particle diameter of 0.1 to 10 microns. Amorphous materials are often smaller, e.g. less than about 0.01 micron. Preferred ion exchange materials have a particle diameter of about 0.2 to 4 microns. The term particle size diameter as used herein means the mean particle size diameter of the weight of a given ion exchange material as determined by conventional analytical techniques, for example, by scanning electron microscopy. The crystalline aluminoslicate ion exchange materials herein are also characterized by a calcium ion exchange rate of at least about 200 mg CaCO2 equivalent of water hardness / g aluminosilicate, calculated as n = anhydrous basis, and which typically ranges from about 300 to 352 mg. eq./g. Aluminosilicate ion exchange materials disclosed herein

1G sp is still characterized by a calcium ion exchange rate of at least about 2 grains of Ca ⁺⁺ (p, alon / minute / gram / gallon of aluminosilicate / anhydrous basis), and is usually in the range of about 2 to 6 grains / golon / minute / grsm / gallon, based on the calcium ion hardness. The aluminoslikate optimum for the bees of the deterrent component exhibits a calcium ion exchange rate of at least about 4 grains / gallon / minute / grem / gallon.

The amorphous aluminosilicate ion exchange materials usually have ob4.4 interpreted _in exchange capacity for the LG, at least about 50 mg eq. CaCO ^ / g / 12 mg ^l-g / g / s K'g exchange rate of at least about 1 grain / gallon / minute / grsm / gallon. The amorphous materials do not produce an observable diffraction (flexure) pattern when investigating Cu radiation (1.54 angstrom units).

The aluminosilicate ion exchange materials used in the practice of the process of the invention can be obtained commercially. Aluminosilicates suitable for the present invention may have a crystalline or amorphous structure and may be natural or synthetic. A method for producing aluminosilicate ion exchange materials is disclosed in U.S. Pat. no. No. 3,955,669, Krummel et al., Issued Oct. 12, 1976, incorporated herein by reference. Preferred synthetic crystalline sluminosilicate ion exchange materials suitable for the present invention are obtainable under the designation Zeolite A, Zeolite B and Zeolite X. In one particularly preferred embodiment, a crystalline aluminosilicate ion exchange material of the formula

K a ₁₂ [CA 10 ₂ ) ₁₂ (SiO ₂ ) ₁₂ ] xH ₂ O wherein x is about 20 to 30, especially about 27; and its particle size is typically less than about 5 microns.

The granular detergentv invention can contain neutral or alkaline salts thereof, wherein p ¹ * jc solution of 7 or more FC-moo lying around Ozu be organic or inorganic. The detergent component salt contributes to obtaining the desired detergent density and volume. granules. Since some salts are inert, many of them act as detergent materials in the wash solution.

Examples of neutral water-soluble salts are alkali metal, ammonium or substituted ammonium chlorides, fluorides and

- 19 sulphates. Preferred is alkali metal salt, especially sodium. In detergent granules. sodium sulfate is typically used and is a particularly preferred salt. After the granular detergents of the invention The m ^ft add the citric acid and, in general, any other organic or inorganic acid, as long as it is chemically compatible / incompatible / aglomerňtovej the rest of the composition.

Other useful water-soluble salts include compounds commonly known as detergent materials. They are usually selected from various water-soluble, alkali-metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, silicates, boritsnes with polyhydroxysulfonates. Preferred are the alkali metal, especially sodium, salts of the above compounds.

Particular examples of inorganic phosphate builders are the ^q Ne and potassium tripolyphosphate, pyrophosphate, metaphosphate polymérv ny with a degree of polymerization: about 6 to 21, and orthophosphate. examples of polyphosphonates. The detergent ingredients are the sodium and potassium salts of ethylene-diphosphonic acid, the sodium and potassium salts of trans-1-hydroxy-1,1-diphosphonic acid, and the sodium and potassium salts of ethane-1,1,2-triphosphonic acid. . Other phosphorous detergent compounds are disclosed in U.S. Pat. 3,159 ºcl, 3,213,030,

422,021, 3,422,137, 3,400,176 with 3,400,148, which are incorporated herein by reference.

Examples of non-phosphonic inorganic detergent builders are sodium and potassium carbonate, bicarbonate, sequicarbonate, tetraborate. decahydrate and silicate having a SiO2 to alkali metal oxide molar ratio of 0.5 to 4.0, preferably about 1.0 to 2.4. Compositions produced by the process of the invention do not require excess carbonate in the treatment and preferably contain no more than 2% finely ground calcium carbonate as described in US Pat. no. No. 4,196,033, Čiarke et al., Issued April 1. 1980, which are mentioned as preferred compositions, the + Cre ^a 8bsehjú no calcium.

As mentioned above, in a preferred embodiment of the present invention, powders commonly used in detergents such as zeolite, carbon dioxide, silicon dioxide, silicate, citrate, phosphate, perborate, etc. may be used. and processing aids such as starch.

Suitable bodies are r ^ft pollution oganikcé polymers, some of which can function as builders, thereby improving detergency. Such polymers may include such sodium lower alkyl carboxycelluloses, sodium lower alkylcelluloses, and lower alkyl sodium hydroxyalkylcelluloses such as non-sodium carboxymethylcellulose, sodium cellulose sodium and sodium hydroxypropylcellulose, polyvinyl alcohol / polyvinyl alcohol / polyvinyl alcohol / polyvinyl alcohol / polyvinyl alcohols. which often contain some polyvinyl acetate, polycrystalline araids, polyacrylates, and cutting copolymers such as maleic acid and hides copolymers. The molecular weights of such polymers are in a wider range, but are generally in the range of 2,090 to 199,999.

Polymeric polycarboxylate detergent builders are described in U.5. No. 3,339,967, Diehl, issued Mar. 7, 1976. Such materials include the water-soluble salts of aliphatic and copolymers. carboxylic acids such as maleic, itaconic, mesaconic, fumaric, rconitic, citreconitic and methylenemalonic acids.

The compositions of the invention may contain other components commonly used in the compositions. These include color-removing aids, bleaching agents and bleach activators, foaming agents or suds suppressors, anti-inflammatory and anticorrosive agents, soil suspending agents, soil release agents, dyes, fillers, optical brighteners. , beta-modifying agents, non-detergent alkalinity sources, hydrotropes, germicides, enzymes and their stabilizing agents, chelating agents, and perfumes.

Optical brighteners may be contained either directly in the agglomerates in question, into which they are incorporated in the powder stream fed to the sintering unit, or added to the final mixture by spray drying, or both.

The foam suppressant particles may also be incorporated either directly into the agglomerates herein, in the powder stream coming into the agglomeration unit, or into the final mixture by adding dry powder. The foaming performance of these particles depends on fatty acids or silicones.

As used herein, the terms LAS and AS refer to sodium laurylbenzanilonate and k.vl sulfate. MES means sodium methyl ester sulfonate. Terms such as C 1-6 denote and C 1-6 -alkyl, unless otherwise indicated. TAS means tallow alkyl sulfate. Isobanol 45E7 is a 7-unit ethylene oxide C C^ / C C-alcohol ethoxylate, manufactured by Shell Co.

The invention of the advantages that n

v.e and more clearly exemplified on the basis of these examples, do not limit the invention in any way. Percentages are based on weight after drying unless otherwise noted. The tables provide an additional description of the procedure.

Examples of the invention

EXAMPLE 1 An aqueous surfactant LAS paste having a detergency efficiency of 78% and a water content of 21% is pumped by a positive displacement pump into a Lodige CB 55 at a rate of 20 t / h. The viscosity of the paste is 25,000 cps at 70 ° C. At the same time, a powder stream containing a 1: 1 mixture of zeolite A and citrate citrate dihydrate finely divided at a rate of 4 t / h is fed to the Lodige CB 55 mixer. Also mentioned in the same mixer are two streams containing recycle from the agglomerate screening, one containing wet coarse particles and the other stream containing dry fine particles. The agglomerates leaving the mixer are dried in a temperature-controlled fluidized bed, leaving air at a temperature of 51-55 ° C. After drying at an average time of over 15 minutes, the agglomerates are cooled in a second fluidized bed of powder having an outlet temperature of 45 ° C. The cold dried product leaves the refrigeration plant and is screened on the nets and the product with the desired particle size is stored in the silo. The agglomerates produced according to this example have a detergency efficiency of 25 &gt; 0 and a density of 780 g / l.

Example 2

The procedure is analogous to Example 1. In this case, an aqueous surfactant paste C 2 AS with a detergency efficiency of 70% and a water content of 25 fed at a rate of 2.0 t / h is used. The viscosity of pass + y is 35,000 cps at 70 ° C. The powder stream consists of a 2: 1 mixture by weight of zeolite A and sodium carbonate finely divided and is reported at a rate of 2.0 t / h. The agglomerates produced according to this example have a detergency efficiency of 39% and a density of C75 g / l.

Example: 3

This example describes a batch operation in a pilot scale in a Sirich PV02 high-speed mixer.

The first mixer is first filled with a mixture of powders used, in this case in a 2: 1 ratio of zeolite A and finely divided sodium carbonate (3 kg). An idSS aqueous surfactant paste having a detergency efficiency of 63% and a water content of 33% was added at the top of the powder mixture, having a sufficient amount of 1.6 kg I-E'S fluid bed and operating at 1607 rpm. It is necessary to add pastes before granulation (in this pasture) is achieved. The agglomerates are discharged into a drier and screened with suitable sieves. The resulting glomerates are produced with a detergency efficiency of 22% and density

750 g / l.

Example 4

This example is similar to Example 3. The powder blend again contains zeolite A and a finely divided 2: 1 carbonate. The surfactant is an aqueous C ... AS powder with a detergency efficiency of ‘i / ° d / 0 c * 0 µS kg /, and a start of granulation. dry ice, said the temperature is a mixture that can run in the cold.

> om water 13 &. In this example, powders (1.05 paste (3 kg)) are added to the mixer (Sirich PV02) before

After the mixer was also added some amount (2 kg) the temperature lowered below -15 ° C. The mixer era was then run at 1600 to / min. At lower levels, first in the form of a fine powder, the blender raises the net temperature to a point (12 ° C), at which grinding occurs. The process is then stopped and the agglomerates are dried in a fluidized bed and screened by sieving. The agglomerates produced had a detergency efficiency of 60% and a density of 625 g / l.

I. have excellent physical properties.

Example 5

The surfactant aqueous ¹ 's active-C and, once a detergent activity of 71 25?' Obsatom water 2 :. b is pumped into a Lodige C3 30 by a positive displacement pump. At the same time, a powder stream containing a mixture of zeolite A and a finely divided sodium carbonate in a weight ratio of 2: 1 is also introduced into the mixer. the powder flow rate is maintained at a constant rate of 400 kg / h. The flow velocity of the paste is varied until agglomerates having the desired particle size distribution (maximum yield between 200 and 1800 µm) are obtained. The process under ambient conditions requires a rate of 245 kg / h of the pumped surfactant paste, with the DCs (after drying) obtaining agglomerates with a detergency efficiency of 27%. A liquid nitrogen stream is then introduced into the mixer at the point of entry of the powder stream. Nitrogen is reported at a rate of 4.5 kg / h. In order to obtain agglomerates with the desired particle size distribution, it is necessary to increase the paste flow rate to 346 kg / h to obtain agglomerates (after drying) with a detergency efficiency of 32% ·

Example 6

In this example, a kitchen food mixer for a versatile purpose is used to produce agglomerates containing a full detergent assembly for use in a laundering process. First, all powder components of the assembly are weighed and then added to the mixer. This mixture contains:

Zeolite A 160.8 g Citrate dihydrate 74 0 g Soka? and CP5 P / V 20.8 g Silicate 20 H 12.7 σ about Sodium carbonate 28.8 g

All powders are finely ground before being added to the blender. The DC mixer is then started at low speed for 1 minute, with the ss. ensure good mixing of the powders, the surfactant pastes being prepared in a separate food mixer. This mixture contains:

LAS / 7c $ active, 21% water /

TAS / 551 active, 44% water /

Lobanol 45S7 / 1 ^ 0% active /

59.2 g 42.0 g 15.4 g

The pastes are mixed well at a higher mixer speed for about 1 minute. The premixed powder is then added to the top of the premixed paste and the mixer does not wait. run at moderate speed until granulation occurs (after about 1 minute). AG1 omelets prepared are dried in suspension / fluidized by ^'nom L * OCT / and classified through sieving by sieves, ^ hese agglomerates have excellent physical properties and a very' giants solubility so that they have excellent efficiency

k.y at washing.

EXAMPLE 7 kg of fast hydrating sodium tripolphosphate (STPP) in finely ground form is placed in a Loeige F ' mixer equipped with internal plowers and high sharp cutting blade knives. ^J T'ore the mixer was added 30 kg of an aqueous surfactant LAS paste with a detergent activity of 78 & ENCN% and a water content of 1 21, and the mixer is closed. The mixer is then started and at the same time water is poured through the opening in the cap to granulate. The agglomerates are then collected, dried in a fluid bed dryer and screened by sieving. The resulting agglomerates have a detergent efficiency of 25 L, excellent physical properties and solubility, thus being suitable for addition to granular detergents.

Example S

This example demonstrates that in a cranked detergent composition

- one part of which consists of an agglomerated active paste, the spray-dried surfactants have improved solubility and dispersing properties compared to typical detergent products which are commercially obtainable granular detergents which are obtained by spray drying of an active anionic surfactant slurry. active substance. The inactive slurry of the blend mentioned under A and C oel and the slurry containing the surfactant of the blend mentioned under 3 are spray dried using a pressure nozzle and under normal conditions. Drying air inlet temperature is 25? to 3.2? ° C, its outlet temperature is 80 to 120 ° C and the nozzle pressure is 50 to 100 bar. Weight composition of slices is:

A

Acrylic-maleic copolymer 21.2

Zeolite A 30.3

Diethylenetriaminepentamethylenephosphonic acid 2,3

Brightener 1.0

Anionic surfactant 0.0

Humidity and various 45.0

7.6

41.2

1.1 0.3 9.6 4.0 0

0.0

5.3 n -n ^c J *

0.0

47.0

It can be seen from Figure 1 that in the range of shear rates of 1,000 to 10,000 s ¹ , the surfactant slurry of composition A of this example has a viscosity that is comparable to that of slurry B, which contains a surfactant and a large amount of detergent component. Spray drying of a mixture with a relatively small amount of zeolite using known pressure nozzles therefore does not present any problems.

It can be seen from Figure 1 that for a slurry of mixture C which contains no zeolite but a larger amount of polymer, the viscosity is higher, so that spray drying is impractical. Because of the good spray-drying properties, it is therefore necessary that the non-surfactant slurry has a minimum amount of detergent component.

Figure 2 shows the solubility of the non-surfactant spray dried powder made from Ä slurry, compared to the spray dried active powder made from slurry B, and the spray dried surfactant powder has a slightly slower dissolution rate resulting in less gel and fewer residues remain after discharge. In a comparative test using a Lannussi washing machine at a water feed rate of 2 liters per minute at 20 ° C, conventional spray-dried detergent detergents leave 30 to 90 / residue, while a granular detergent containing a surfactant inactive spray-dried powder and agglomerated the surfactant paste leaves an excess of less than 5 °.

The particle size distribution of the non-surfactant (spray-dried) powder is suitable for use in a detergent powder, the proportion remaining on the standard sieves being:

No. Eye width, / um

14 1180 3.1 / n C á. 850 3.7 / 36 425 18.8% 69 250 33,9 / 109 150 30.4%, 10.1% do not fall through the normal sieve 100. At spray dried products are required to have ms-

This avoids the crushing of the fine deterrent bit during storage and handling. The friability of the surface ineffective spray-dried powder is tested so that its proportion remaining in standard sieves no. 22 and 36 are poured into a ball mill in which they are ground for 5 minutes, and then the percentage that passes from the milled portion through a standard sieve 36 is determined. This amount makes 66.15% inactive spray powder, which is comparable to the friability powders prepared from slurry of composition B of this example.

Granular detergent powders formed by granulating a high active paste using most of the total amount of detergent component contained in the detergent powder and, when mixed with inactive spray dried powder and other ingredients, have. in many respects, laundering efficiency is less than that of some or all of the spray dried surfactants.

- 27 Example 9

This example 'he instrument that v.ysokohustotný grenulovaný provide extended detergent surfactant spray drying process inefficient slurry, then spraying the non-ionic surfactant to non-surfactant spray-dried slurry and mixing the resulting powder with a granulating ^one surface active alkoxylated and dry additives such as bleach and an enzyme.

The inactive inactive slurry is spray dried using a pressure of 50 to 100 bar in a pressure nozzle, the drying air having a temperature of 2> 0 to 320 ° C at the inlet and an outlet of 0 to 120 ° C at the outlet. The composition of the slurry is as follows in% by weight:

_fc Acrylomalein copolymer 9.8

Zeolite 44,7 * Ethylenetriaminepentamethylenephosphonic acid 1,7 Magnesium sulphate 1,8 Brightener 0,8 rgzne / vods 41,2

The spray-dried powder has a bulk density of 610 g / l. The non-ionic coating agent is sprayed onto the spray-dried powder with condensate of alkyl alcohol with ethylene oxide (AE). ingredients such as detersive ingredients, bleach and enzyme.

Ready-to-use detergent mix, having this weight composition density 80 µg / l. spray - dried powder 20 Ixionic surfactant 6 Surfactant powder made agglomeration 19 Eetergent component 17 Bleaching system 30 enzyme 3 Various board / water 5

^r rí

This example demonstrates that spray-drying a non-surfactant slurry containing a detergent component will obtain a powder having a relatively high absorption power for non-ionic surfactants compared to the absorbed droplet of the detergent component powder spray-dried. Therefore, more nonionic surfactant can be incorporated into the less detergent scrubber so that more powder of the detergent component is available to agglomerate the surfactant paste. This is contrary to the expectation that more efficient use of detergent powders can be achieved. ^and spray-drying the slices which contain very little or no amounts of the de-ergic powder at all and spraying the non-ionic surfactant but the resulting powder while adding dry detergent powders.

By spray-drying, a powder containing the following components in weight:

D E Acrylic-maleic copolymer 24.3 14.6 Z e o 1 i t A 53.0 66.3 Diethylenetriamine inpentamethylmonium acid. 4.2 2.5 Magnesium siren 4.4 2.7. brightener 2.9 M Cutting data ^ / water 14.3 12.3 The powder blends listed in L and E are spray with alcohol

containing 2? carbon atoms, ethoxylated with 3 moles of ethylene oxide per mole of alcohol (C1-EA) as nonionic surfactant.

If it is desired to produce a powder with good manageability, then additional zeolite A is added. The resulting powder of the compositions listed under D and E contains these components / in mass. ; & /: _{p P}

Spray-dried powder (kg) 9.9 15.1

The Keionic surfactant (C ^-EA) / K Zkg 5.9 5.9

Added zeolite A / kg / 11.3 9.99

Total 25.3 29.1

Total zeolite A / nonionic component ratio 3.2 2.90

Total dry powder / nonionic component ratio 4.1 3.0

7, said residual zeolite v / v / v / v / v

And it can be a tive paste or for dry mixing.

e mixture E requires less zeolite A, so to experience n3 agglomeration by surface and

Claims (11)

What is claimed is: 1. A process for the manufacture of a free-flowing, aranged detergent, comprising: a A. admixing an effective amount of an aqueous surfactant paste having a detergency of at least 40 &apos; with an effective amount of a dry detergent component or powder in a ratio of 0.05: 1 to 19: 1 to form a mixture, D. rapidly forming a uniform mixture in the form of substantially free-flowing particles from the initial mixture at 0 to 80 ° C, C. The uniform mixture is granulated into separate detergent granules using high speed mixing with a peripheral speed of 5 to 50 m / s, wherein the surfactant contains at least one anionic surfactant and optionally other surfactants. They are selected from the group of anionic, naionic, objacionic, ampholytic and cationic surfactants and mixtures thereof, and the mixing and granulation is performed simultaneously or immediately separately. ° C. I mean, Method according to claim 1, v y wit at JUC that is used for granulating the mixture yawns temperature 0 to 50 The method of claim 1, V V wit at JUC that is performed at peripheral j speed 15 to 40 peeling is 0.2 to 4 minutes. The method of claim 1, v y wit at JUC The composition of claim ¹ , wherein the surfactant paste and the dry detergent component or powder are used in a weight ratio of 0.1: 1 to 5: 1 s having a detergent efficiency of up to 95% and a viscosity of 10,000 to 10,000,000 cps. The method of claim 1, wherein the active paste and dry detergent ingredients or powders are used in a ratio of 0.15: 1 to 5: 1 and the paste has. a detergent activity of 50 to 60% and a viscosity of 10,000 to 7,000,000 cps, preferably 20,000 to 100,000 cps, wherein the DC active paste is used at an initial temperature of 60-60 ° C and a granulated temperature of 20-50 ° C; Separate grain-shaped detergent granules have an average particle size of 300 to 1200 microns with dried granules having a bulk density of 0.5 to 1.1 g / ml. - 30 The method of claim 1 or 5, wherein the ratio of dry detergent component or powder is 0.2: 1 to 0.5: 1 with the detergent activity active. the paste is 65 θ * 75 ó and the density of the granules is 0.7 to 0.9 g / ml. 7. A method according to claim 1, wherein the moisture of the separated granules is reduced by drying in a bed dryer in a moisture content of 1-8. SPO-8 process according to claim 1 to 5, characterized uj account _no. characterized in that the paste is added to the mixer / granulator by pumping or extrusion. 9. The method of claim 1. c i do by s? paste moisture will decrease between pumping and paste entry into the mixer / granulator by heating and instant evaporation. A method according to claim 9, characterized in that the paste is extruded by entering into a 4/ ^4- ml granules. no, no A method for producing a free-flowing detergent composition according to any one of the preceding claims, wherein the detergent composition comprises a total amount of a baby ingredient in the form of a powder, wherein the method number j comprises x-grades. L. spray-drying of aqueous slurry containing no surfactant and comprising part of the total amount of detergent powder to form a spray-dried powder, and E. combining the spray-dried powder with the granules obtained by the process of claims 1 to 10. 12. The method of claim 11, wherein the detergent powder is a zeolite. 13. A method according to claim 11 or 12, wherein the surfactant-free slurry contains 15 to 55% by weight detergent powder. The method according to any one of claims 11 to 13, characterized in that the nonionic surfactant is sprayed onto the spray-dried surfactant-free slurry before mixing with the detergent granules obtained by the process according to claims 1 to 14. 10th