EP1117759B1 - Granulation method - Google Patents

Abstract

Disclosed is a novel granulation method, wherein a surface active foam obtained by foaming a flowable component that contains a surface active agent with a gaseous medium is used as granulation adjuvant. The surface active foam has an average pore size of less than 10 mm.

Description

The present invention relates to a process for the preparation of surfactant granules. It relates in particular to a process which allows surfactant granules or surfactant-containing Components of detergent and cleaner compositions or complete Detergent and detergent compositions with no or reduced use to prepare spray drying steps.

Granular detergent compositions or components thereof are produced to a large extent by spray drying. When spray drying the ingredients such as surfactants, builders, etc. with about 35 to 50 wt .-% of water an aqueous slurry, the so-called slurry, mixed and in spray towers sputtered in a hot gas stream, wherein the detergent particles and detergent form. Both the equipment for this process and the implementation of the process are costly because most of the slurry water is evaporated in order to obtain particles with residual water contents around 5 to 10% by weight. moreover Although the granules produced by spray-drying usually have an excellent Solubility, but have only low bulk densities, resulting in higher packaging volumes as well as transport and storage capacities. Also, the flowability of spray-dried Granules are not optimal due to their irregular surface structure, which also affects their visual appearance. Spray drying method exhibit Another number of disadvantages, so that there was no lack of attempts, the Manufacture of detergents and cleaners completely without spray drying or at least the lowest possible levels of spray-drying products in the finished product to have.

For example, W. Hermann de Groot, I. Adami, GF Moretti "The Manufacture of Modern Detergents Powders", Hermann de Groot Academic Publisher, Wassenaar, 1995, page 102 ff. Describes various mixing and granulation processes for the production of detergents and cleaners. These methods have the commonality that premixed solids are granulated with the addition of the liquid ingredients and optionally post-dried.

Also in the patent literature there is a broad state of the art for non-tower manufacturing of detergents and cleaners. In particular to different apparatus, which are operated under varying conditions, to different Granulationshilfsmitteln and their application to presented in the mixer solids and Combinations of ingredients with physical conditions during granulation are to be kept, many publications can be found.

Thus, European Patent EP 642 576 (Henkel) describes a two-stage granulation in two successive mixers / granulators, wherein in a first, low-speed granulator 40-100 wt .-%, based on the total amount of the ingredients used, the solid and liquid components vorgranuliert and in a second, high-speed granulator, the pregranulate optionally mixed with the remaining ingredients and transferred into a granulate the following process parameters are met: granulation in the first mixer at peripheral speeds of the tools of 2-7 m / s over 0.5-10 min, in the second mixer at peripheral speeds of 8-35 m / s over 0.1-30 (0.5-2) s; Pre-granulate temperature when entering the second granulation stage 30-60 ° C.

According to the teaching of the European patent EP 560 802 (Henkel) surfactant-containing zeolite granules having bulk densities of 750 to 1000 g / l can be prepared by using as granulating a mixture of water, surfactants and (co) polymeric carboxylates, wherein the content the granulating liquid to surfactants at least 10 wt .-% is. The feeding of the granulation takes place according to the teaching of this document by a spray nozzle.

European patent application EP-A-0 402 111 (Procter & Gamble) discloses a granulation process for the preparation of surfactant granules in which surfactants, water and optionally fine powders are mixed to form a dough which is prepared by adding a deagglomerating agent Powder) is granulated in a high speed mixer.

European Patent Application EP-A-0 508 543 (Procter & Gamble) discloses a process in which a surfactant acid is neutralized with an excess of alkali to form an at least 40 wt% surfactant paste, which is subsequently conditioned and granulated, with a Direct cooling with dry ice or liquid nitrogen takes place.

Surfactant mixtures which are subsequently sprayed onto solid absorbents and which provide detergent compositions or components therefor are also described in EP 265 203 (Unilever). The liquid surfactant mixtures disclosed in this document contain sodium or potassium salts of alkylbenzenesulfonic acids or alkylsulfuric acids in amounts of up to 80% by weight, ethoxylated nonionic surfactants in amounts of up to 80% by weight and at most 10% by weight of water.

Similar surfactant mixtures are also disclosed in the older EP 211 493 (Unilever). According to the teaching of this document, the surfactant mixtures to be sprayed contain between 40 and 92% by weight of a surfactant mixture and more than 8 to at most 60% by weight of water. The surfactant mixture is in turn at least 50% of polyalkoxylated nonionic surfactants and ionic surfactants.

In the European patent EP 772 674 (Henkel KGaA) describes a process for the preparation of surfactant granules by spray drying, the anionic acid (s) and highly concentrated alkaline solutions separately charged with a gaseous medium and mixed in a multi-fluid nozzle, neutralized and by spraying in a Hot gas stream are spray-dried. The finely divided surfactant particles thus obtained are then agglomerated in a mixer to form granules having bulk densities above 400 g / l.

The German patent application DE-A-4304062 (Henkel KGaA) discloses a granulation process in which an anionic surfactant in its acid form or a mixture of several anionic surfactants in acid form in which an aqueous alkaline solution separately with a gaseous medium are applied. Subsequently, these preparation forms are sprayed into a granulation and granulated with a solid.

It is an object of the present invention to provide a method which it allows surfactant granules for detergents and cleaners with or without reduced Use of spray drying steps produce. The procedure to be provided should be universally applicable and regarding the usable solids and Granulicrflüssigkeiten be subject to no restrictions, the disadvantage of energy-consuming evaporation of water but largely avoided.

The solution of these different tasks succeeds in a mixing and granulation process, in which a surfactant-containing flowable component by application of a gaseous medium is foamed to a foam, which as Granulierhilfsmittel serves. The invention thus relates to a process for the preparation of surfactant granules, in which a surfactant-containing flowable component with a gaseous Medium is applied, wherein the surfactant-containing flowable component through the foamed gaseous medium and the resulting surfactant-containing foam below is added to a charged in a mixer solid bed.

The process of the invention has compared to the use of conventional Granulating liquids considerable advantages. Through the use of a "granulating foam" Instead of conventional Granulierflüssigkeiten is a much more homogeneous Liquid distribution on the solid bed reached. The particles of the bed of solids become wets better and it is less granulating liquid to form the total Granules needed, so that can be dispensed with subsequent drying steps. Another advantage is the more homogeneous particle size distribution of the resulting granules, because of the use of granulating foam overagglomeration and training is avoided by lumps. In addition, dust and fines become more effective bound so that the yields of granules in the desired particle size range (about 400 to 1600 microns) compared to conventional liquid granulation significantly improved become. In contrast to conventional granulation with granulating liquids, which atomises or must be sprayed, the inventive method also allows the Use of significantly more viscous granulating liquids without procedural problems. Details will be given below. The term "flowable" in the context of the present application, components which have a measurable viscosity have, ie without outer containers are not dimensionally stable and cut resistant. "Flowable" in the sense of the present application are therefore in particular liquids with viscosities below 20000 mPas.

The term "foam" used in the context of the present invention denotes Structures of gas-filled, spherical or polyhedron-shaped cells (pores), which by liquid, semi-liquid or highly viscous cell webs are limited.

When the volume concentration of the gas forming the foam is more homodisperse Distribution is less than 74%, so are the gas bubbles because of the surface-reducing Effect of interfacial tension spherical. Above the limit of the densest sphere packing the bubbles are deformed into polyhedral lamellae of about 4-600 be limited to thin skins. The cell bridges, connected via so-called nodal points, form a coherent framework. Between the cell ridges tension the Foam lamellae (closed-cell foam). Are the foam lamellae destroyed or If they flow back into the cell ridges at the end of foaming, you get an open-celled one Foam. Foams are thermodynamically unstable, because by reduction of the surface Surface energy can be recovered. The stability and thus the existence The foams of the invention is thus dependent on how far they succeed in their self-destruction to prevent.

To generate the foam, the gaseous medium in the surfactant-containing flowable Component is blown in, or the foaming is achieved by intensive beating, Shaking, splashing or stirring the liquid in the gas atmosphere concerned. Due to the lighter and better controllable and feasible foaming is in According to the present invention, the generation of foam by the injection of the gaseous Medium ("fumigation") over the other variants clearly preferred. The gassing takes place depending on the desired process variant continuously or discontinuously over perforated plates, sintered disks, sieve inserts, Venturi nozzles or others usual systems.

As a gaseous medium for foaming, any gases or gas mixtures be used. Examples of gases used in the art are nitrogen, oxygen, Noble gases and noble gas mixtures such as helium, neon, argon and their Mixtures, carbon dioxide, etc. For cost reasons, the inventive method preferably carried out with air as the gaseous medium. When the frothing up Components are stable to oxidation, the gaseous medium can also be wholly or partially made of ozone, causing oxidatively destructible impurities or discoloration eliminated in the foaming surfactant-containing flowable components or a germ attack of these components can be prevented.

The inventive method includes the independent sub-steps of Production of foam from a surfactant-containing flowable component and the subsequent Addition to a moving in a mixer solid bed, the foam as Granulation aid is used. The ingredients of the surfactant-containing produced in the first sub-step Foams are described below.

The surfactant-containing flowable component contains surfactants from the Group of anionic, nonionic, zwitterionic or cationic surfactants, wherein anionic surfactants for economic reasons and because of their power spectrum are clearly preferred. The content of the flowable surfactant-containing component Surfactant (s) can vary within wide limits. According to the invention are methods preferred in which the surfactant-containing flowable component one or more surfactants from the group of anionic and / or nonionic and / or cationic and / or amphoteric surfactants in amounts of 20 to 100 wt .-%, preferably from 50 to 95 wt .-% and in particular from 60 to 90 wt .-%, each based on the surfactant-containing Component containing. As mentioned above, process variants according to the invention are preferred in which the surfactant-containing flowable component anionic (s) surfactant (s) in amounts of 10 to 90 wt .-%, preferably from 20 to 85 wt .-% and in particular from 30 to 80 wt .-%, each based on the surfactant-containing component.

As anionic surfactants, for example, those of the sulfonate type and sulfates are used. The surfactants of the sulfonate type are preferably C _9-13 -alkylbenzenesulfonates, olefinsulfonates, ie mixtures of alkene and hydroxyalkanesulfonates and disulfonates, as are obtained, for example, from C _12-18 -monoolefins having terminal or internal double bonds by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acid hydrolysis of the sulfonation products into consideration. Also suitable are alkanesulfonates which are obtained from C _12-18 alkanes, for example by sulfochlorination or sulfoxidation with subsequent hydrolysis or neutralization. Likewise, the esters of α-sulfo fatty acids (estersulfonatec), for example the α-sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids are also suitable. According to the invention, preference is given to processes in which the surfactant-containing flowable component comprises alkali metal salts of alkylbenzenesulfonic acids in amounts of from 20 to 90% by weight, preferably from 30 to 85% by weight and in particular from 40 to 80% by weight, based in each case on the surfactant Component containing.

Further suitable anionic surfactants are sulfated fatty acid glycerol esters. Among fatty acid glycerol esters are the mono-, di- and triesters and their mixtures to understand, as with the preparation by esterification of a monoglycerol with 1 to 3 mol fatty acid or obtained in the transesterification of triglycerides with 0.3 to 2 moles of glycerol. preferred Sulfated fatty acid glycerol esters are the sulfonation products of saturated fatty acids with 6 to 22 carbon atoms, for example caproic acid, caprylic acid, capric acid, Myristic, lauric, palmitic, stearic or behenic acid.

Alk (en) ylsulfates are the alkali metal salts and in particular the sodium salts of the sulfuric monoesters of C ₁₂ -C ₁₈ fatty alcohols, for example coconut fatty alcohol, tallow fatty alcohol, lauryl, myristyl, cetyl or stearyl alcohol or the C ₁₀ -C ₂₀ oxo alcohols and those half-esters of secondary alcohols of these chain lengths are preferred. Also preferred are alk (en) ylsulfates of said chain length, which contain a synthetic, produced on a petrochemical basis straight-chain alkyl radical, which have an analog environmental compatibility as the adequate compounds based on oleochemical raw materials. Of washing technology interest, the C ₁₂ -C ₁₆ alkyl sulfates and C ₁₂ -C ₁₅ alkyl sulfates and C ₁₄ -C ₁₅ alkyl sulfates are preferred. Also, 2,3-alkyl sulfates, which are prepared, for example, according to US Pat . Nos . 3,234,258 or 5,075,041 and can be obtained as commercial products of the Shell Oil Company under the name DAN®, are suitable anionic surfactants.

The sulfuric acid monoesters of straight-chain or branched C _7-21 -alcohols ethoxylated with from 1 to 6 mol of ethylene oxide, such as 2-methyl-branched C _9-11- alcohols having on average 3.5 mol of ethylene oxide (EO) or C _12-18 . Fatty alcohols with 1 to 4 EO are suitable. Due to their high foaming behavior, they are only used in detergents in relatively small amounts, for example in amounts of from 1 to 5% by weight.

Further suitable anionic surfactants are also the salts of alkylsulfosuccinic acid, which are also referred to as sulfosuccinates or as sulfosuccinic acid esters and the monoesters and / or diesters of sulfosuccinic acid with alcohols, preferably fatty alcohols and in particular ethoxylated fatty alcohols. Preferred sulfosuccinates contain C _8-18 fatty alcohol residues or mixtures of these. Particularly preferred sulfosuccinates contain a fatty alcohol residue derived from ethoxylated fatty alcohols, which in themselves constitute nonionic surfactants (see description below). Sulfosuccinates, whose fatty alcohol residues are derived from ethoxylated fatty alcohols with a narrow homolog distribution, are again particularly preferred. Likewise, it is also possible to use alk (en) ylsuccinic acid having preferably 8 to 18 carbon atoms in the alk (en) yl chain or salts thereof.

As further anionic surfactants are particularly soaps into consideration. Are suitable saturated fatty acid soaps, such as the salts of lauric acid, myristic acid, palmitic acid, Stearic acid, hydrogenated erucic acid and behenic acid and in particular from natural Fatty acids, e.g. Coconut, palm kernel or tallow fatty acids, derived soap mixtures.

The anionic surfactants including soaps may be in the form of their sodium, potassium or ammonium salts and as soluble salts of organic bases, such as mono-, di- or Triethanolamine. Preferably, the anionic surfactants are in the form of their Sodium or potassium salts, especially in the form of the sodium salts.

When selecting the anionic surfactants used in the detergent tablets according to the invention are used, the freedom of formulation are none to be observed in the way. In preferred process variants has however, the surfactant-containing component has a soap content of 0.2% by weight on the total weight of the resulting granules. In particularly preferred Process contains the surfactant-containing flowable component in addition soaps in quantities from 1 to 30 wt .-%, preferably from 2 to 25 wt .-% and in particular from 5 to 20 Wt .-%, each based on the surfactant-containing component.

Preferred anionic surfactants are generally the alkylbenzenesulfonates and Fatty alcohol sulfates, with preferred surfactant granules more than 5 wt .-%, preferably more than 15% by weight and in particular more than 25% by weight of alkylbenzenesulfonate (s) and / or fatty alcohol sulfate (s), in each case based on the granule weight

In addition to anionic surfactants, nonionic surfactants are the most important surfactants Links. In addition to anionic surfactants or in their place, the surfactant-containing flowable component nonionic (s) surfactant (s), wherein method are preferred in which the surfactant-containing flowable component nonionic (s) Surfactant (s) in amounts of 1 to 100 wt .-%, preferably from 2 to 70 wt .-% and in particular from 5 to 30 wt .-%, each based on the surfactant-containing component.

The nonionic surfactants used are preferably alkoxylated, advantageously ethoxylated, in particular primary, alcohols having preferably 8 to 18 carbon atoms and on average 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, in which the alcohol radical can be linear or preferably methyl-branched in the 2-position or linear and methyl-branched radicals in the mixture can contain, as they are usually present in Oxoalkoholresten. In particular, however, alcohol ethoxylates with linear radicals of alcohols of natural origin having 12 to 18 carbon atoms, for example of coconut, palm, tallow or oleyl alcohol, and on average 2 to 8 EO per mole of alcohol are preferred. The preferred ethoxylated alcohols include, for example, C _12-14 alcohols with 3 EO or 4 EO, C _9-11 alcohols with 7 EO, C _13-15 alcohols with 3 EO, 5 EO, 7 EO or 8 EO, C _12-18 alcohols with 3 EO, 5 EO or 7 EO and mixtures of these, such as mixtures of C _12-14 -alcohol with 3 EO and C _12-18 -alcohol with 5 EO. The degrees of ethoxylation given represent statistical means which, for a particular product, may be an integer or a fractional number. Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NRE). In addition to these nonionic surfactants, fatty alcohols with more than 12 EO can also be used. Examples include tallow fatty alcohol with 14 EO, 25 EO, 30 EO or 40 EO.

The use of alkoxylated nonionic surfactants is preferred in the context of the present invention. Process variants in which the surfactant-containing flowable component alkoxylated, preferably ethoxylated nonionic surfactants in amounts of 20 to 90 wt .-%, preferably from 30 to 85 wt .-% and in particular from 40 to 80 wt .-%, each based on the surfactant-containing Component contains, in this case have advantages, wherein processes are particularly preferred in which the surfactant-containing flowable component as ethoxylated nonionic surfactants, the reaction products of C _8-22 fatty alcohols, preferably C _12-20 fatty alcohols and in particular C _14-18 fatty alcohols with from 1 to 30 mol of ethylene oxide, preferably from 2 to 20 mol of ethylene oxide and in particular from 5 to 10 mol of ethylene oxide, in amounts of from 10 to 80% by weight, preferably from 20 to 75% by weight and in particular from 30 to 70% by weight. %, in each case based on the surfactant-containing component contains.

Another class of preferred nonionic surfactants used either as the sole nonionic surfactant or in combination with other nonionic surfactants are alkoxylated, preferably ethoxylated or ethoxylated and propoxylated fatty acid alkyl esters, preferably having from 1 to 4 carbon atoms in the alkyl chain, especially fatty acid methyl esters as they are for example, in Japanese Patent Application JP 58/217598 , or which are preferably prepared according to the method described in International Patent Application WO-A-90/13533 .

Another class of nonionic surfactants that can be used to advantage are the alkyl polyglycosides (APG). Usable Alkypolyglycoside meet the general formula RO (G) _z , in which R is a linear or branched, especially in the 2-position methyl branched, saturated or unsaturated, aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms and G is the Is a symbol which represents a glycose unit having 5 or 6 C atoms, preferably glucose. The degree of glycosidation z is between 1.0 and 4.0, preferably between 1.0 and 2.0 and in particular between 1.1 and 1.5.

Preference is given to using linear alkyl polyglucosides, ie alkyl polyglycosides in which the polyglycosyl radical is a glucose radical and the alkyl radical is an n-alkyl radical.

The surfactant granules according to the invention may preferably contain alkylpolyglycosides, wherein contents of the granules of APG exceed 0.2% by weight, based on the total granules, are preferred. Particularly preferred surfactant granules contain APG in amounts of 0.2 to 10 wt .-%, preferably 0.2 to 5 wt .-% and in particular from 0.5 to 3 wt .-%.

Nonionic surfactants of the amine oxide type, for example N-cocoalkyl-N, N-dimethylamine oxide and N-tallow alkyl-N, N-dihydroxyethylamine oxide, and the fatty acid alkanolamide may be suitable. The amount of these nonionic surfactants is preferably not more than that of ethoxylated fatty alcohols, in particular not more than half of it.

in der RCO für einen aliphatischen Acylrest mit 6 bis 22 Kohlenstoffatomen, R¹ für Wasserstoff, einen Alkyl- oder Hydroxyalkylrest mit 1 bis 4 Kohlenstoffatomen und [Z] für einen linearen oder verzweigten Polyhydroxyalkylrest mit 3 bis 10 Kohlenstoffatomen und 3 bis 10 Hydroxylgruppen steht. Bei den Polyhydroxyfettsäureamiden handelt es sich um bekannte Stoffe, die üblicherweise durch reduktive Aminierung eines reduzierenden Zukkers mit Ammoniak, einem Alkylamin oder einem Alkanolamin und nachfolgende Acylierung mit einer Fettsäure, einem Fettsäurealkylester oder einem Fettsäurechlorid erhalten werden können. Further suitable surfactants are polyhydroxy fatty acid amides of the formula (I)

wherein RCO is an aliphatic acyl group having 6 to 22 carbon atoms, R ^{1 is} hydrogen, an alkyl or hydroxyalkyl group having 1 to 4 carbon atoms and [Z] is a linear or branched polyhydroxyalkyl group having 3 to 10 carbon atoms and 3 to 10 hydroxyl groups. The polyhydroxy fatty acid amides are known substances which can usually be obtained by reductive amination of a reducing sugar with ammonia, an alkylamine or an alkanolamine and subsequent acylation with a fatty acid, a fatty acid alkyl ester or a fatty acid chloride.

in der R für einen linearen oder verzweigten Alkyl- oder Alkenylrest mit 7 bis 12 Kohlenstoffatomen, R¹ für einen linearen, verzweigten oder cyclischen Alkylrest oder einen Arylrest mit 2 bis 8 Kohlenstoffatomen und R² für einen linearen, verzweigten oder cyclischen Alkylrest oder einen Arylrest oder einen Oxy-Alkylrest mit 1 bis 8 Kohlenstoffatomen steht, wobei C_1-4-Alkyl- oder Phenylreste bevorzugt sind und [Z] für einen linearen Polyhydroxyalkylrest steht, dessen Alkylkette mit mindestens zwei Hydroxylgruppen substituiert ist, oder alkoxylierte, vorzugsweise ethoxylierte oder propoxylierte Derivate dieses Restes.The group of polyhydroxy fatty acid amides also includes compounds of the formula (II)

in the R is a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms, R ^{1 is} a linear, branched or cyclic alkyl radical or an aryl radical having 2 to 8 carbon atoms and R ^{2 is} a linear, branched or cyclic alkyl radical or an aryl radical or an oxyalkyl radical having 1 to 8 carbon atoms, with C _1-4 alkyl or phenyl radicals being preferred and [Z] being a linear polyhydroxyalkyl radical whose alkyl chain is substituted by at least two hydroxyl groups, or alkoxylated, preferably ethoxylated or propoxylated Derivatives of this residue.

[Z] is preferably obtained by reductive amination of a reduced sugar, for example glucose, fructose, maltose, lactose, galactose, mannose or xylose. The N-alkoxy- or N-aryloxy-substituted compounds can then be converted into the desired polyhydroxy fatty acid amides, for example according to the teaching of the international application WO-A-95/07331, by reaction with fatty acid methyl esters in the presence of an alkoxide as catalyst.

The surfactant-containing flowable component according to the invention completely from a or more surfactants and thus be free of non-surfactant compounds. It is according to the invention but also possible, other ingredients of detergents and cleaners to incorporate into the surfactant-containing component. In addition to active and Active substances, the surfactant-containing component may also contain water due to the production process, this water being used for setting advantageous viscosity values or for optimization the foaming process of the surfactant-containing component also be added can. In preferred processes, however, the surfactant-containing flowable component contains less than 20% by weight, preferably less than 15% by weight, and in particular less than 10 wt .-% water, in each case based on the surfactant-containing component.

In particular, so-called "small components" can according to the inventive method advantageous over the serving as granulating foam in the surfactant granules be introduced. In preferred processes according to the invention, the surfactant-containing flowable component further ingredients of detergents and cleaners, in particular substances from the group of complexing agents, polymers, optical brighteners, Dyes and fragrances and alkalis. This preferably the surfactant-containing flowable component to be added small components are described below.

The foaming of the flowable surfactant-containing component can be as desired Properties of the foam at room temperature or under cooling or heating respectively. Preferred process variants are carried out so that the foamed surfactant-containing flowable component before foaming temperatures of 20 to 120 ° C, preferably from 30 to 90 ° C and in particular from 50 to 75 ° C, having. By selecting the ingredients, the viscosity of the surfactant-containing component in wide limits are varied, with less liquid surfactant-containing components in the Usually deliver less stable foams.

As already mentioned above, it is an advantage of the method according to the invention that in Contrary to conventional granulation also Granulierflüssigkeiten used can be, whose viscosity is high. Thus, in the method according to the invention surfactant-containing liquid components whose viscosity is above 100 mPas is, but also liquid components with viscosities over 1000 mPas, even more than 5000 mPas, can be foamed according to the invention and in the form of "granulating foam" easy to use as Granulationshilfsmittel. The invention is interesting Method especially when two liquid components are used whose mixture would have too high a viscosity, or when mixed Form gel phases. Here, according to the invention, a surfactant-containing liquid component foamed and this foam with that of another liquid component produced foam are combined, which then serves as granulating foam. It is not imperative that the second liquid component is surfactant, for the sake of However, foam stability may be preferred. The problem of one for the fine-pored foaming Too high viscosity entire mixture is thereby elegantly bypassed.

The flowable surfactant-containing component is through the gaseous medium to a Foamed foam, wherein liquid and gaseous medium in varying amounts or ratios to each other can be used. From process engineering It is preferred, for the production of foam, the gaseous medium in each case in quantities of at least 20% by volume, based on the amount of liquid to be foamed.

If, for example, one liter of a surfactant-containing component is to be foamed, Preferably, at least 200 ml of gaseous medium are used for foaming. In preferred methods, the amount of gaseous medium is significantly higher this value, so that methods are preferred in which the used for foaming Gas quantity one to three hundred times, preferably five to two hundred times and in particular ten to one hundred times the volume of the foaming Amount of fluid. As already mentioned above, is called gaseous medium in this case preferably used air. But it is also possible other gases or Use gas mixtures for foaming. For example, it may be preferable to air or passing oxygenated air through an ozonizer before passing the gas to the Foaming is used. In this way one can produce gas mixtures which For example, 0.1 to 4 wt .-% ozone. The ozone content of the foaming gas then leads to the oxidative destruction of undesirable components in the foaming Liquids. In particular, in the case of partially discolored anionic surfactant acids, the Blend of ozone can be achieved a significant brightening.

For foaming the above exemplarily quoted liter of the surfactant-containing component Thus, preferably 1 to 300 liters, preferably 5 to 200 liters and in particular 10 used up to 100 liters of air.

By way of the temperature of the liquid to be foamed on the one hand and the temperature of the gaseous medium on the other hand, the temperature of the resulting foam can be controlled. In preferred variants of the process according to the invention, the resulting foam has temperatures below 115 ° C., preferably between 20 and 80 ° C. and in particular between 30 and 70 ° C. The resulting foam, which is used in the next process step as Granulationshilfsmittel can be characterized by other physical parameters. For example, it is preferred that the foam has a density below 0.80 gcm ^-3 , preferably from 0.10 to 0.6 gcm ^-3 and especially from 0.30 to 0.55 gcm ^-3 . It is further preferred that the foam has average pore sizes below 10 mm, preferably below 5 mm and in particular below 2 mm.

The mentioned physical parameters of temperature, density and mean pore size characterize the foam at the time of its formation. Preferably However, the process is chosen so that the foam the criteria mentioned even when added to the mixer met.

This procedural guides are possible in which the foam only one or two of the met criteria mentioned in the addition to the mixer, but are both preferred the temperature, as well as the density and the pore size in said areas, though the foam gets into the mixer.

The foam is after its formation on a submitted in a mixer solid bed given there and serves as Granulationshilfsmittel. This process step can be found in the a variety of mixing and granulating be performed, as farther is described in detail below. The solid bed submitted in the mixer can thereby All substances used in detergents and cleaners contain. In this way can be prepared by the process according to the invention finished washing and cleaning agents become. Usually, however, certain ingredients of detergents and cleaners not granulated to avoid unwanted reactions of these constituents under the mechanical action of the granulating tools. Ingredients which are usually only subsequently added to the resulting surfactant granules, i. in the Following granulation are bleaches, Bleach activators, enzymes and foam inhibitors.

It is preferred that the surfactant granules prepared according to the invention are present in addition to the surfactant Contain substances which in the later detergents and cleaners as active substances act. In preferred processes, the solid bed provided in the mixer therefore contains one or more substances from the group of builders, in particular the alkali metal carbonates, sulfates and silicates, zeolites and polymers.

In addition to the washing-active substances, builders are the most important ingredients of Detergents and cleaners. In the process according to the invention, all can usually be used builders used in detergents and cleaners in a solid bed zeolites, silicates, carbonates, organic co-builders and if there are no environmental concerns about their use - even the phosphates.

Suitable crystalline layered sodium silicates have the general formula NaMSi _x O _{2x + 1} .H ₂ O, where M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20 and preferred values for x 2, 3 or 4 are. Such crystalline sheet silicates are described, for example, in European Patent Application EP-A-0 164 514 . Preferred crystalline layered silicates of the formula given are those in which M is sodium and x assumes the values 2 or 3. In particular, both β- and δ-sodium disilicates Na ₂ Si ₂ O ₅ .yH ₂ O are preferred, whereby β-sodium disilicate can be obtained, for example, by the process described in international patent application WO-A-91/08171 .

It is also possible to use amorphous sodium silicates with a Na ₂ O: SiO ₂ modulus of from 1: 2 to 1: 3.3, preferably from 1: 2 to 1: 2.8 and in particular from 1: 2 to 1: 2.6, which Delayed and have secondary washing properties. The dissolution delay compared with conventional amorphous sodium silicates may have been caused in various ways, for example by surface treatment, compounding, compaction / densification or by overdrying. In the context of this invention, the term "amorphous" is also understood to mean "X-ray amorphous". This means that the silicates do not yield sharp X-ray reflections typical of crystalline substances in X-ray diffraction experiments, but at most one or more maxima of the scattered X-rays having a width of several degrees of diffraction angle. However, it may well even lead to particularly good builder properties if the silicate particles provide blurred or even sharp diffraction maxima in electron diffraction experiments. This is to be interpreted as meaning that the products have microcrystalline regions of size 10 to a few hundred nm, values of up to max. 50 nm and in particular up to max. 20 nm are preferred. Such so-called X-ray-amorphous silicates, which likewise have a dissolution delay compared to the conventional water glasses, are described, for example, in German patent application DE-A-44 00 024 . Particularly preferred are compacted / compacted amorphous silicates, compounded amorphous silicates and overdried X-ray amorphous silicates.

The finely crystalline, synthetic and bound water-containing zeolite used is preferably zeolite A and / or P. As zeolite P, zeolite MAP® (commercial product from Crosfield) is particularly preferred. Also suitable, however, are zeolite X and mixtures of A, X and / or P. Commercially available and preferably usable in the context of the present invention is, for example, a cocrystal of zeolite X and zeolite A (about 80% by weight of zeolite X) ), which is sold by the company CONDEA Augusta SpA under the brand name VEGOBOND AX® and by the formula n Na ₂ ^O. (1-n) K ₂ ^O. Al ₂ O ₃ ^. (2 - 2.5) SiO ₂ ^. (3.5-5.5) H ₂ O can be described. Suitable zeolites have an average particle size of less than 10 μm (volume distribution, measuring method: Coulter Counter) and preferably contain 18 to 22% by weight, in particular 20 to 22% by weight, of bound water.

Of course, a use of the well-known phosphates as builders possible, unless such use is avoided for environmental reasons should be. Particularly suitable are the sodium salts of orthophosphates, pyrophosphates and in particular the tripolyphosphates.

Useful organic builders are, for example, those in the form of their sodium salts usable polycarboxylic acids, such as citric acid, adipic acid, succinic acid, Glutaric acid, tartaric acid, sugar acids, aminocarboxylic acids, nitrilotriacetic acid (NTA), if such an operation is not objectionable for ecological reasons, as well as Mixtures of these. Preferred salts are the salts of polycarboxylic acids such as citric acid, Adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids and mixtures from these.

The solid bed submitted in the mixer may also contain compounded raw materials, i.e. Ingredients that themselves are process end product of previous process steps. Next granulated, compacted or extruded raw materials are spray-dried Base powder as part of the submitted in the mixer bed of solids on. This spray-dried Base powders may be surfactant-free (for example polymer compounds), but preferably contain surfactants. If such spray-dried base powder used be so contains the submitted in the mixer solid bed based on those in the mixer submitted solids in preferred process variants, the spray-dried Base powder, preferably the surfactant-containing spray-dried base powder, in quantities from 10 to 80% by weight, preferably from 15 to 70% by weight and especially from 20 to 60% by weight.

By adding the foam and under the action of the mixer tools is a Surfactant granules formed. In this case, methods according to the invention are preferred in which the Surfactant foam in the weight ratio foam: solid from 1: 100 to 9: 1, preferably from 1:30 to 2: 1 and especially from 1:20 to 1: 1, to the solid bed charged in the mixer is given. In the preferred amounts of granulation (surfactant) optimal granulation results are achieved.

As already mentioned, the process of the invention can be used in a variety of common Perform mixing and granulating devices. For carrying out the invention Suitable mixers are, for example, Eirich® mixers of the R series or RV (trademark of Maschinenfabrik Gustav Eirich, Hardheim), the Schugi® Flexomix, the Fukae® FS-G blenders (trademarks of Fukae Powtech, Kogyo Co., Japan), the Lödige® FM, KM and CB mixers (trademark of Lödige Maschinenbau GmbH, Paderbom) or the Drais® series T or K-T (trademark of Drais-Werke GmbH, Mannheim). Some preferred embodiments of the invention Method will be described below.

For example, it is possible and preferred that the inventive method in a low-speed mixer / granulator at peripheral speeds of the tools of 2 m / s to 7 m / s, wherein the surfactant-containing foam in a time between 0.5 and 10 minutes, preferably between 1 and 7 minutes and especially between 2 and 5 minutes, is added to the solid bed provided in the mixer.

Alternatively, in preferred process variants of the surfactant-containing foam in a high-speed mixer / granulator at peripheral speeds of 8 m / s to 35 m / s in a time between 0.1 and 30 seconds, preferably up to 10 seconds and in particular between 0.5 and 2 seconds, are added to the solid bed submitted in the mixer.

While the two process variants described above use each describe a mixer, it is also possible according to the invention, two mixers with each other to combine. For example, methods are preferred in which the surfactant-containing Foam in a first, low-speed mixer / granulator on a moving solid bed is given, wherein 40 to 100 wt .-%, based on the total amount of the used Ingredients that pre-granulate solid and liquid ingredients and in one second, high-speed mixer / granulator the pregranulate from the first stage of the process optionally mixed with the remaining solid and / or liquid components and in a granulate is transferred. In this process variant, the surfactant-containing foam in the first mixer / granulator placed on a solid bed and the mixture pre-granulated. The composition of the foam and the solid bed presented in the first mixer are chosen so that 40 to 100 wt .-%, preferably 50 to 90 wt .-% and in particular 60 to 80 wt .-%, of the solid and liquid components, based on the Total amount of ingredients used, are in the "pre-granules". This "Vorgranulat" is now mixed in the second mixer with other solids and under Granulated addition of further liquid components to the finished surfactant granules. in this connection it is possible and preferred according to the invention, that in the second step, the Liquid ingredients are not aufgesüst as a liquid, but in the form of a Foam serve as Granulationshilfsmittel ("granulation"). The composition The foam that is added to the second mixer may depend on the composition of the foam used in the first mixer, so that above described method are preferred in which in the second, high-speed mixer / granulator the pregranulate from the first stage of the process also with addition a surfactant-containing foam, the composition of which in the first process stage used foam, is granulated to the finished granules.

The said order of low-speed high-speed mixer can according to the invention be reversed, so that a method according to the invention results, in which the surfactant-containing foam in a first, high-speed mixer / granulator aufein moved Solid bed is given, wherein 40 to 100 wt .-%, based on the total amount of ingredients that pre-granulate solid and liquid ingredients and all in one second, low-speed mixer / granulator the pregranulate from the first stage of the process optionally mixed with the remaining solid and / or liquid components and transferred to a granule.

In this process variant, what has been said above is to be applied analogously, so that here too Methods are preferred in which in the second, low-speed mixer / granulator Pre-granulate from the first stage also with the addition of a surfactant-containing Foam, the composition of which is used in the first stage of the process Foam may differ, is granulated to the finished granules.

All the above-described embodiment variants of the method according to the invention can be carried out batchwise or continuously. In the above described embodiments of the method according to the invention are for Part used high-speed mixer / granulators. It is within the scope of the present Invention particularly preferred that uses a mixer as a high-speed mixer is having both a mixing and a crushing device, wherein the Mixing shaft at rotational speeds of 50 to 150 revolutions / minute, preferably from 60 to 80 revolutions / minute and the shaft of the comminution device at rotational speeds of 500 to 5000 revolutions / minute, preferably from 1000 to 300 revolutions / minute.

The method according to the invention is with regard to the selection of the ingredients to be used and their concentration can be varied over a wide range. Nevertheless, it is it is preferred, when according to the invention surfactant granules are prepared, the surfactant contents above 10% by weight, preferably above 15% by weight and in particular above 20 wt .-%, each based on the granules, and bulk densities above 600 g / l, preferably above 700 g / l and in particular above 800 g / l.

The granulation process according to the invention can be carried out in such a way that particles predetermined size distribution result. Here are methods of the invention in which the surfactant granules have a particle size distribution in which at least 50% by weight, preferably at least 60% by weight, in particular at least 70 wt .-% of the particles have sizes in the range of 400 to 1600 microns. Also the Residual moisture content of the surfactant granules according to the invention can be determined by the Selection of raw materials are predetermined so that subsequent drying steps can be waived. In preferred processes, the surfactant granules have residual contents in free water from 2 to 15 wt .-%, preferably from 4 to 10 wt .-%, based on the surfactant granules, on. The residual content of free water can, for example, by means of a modified UX method (Sartorius MA 30, program 120 ° C over 10 minutes) be determined.

It is possible by the process according to the invention, components for washing and To produce detergent, which only after mixing with other ingredients give the finished detergent and cleaning agent. Of course, according to the invention but also surfactant granules are produced, which in itself already a finished washing and cleaning agent (for example a textile color detergent) are.

The surfactant granules produced by the process according to the invention can be described below with other ingredients of detergents and cleaners to the finished product be mixed. If appropriate, however, these ingredients can also be passed over the solid bed or be incorporated directly into the surfactant granules via the surfactant foam and are described below:

In addition to the constituents surfactant and builders, especially in detergents and detergents conventional ingredients from the group of bleaches, bleach activators, Enzymes, pH adjusters, fragrances, perfume carriers, fluorescers, dyes, Foam inhibitors, silicone oils, anti redeposition agents, optical brighteners, grayness inhibitors, Color transfer inhibitors and corrosion inhibitors of importance.

Among the compounds serving as bleaches in water H ₂ O ₂ , sodium perborate tetrahydrate and sodium perborate monohydrate are of particular importance. Other useful bleaching agents are, for example, sodium percarbonate, peroxypyrophosphates, citrate perhydrates and H ₂ O ₂ -producing peracidic salts or peracids, such as perbenzoates, peroxophthalates, diperazelaic acid, phthaloiminoperacid or diperdodecanedioic acid. Typical organic bleaches are the diacyl peroxides such as dibenzoyl peroxide. Other typical organic bleaches are the peroxyacids, examples of which include the alkyl peroxyacids and the aryl peroxyacids. Preferred representatives are (a) the peroxybenzoic acid and its ring-substituted derivatives, such as alkylperoxybenzoic acids, but also peroxy-α-naphthoic acid and magnesium monoperphthalate, (b) the aliphatic or substituted aliphatic peroxyacids, such as peroxylauric acid, peroxystearic acid, ε-phthalimidoperoxycaproic acid [phthaloiminoperoxyhexanoic acid (PAP )], o-carboxybenzamidoperoxycaproic acid, N-nonenylamidoperadipic acid and N-nonenylamidopersuccinate, and (c) aliphatic and araliphatic peroxydicarboxylic acids such as 1,12-diperoxycarboxylic acid, 1,9-diperoxyazelaic acid, diperoxysebacic acid, diperoxybrassic acid, the diperoxyphthalic acids, 2-decyldiperoxybutan-1, 4-diacid, N, N-terephthaloyl-di (6-aminopercapronate) can be used.

Also useful as bleaching agents in automatic dishwashing compositions Chlorine or bromine releasing substances are used. Under the appropriate chlorine or bromine-releasing materials include, for example, heterocyclic N-bromo and N-chloroamides, for example trichloroisocyanuric acid, tribromoisocyanuric acid, Dibromoisocyanuric acid and / or dichloroisocyanuric acid (DICA) and / or salts thereof with Cations such as potassium and sodium into consideration. Hydantoin compounds, such as 1,3-dichloro-5,5-dimethylhydanthoin are also suitable.

To improve when washing or cleaning at temperatures of 60 ° C and below To achieve bleaching effect, bleach activators can be incorporated. When Bleach activators may be compounds which are aliphatic under perhydrolysis conditions Peroxycarboxylic acids having preferably 1 to 10 C atoms, in particular 2 to 4 C atoms, and / or optionally substituted perbenzoic acid, can be used. Suitable substances are the O- and / or N-acyl groups of said C atom number and / or optionally substituted benzoyl groups. Preference is given several times acylated alkylenediamines, in particular tetraacetylethylenediamine (TAED), acylated triazine derivatives, in particular 1,5-diacetyl-2,4-dioxohexahydro-1,3,5-triazine (DADHT), acylated Glycolurils, in particular tetraacetylglycoluril (TAGU), N-acylimides, in particular N-nonanoylsuccinimide (NOSI), acylated phenolsulfonates, especially n-nonanoyl or Isononanoyloxybenzenesulfonate (n- or iso-NOBS), carboxylic anhydrides, in particular Phthalic anhydride, acylated polyhydric alcohols, especially triacetin, ethylene glycol diacetate and 2,5-diacetoxy-2,5-dihydrofuran.

In addition to the conventional bleach activators or in their place may also so-called bleach catalysts are incorporated. These substances are to bleach-enhancing transition metal salts or transition metal complexes such as Mn, Fe, Co, Ru or Mo saline complexes or carbonyl complexes. Also Mn, Fe, Co, Ru, Mo, Ti, V and Cu complexes with N-containing tripod ligands and Co, Fe, Cu and Ru ammine complexes are useful as bleach catalysts.

Enzymes are those from the class of proteases, lipases, amylases, cellulases or mixtures thereof in question. Particularly suitable are from bacterial strains or Fungi such as Bacillus subtilis, Bacillus licheniformis and Streptomyces griseus enzymatic agents. Preferably, subtilisin-type proteases and in particular Proteases derived from Bacillus lentus. These are enzyme mixtures, for example from protease and amylase or protease and lipase or Protease and cellulase or cellulase and lipase or protease, amylase and lipase or protease, lipase and cellulase, but especially cellulase-containing mixtures of special interest. Peroxidases or oxidases have also been found in some Cases proved to be suitable. The enzymes can be adsorbed to carriers and / or embedded in encapsulants to protect against premature decomposition.

In addition, it is also possible to use components which are oil and grease washable from textiles positively influence (so-called soil repellents). This effect becomes particularly clear when a textile is soiled several times before with a detergent according to the invention containing this oil and fat dissolving component contains, was washed. Among the preferred oil and fat dissolving components include for example, nonionic cellulose ethers such as methyl cellulose and methyl hydroxypropyl cellulose with a proportion of methoxyl groups of 15 to 30 wt .-% and of hydroxypropoxyl groups from 1 to 15 wt .-%, each based on the nonionic Cellulose ethers, and the known from the prior art polymers of phthalic acid and / or terephthalic acid or its derivatives, in particular polymers of ethylene terephthalates and / or polyethylene glycol terephthalates or anionic and / or nonionic modified derivatives of these. Especially preferred of these are the sulfonated ones Derivatives of phthalic and terephthalic acid polymers.

The detergents and cleaning agents can be used as optical brighteners derivatives of Diaminostilbendisulfonsäure or their alkali metal salts. Suitable are e.g. Salts of 4,4'-bis (2-anilino-4-morpholino-1,3,5-triazinyl-6-amino) stilbene-2,2'-disulfonic acid or similar compounds which, instead of the morpholino group, have a diethanolamino group, a methylamino group, an anilino group or a 2-methoxyethylamino group wear. Furthermore, brighteners of the type of substituted Diphenylstyryle present be, e.g. the alkali salts of 4,4'-bis (2-sulfostyryl) -diphenyl, 4,4'-bis (4-chloro-3-sulfostyryl) -diphenyl, or 4- (4-chlorostyryl) -4 '- (2-sulfostyryl) -diphenyls. Also mixtures The aforementioned brightener can be used.

Dyes and fragrances are added to detergents and cleaners to enhance the aesthetic To enhance the impression of the products and the consumer in addition to the softness performance a visual and sensory "typical and unmistakable" product to deliver. As perfume oils or perfumes, individual fragrance compounds, e.g. the synthetic products of the ester type, ethers, aldehydes, ketones, alcohols and hydrocarbons are used. Fragrance compounds of the ester type are e.g. Benzyl acetate, phenoxyethyl isobutyrate, p-tert-butylcyclohexyl acetate, linalyl acetate, Dimethylbenzylcarbinylacetate, phenylethylacetate, linalylbenzoate, benzylformate, Ethyl methyl phenyl glycinate, allyl cyclohexyl propionate, styrallyl propionate and benzyl salicylate. The ethers include, for example, benzyl ethyl ether, to the aldehydes e.g. the linear alkanals with 8-18 C atoms, citral, citronellal, citronellyloxyacetaldehyde, cyclamenaldehyde, Hydroxycitronellal, lilial and bourgeonal, to the ketones e.g. the Jonone, Α-isomethylionone and methyl cedryl ketone, to the alcohols anethole, citronellol, Eugenol, geraniol, linalool, phenylethyl alcohol and terpineol, to the hydrocarbons mainly include the terpenes such as limes and pinene. However, preference is given Used mixtures of different fragrances, which together create an appealing Create a fragrance. Such perfume oils may also contain natural fragrance mixtures, as available from plant sources, e.g. Pine, Citrus, Jasmine, Patchouly, Rose or Ylang-Ylang oil. Also suitable are muscatel, sage oil, chamomile oil, Clove oil, lemon balm oil, mint oil, cinnamon leaf oil, lime blossom oil, juniper berry oil, Vetiver oil, Olibanum oil, Galbanum oil and Labdanum oil and Orange blossom oil, Neroliol, Orange peel oil and sandalwood oil.

The content of detergents and cleaning agents is usually less than that of dyes 0.01% by weight, while perfumes account for up to 2% by weight of the total formulation can.

The fragrances can be incorporated directly into the detergents and cleaners, it However, it may also be advantageous to apply the fragrances to carriers, the adhesion of the perfume on the lingerie and by a slower release of fragrance for long-lasting fragrance of the textiles. As such carrier materials, for example Cyclodextrins proven, the cyclodextrin-perfume complexes in addition can still be coated with other excipients.

To improve the aesthetic impression of detergents and cleaners, you can they are dyed with suitable dyes. Preferred dyes, their selection the expert no difficulty, have a high storage stability and Insensitivity to the other ingredients of the agent and against light as well no pronounced substantivity to textile fibers so as not to stain them.

Another object of the present invention is the use of the surfactant foams according to the invention as granulation liquid in the production of Surfactant granules. Regarding the proportions between Granulationshilfsmittel (Tensidschaum) and solid bed, the mixer to be used and in the solid bed usable ingredients are here referred to the above statements.

Examples:

A surfactant-containing, flowable component of the composition given in Table 1 was metered at a temperature of 80 ° C in a equipped with a check valve pipe section and foamed via sintered disks with compressed air (16 m ³ / h). The resulting foam (density: 0.45 gcm ^-3 , pore size <1 mm, temperature: 75 ° C) was in the ratio foam: solid of ~ 1: 4.7 in a plowshare mixer with 2 cutter heads (KM300-D, Gebrueder Lödige, Paderbom), the foam impinging on the moving solid bed (composition see Table 2) in the area of the first cutter head. The result was a pure white, free-flowing surfactant granules whose composition is given in Table 3 and whose physical properties are summarized in Table 4. Composition of flowable surfactant component [% by weight] Na C _9-13 alkyl benzene sulphonate 52.2 C _12-18 soap 5.4 C _12-18 fatty alcohol with 7 EO 28.8 HEDP 2.3 water 11.3 Composition of the solid bed [% by weight] Zeolite A (Wessalith® P, Degussa) 36.1 sodium sulphate 32.0 sodium 21.2 Sokalan® CP 5, 50% in water 10.7 Composition of the surfactant granules [% by weight] Na C _9-13 alkyl benzene sulphonate 11.4 C _12-18 soap 1.3 C _12-18 fatty alcohol with 7 EO 6.3 Zeolite A (Wessalith® P, Degussa) 26.9 sodium sulphate 25.6 sodium 17.0 HEDP * 0.5 Sokalan® CP 5 4.3 water 6.7 Physical data of the surfactant granules Bulk density [g / l] 840 Sieve analysis [% by weight]: > 1.6 mm 3 > 1.2 mm 9 > 0.8 mm 26 > 0.4 mm 40 <0.4 mm 22 colour pure white

Zusammensetzung der Tensidgranulate [Gew.-%] E2 E3 E4 E5 E6 Schaum (Tabelle 5) 6,4 9,1 11,9 6,4 9,8 Feststoffe (Tabelle 6) 93,6 90,9 88,1 93,6 90,2 Physikalische Daten der Tensidgranulate E2 E3 E4 E5 E6 Schüttgewicht [g/l] 615 544 562 556 515 Siebanalyse [Gew.-%]:    > 1,6 mm 2 6 3 5 6    > 1,2 mm 7 17 12 14 17    > 0,8 mm 21 34 32 33 31    > 0,4 mm 32 40 48 47 35    < 0,4 mm 38 3 5 1 11 Farbe reinweiß reinweiß reinweiß reinweiß reinweiß Further experiments on a production scale were carried out with surfactant-containing, flowable components of the composition given in Table 5. For this purpose, the components were metered separately at a temperature of 50 ° C in equipped with a check valve pipe sections and foamed via sintered disks with the 50-fold volume of compressed air and mixed together. The resulting foam (density: 0.5 gcm ^-3 , pore size <1 mm, temperature: 50 ° C) was metered into a ploughshare mixer with 2 cutter heads (type KM300-D, Gebrüder Lödige, Paderbom), wherein the foam in the range first cutter head impacted on the moving solid bed (composition see Table 6) and the mixer tools were moved at peripheral speeds of 3 m / s. The continuous granulation was carried out with a mass output of 1 t / h. In turn, pure white free-flowing surfactant granules were produced, whose composition is given in Table 7 and whose physical properties are summarized in Table 8. Composition of flowable surfactant components [% by weight] E2 E3 E4 E5 E6 Sodium silicate solution, 30% by weight - 31.2 25.9 - - Sokalan® CP 5 - - 22.3 - - C _12-14 alkyl-1,4-glucoside - - - - 39.2 C _12-18 fatty alcohol with 7 EO 10 68.8 51.8 100 60.8

Composition of the surfactant granules [% by weight] E2 E3 E4 E5 E6 Foam (Table 5) 6.4 9.1 11.9 6.4 9.8 Solids (Table 6) 93.6 90.9 88.1 93.6 90.2 Physical data of the surfactant granules E2 E3 E4 E5 E6 Bulk density [g / l] 615 544 562 556 515 Sieve analysis [% by weight]: > 1.6 mm 2 6 3 5 6 > 1.2 mm 7 17 12 14 17 > 0.8 mm 21 34 32 33 31 > 0.4 mm 32 40 48 47 35 <0.4 mm 38 3 5 1 11 colour pure white pure white pure white pure white pure white

Claims (34)

1. A process for the production of surfactant granules in which a surfactant-containing flowable component is exposed to the action of a gaseous medium, characterized in that the surfactant-containing flowable component is foamed by the gaseous medium and the surfactant-containing foam formed is subsequently added to a bed of solids introduced into a mixer.
2. A process as claimed in claim 1, characterized in that the surfactant-containing flowable component contains one or more surfactants from the group of anionic and/or nonionic and/or cationic and/or amphoteric surfactants in quantities of 20 to 100% by weight, preferably 50 to 95% by weight and more preferably 60 to 90% by weight, based on the surfactant-containing component.
3. A process as claimed in claim 1 or 2, characterized in that the surfactant-containing flowable component contains anionic surfactant(s) in quantities of 10 to 90% by weight, preferably 20 to 85% by weight and more preferably 30 to 80% by weight, based on the surfactant-containing component.
4. A process as claimed in claim 3, characterized in that the surfactant-containing flowable component contains alkali metal salts of alkyl benzenesulfonic acids in quantities of 20 to 90% by weight, preferably 30 to 85% by weight and more preferably 40 to 80% by weight, based on the surfactant-containing component.
5. A process as claimed in any of claims 1 to 4, characterized in that the surfactant-containing flowable component additionally contains soaps in quantities of 1 to 30% by weight, preferably 2 to 25% by weight and more preferably 5 to 20% by weight, based on the surfactant-containing component.
6. A process as claimed in any of claims 1 to 5, characterized in that the surfactant-containing flowable component contains nonionic surfactant(s) in quantities of 1 to 100% by weight, preferably 2 to 70% by weight and more preferably 5 to 30% by weight, based on the surfactant-containing component.
7. A process as claimed in claim 6, characterized in that the surfactant-containing flowable component contains alkoxylated, preferably ethoxylated, nonionic surfactants in quantities of 20 to 90% by weight, preferably 30 to 85% by weight and more preferably 40 to 80% by weight, based on the surfactant-containing component.
8. A process as claimed in claim 7, characterized in that the surfactant-containing flowable component contains the reaction products of C_8-22 fatty alcohols, preferably C_12-20 fatty alcohols and more preferably C_14-18 fatty alcohols with 1 to 30 mol ethylene oxide, preferably 2 to 20 mol ethylene oxide and more preferably 5 to 10 mol ethylene oxide in quantities of 10 to 80% by weight, preferably 20 to 75% by weight and more particularly 30 to 70% by weight, based on the surfactant-containing component, as the ethoxylated nonionic surfactants.
9. A process as claimed in any of claims 1 to 8, characterized in that the surfactant-containing flowable component contains less than 20% by weight, preferably less than 15% by weight and more preferably less than 10% by weight of water, based on the surfactant-containing component.
10. A process as claimed in any of claims 1 to 9, characterized in that the surfactant-containing flowable component contains other ingredients of detergents, more particularly from the group of complexing agents, polymers, optical brighteners, dyes and perfumes and alkalis.
11. A process as claimed in any of claims 1 to 10, characterized in that the quantity of gas used for foaming makes up one to three hundred times, preferably five to two hundred times and more preferably ten to one hundred times the volume of the quantity of surfactant-containing flowable component to be foamed.
12. A process as claimed in any of claims 1 to 11, characterized in that air is used as the gaseous medium.
13. A process as claimed in any of claims 1 to 12, characterized in that the surfactant-containing flowable component to be foamed has temperatures before foaming of 20 to 120°C, preferably 30 to 90°C and more preferably 50 to 75°C.
14. A process as claimed in any of claims 1 to 13, characterized in that a surfactant-containing liquid component is foamed and the foam formed is combined with a foam produced from another liquid component which then serves as granulation foam.
15. A process as claimed in claim 14, characterized in that the second liquid component to be foamed is surfactant-containing.
16. A process as claimed in any of claims 1 to 15, characterized in that the surfactant-containing foam has temperatures below 115°C, preferably between 20 and 80°C and more preferably between 30 and 70°C.
17. A process as claimed in any of claims 1 to 16, characterized in that the surfactant-containing foam has a density below 0.80 gcm^-3, preferably between 0.10 and 0.60 gcm^-3 and more preferably between 0.30 and 0.55 gcm^-3.
18. A process as claimed in any of claims 1 to 17, characterized in that the surfactant-containing foam has mean pore sizes below 10 mm, preferably below 5 mm and more preferably below 2 mm.
19. A process as claimed in any of claims 14 to 18, characterized in that the surfactant-containing foam satisfies the criteria mentioned when added to the mixer.
20. A process as claimed in any of claims 1 to 19, characterized in that the bed of solids introduced into the mixer contains one or more substances from the group of builders, more particularly alkali metal carbonates, sulfates and silicates, zeolites and polymers.
21. A process as claimed in any of claims 1 to 20, characterized in that the bed of solids introduced into the mixer contains spray-dried basic powders, preferably surfactant-containing spray-dried basic powders, in quantities of 10 to 80% by weight, preferably 15 to 70% by weight and more preferably 20 to 60% by weight, based on the solids introduced into the mixer.
22. A process as claimed in any of claims 1 to 21, characterized in that the surfactant-containing foam is added to the bed of solids in the mixer in a ratio by weight of foam to solids of 1:100 to 9:1, preferably 1:30 to 2:1 and more preferably 1:20 to 1:1.
23. A process as claimed in any of claims 1 to 22, characterized in that the surfactant-containing foam is added to the bed of solids in the mixer in a low-speed mixer/granulator at peripheral speeds of the tools of 2 m/s to 7 m/s over a period of 0.5 to 10 minutes, preferably over a period of 1 to 7 minutes and more preferably over a period of 2 to 5 minutes.
24. A process as claimed in any of claims 1 to 22, characterized in that the surfactant-containing foam is added to the bed of solids in the mixer in a high-speed mixer/granulator over a period of 0.1 to 30 seconds, preferably up to 10 seconds and more preferably between 0.5 and 2 seconds at peripheral speeds of 8 m/s to 35 m/s.
25. A process as claimed in any of claims 1 to 22, characterized in that the surfactant-containing foam is added is added to an agitated bed of solids in a first low-speed mixer/granulator, 40 to 100% by weight, based on the total quantity of constituents used, of the solid and liquid constituents being pregranulated and the "pregranules" from the first process step optionally being mixed with the remaining solid and/or liquid constituents and converted into granules in a second high-speed mixer/granulator.
26. A process as claimed in claim 25, characterized in that the "pregranules" from the first process step are granulated into the final granules in the second, high-speed mixer/granulator, again with addition of a surfactant-containing foam of which the composition may differ from that of the foam used in the first process step.
27. A process as claimed in any of claims 1 to 22, characterized in that the surfactant-containing foam is added to an agitated bed of solids in a first high-speed mixer/granulator, 40 to 100% by weight, based on the total quantity of constituents used, of the solid and liquid constituents being pregranulated and the pregranules from the first process step optionally being mixed with the remaining solid and/or liquid constituents and converted into granules in a second low-speed mixer/granulator.
28. A process as claimed in claim 27, characterized in that the pregranules from the first process step are granulated into the final granules in the second, low-speed mixer/granulator, again with addition of a surfactant-containing foam of which the composition may differ from that of the foam used in the first process step.
29. A process as claimed in any of claims 23 to 28, characterized in that it is carried out in batches or continuously.
30. A process as claimed in any of claims 24 to 29, characterized in that a mixer comprising both a mixing unit and a size-reducing unit is used as a high-speed mixer, the mixing shaft being driven at peripheral speeds of 50 to 150 r.p.m. and preferably 60 to 80 r.p.m. and the shaft of the size-reducing unit being driven at rotational speeds of 500 to 5,000 r.p.m. and preferably 1,000 to 300 r.p.m.
31. A process as claimed in any of claims 1 to 30, characterized in that the surfactant granules have surfactant contents above 10% by weight, preferably above 15% by weight and more preferably above 20% by weight, based on the granules, and bulk densities above 600 g/l, preferably above 700 g/l and more preferably above 800 g/l.
32. A process as claimed in any of claims 1 to 31, characterized in that the surfactant granules have a particle size distribution where at least 50% by weight, preferably at least 60% by weight and more preferably at least 70% by weight of the particles are between 400 and 1600 µm in size.
33. A process as claimed in any of claims 1 to 32, characterized in that the surfactant granules have residual free water contents of 2 to 15% by weight and preferably 4 to 10% by weight, based on the surfactant granules.
34. The use of surfactant foams with mean pore sizes below 10 mm, preferably below 5 mm and more particularly below 2 mm as a granulation liquid in the production of surfactant granules.