DE3926253A1 - Compressed solid granules prepn. of washing agent - by extruding mixt. of solid components and plasticiser, cutting strand to size, treating with further active materials and drying - Google Patents

Abstract

In prepn. of compressed solid granulates of pre-determined particle size from mixts. of at least partly solid components of washing and/or cleaning agents for the household or industry, esp. for washing textiles, the solid mixt., opt. contg. liq. components, is processed with addn. of water-sol., water-emulsifiable and/or water-dispersible plasticisers and/or lubricants, to a uniform compsn. which can be pressed to shape. This compsn. is pressed to a strand through a perforated plate with openings of the pre-determined size of the granules, and cut to the required size, and the still plastic granules are opt. rounded before being treated with other active materials and/or being dried to a free-flowing granulate. Before, during or after being rounded off, the granulate may be mixed with a finely divided dry powder, opt. a component of the final prod., and pref. a zeolite NaA of washing agent quality. ADVANTAGE - The prod. is non-tacky and stable on storage, with increased bulk wt. (up to 1,000 g/l).

Description

In the field of finely divided solid and free-flowing washing and Household and commercial cleaning agents, especially on the Field of powder detergents for textiles currently a trend towards manufacturing products with increased Powder bulk weights. Newer commercial products of this type bulk weights are currently in the range of about 700 g / l. These Raising the bulk weights is related to Forde environmental protection after less packaging. In the same direction, washing and cleaning efforts are aimed detergent - and here again textile detergent - in Form of more concentrated mixtures of ingredients to be able to offer. At first, the reduction of Adding agents in the concentrates as unnecessary salt load Offer. However, a solution to this problem is not without further possible. Prerequisite for such recipe modifications is understandable that on the one hand the required washing and cleaning-technical requirements compared to At least get the usual market products today remain, on the other hand, but also ensuring the storage stability free-flowing and free-flowing forms of detergent preparation. The Fulfillment of this requirement profile poses not insignificant technological problems.

Are from the relevant printed state of the art in particular granules with a content of carrier substances and liquid or paste-like surfactants adsorbed thereon,  especially known nonionic surfactants. To Manufacturing processes have been developed in which the liquid or melted nonionic surfactant on a previously spray-dried powder sprayed on or with a powder ver migen carrier under granulating conditions is mixed. Loose, especially spray-dried water-soluble salts or salt mixtures of the Detergent range - for example phosphates, silicates and / or Perborate - proposed as well as the water-insoluble ver bonds, for example zeolites, bentonites and / or very fine partial silicon dioxide. Absorbent carrier grains of this type, the especially for the adsorption of nonionic surfactants have been wrapped and mostly by spray drying are described, for example, in US Pat 38 49 327, 38 86 098, 38 38 027 and 42 69 722. The US-PS 47 07 290 describes a granular adsorbent, which in the Should be able to high levels of liquid to pasty washing absorb medium components and by spray drying is provided. In practice it has been shown that products of this Can show some kind of difficulties during the induction phase, they do not come off completely and leave residues. A such worsened induction behavior is not only shown by concerned particles themselves, they can also influence the Solubility or the induction behavior of the other powdery Exercise detergent components. The result is that one in itself powder mixture that can be easily washed in overall difficult to wash in if there are such powder components in the Mixture contains. Further suggestions of this kind can be found for example in DE 34 44 960 A1 and EP 1 49 264.

All of these suggestions are comparatively complex. First an aqueous slurry of the carrier is prepared, the then by spray drying into a granular porous intermediate must be transferred. In a second process stage  the carrier grains with the liquid component, in particular sprayed nonionic surfactant. Diffusing the not ionic surfactants are delayed and adsorbates with high proportion of nonionic surfactants are only after one certain treatment and rest times sufficiently free-flowing. Go one, however, from powdery precursors, for example of fine crystalline zeolites or crystalline water soluble carrier salts and treats them with liquid or melted nonionic surfactants with granulating loading conditions are usually granules with very uneven grain spectrum and reduced pouring properties. In front all things, however, is the absorption capacity of such granules comparatively limited for nonionic surfactants if not essential material properties, especially the good trickle ability to get lost.

In contrast, the teaching of the present invention proceeds from a new technological concept for solving the here given problem. The invention wants one on the one hand the production of solid, free-flowing and in their special shape design of predeterminable granules of Allow ingredients of detergents and cleaning agents, whereby at the same time the setting of significantly increased bulk weights should be accessible. In addition and in connection with this The object of the invention also aims to solve a further problem rich, especially from the field of storage stable free-flowing Detergents and cleaning agents, especially for textiles, are better open up. Here in particular the access to bulk and free-flowing detergent concentrates are opened, too when storing for longer periods and under difficult Storage conditions maintain their pourability.

The invention particularly wants textile detergents in granular form make available, which is in bulk weights up to about  1000 g / l by a predeterminable uniform or disunited uniform shape of the granulate with good flowability draw and in practical use without problems against today and textile detergents common in the recent past powder can be exchanged. The invention covers with their granules produced in a new way both Range of ready-to-use multi-substance mixtures of the specified Purposes in the form of uniformly mixed granules as also partial products for the mentioned area of application, which are used for Completion of the recipe, even mixing with other ingredients components of the relevant washing and / or cleaning by means of need. The invention captures in a particular Aus form of management in particular also such mixtures of the the inventive method described below produced granules and subsequently applied to them or further active ingredient mixture mixed with the granules elements of the respective overall recipe.

The core of the teaching according to the invention is as follows described granulation process in which finely divided solid and if required, liquid ingredients of the respective overall recipe for compacted granulate in a new kind Way to be worked up.

The invention accordingly relates to a first Embodiment the new method of manufacturing ver sealed solid granules of predetermined particle size Mixtures of at least partially solid, finely divided ingredients of detergents and / or cleaning agents for household and commercial use be, especially laundry detergents. The new Process is characterized in that the given if solid containing mixed liquid ingredients mixture of substances with the addition of water-soluble, water emul gible and / or water-dispersible plasticizing and / or  Lubricants to a homogeneous, form-compressible mass processed, this mass over hole shapes with opening widths of predetermined pellet dimension extruded, which from occurring compacted strands of material to the predetermined Granulate dimension to length and, if desired, the still pla round granular particles to round off the shape and to form grain free-flowing granules. If necessary can the primarily formed still plastic granules before, during and / or after rounding off with further effects substances are applied, but in particular this can also be the case material dried to form granular, free-flowing granules acted upon with such additional components and / or from be mixed. It is possible to add these Components essentially evenly on the surface of the to apply granular granules according to the invention and / or these additional components in turn in particle form - for example also in granular form - in the one designed according to the invention Mix in granular material.

In further embodiments, the invention relates to of the conception according to the invention, and especially free-flowing granules of the type described and the use of these granules in washing and cleaning detergents, especially in detergents for textiles. In the end However, the invention relates in a further embodiment also the application of the described pelletizing process Manufacture of essentially adhesive-free bulk and free-flowing storage-stable washing and cleaning agent concentrates, in particular corresponding high concentrates for textile washing medium with a significantly excessive detergent content, especially on detergent surfactants, the more common point to undesired softening and / or sticking of the lead particulate goods.  

The core of the process according to the invention for producing granules lung lies in the targeted preparation and conversion of a finely divided solid, if desired also limited amounts of active ingredient mixture containing liquid components to a homogeneous, plasticized and coherent when using high Press compressible mass using selected plastifi decorative and / or lubricant. These tools come within the scope polyfunctional meaning of the invention. With the granules manufacture enable the formation of the granulate blanks and their subsequent shaping, if desired work, especially rounding off the primary granules. Wear after the granules have dried an important version of these plasticizers and lubricants Form of the invention in turn for the stability of the granules kornes, they preserve its predetermined spatial shape in particular where necessary with the mixing with white other components, in filling, in transport and in Storage of the granular material and prevent in particular the formation of unwanted dusty parts. In practical terms Enable use of the granular detergent or cleaning agent the reverse, however, the rapid dissolution of the granular good, being in an important embodiment of the Invention of this solution, emulsification or dispersion step in use by the pla lubricant and lubricant is currently favored. After all, can in particularly important embodiments of the invention auxiliaries of the method according to the invention discussed here Intrinsic effect in the washing or cleaning process and in particular in the interaction with the other components of the mixture Detergents and / or cleaning agents.

A particularly preferred embodiment of the fiction The method is characterized in that as Pla stiffening and / or lubricating agents pasty to flowable  Preparations based on water-soluble or water-emulsifiable Polymer compounds and / or based on surfactant components ten uses, in each case corresponding aqueous and / or water-miscible preparations are particularly preferred.

Detergents and cleaning agents, regardless of whether they are for the Tex til wash, for cleaning hard surfaces, in the house stop, used in trade or in technical use, are always made by combining basic ingredients indicates. A class of these usually existing In Ingredients are the surfactant components that generally in the form of selected and adapted to the respective purpose Find combinations of surfactants. The invention makes the fact in the embodiment concerned here use that in particular highly concentrated aqueous mixtures such surfactants or surfactant mixtures show a state image that as a pasty or gel-like preparation with lubricant character can be called. This plasticizing and at the same time lubricant-like or lubricant-like state of water Concentrated surfactant blends can be effective position of the mass characteristics are used as they using high pressures to shape the appearing as a mixture of active substances in the first stages of homogenization and shaping the pressing as well as in the formation of the plasticized Granule blanks are needed. When they dry up, they form like this registered surfactants or surfactant proportions like binders covering and intermediate layers that are jointly responsible for are the grain cohesion. In practical use of the kornför accelerate good in especially aqueous liquid phases But these surfactants then favor and promote the rapid Grain breakdown with dissolution, emulsification and / or dispersion of fine grain-forming particles.  

Just like the use of surfactant components Use of polymer compounds in numerous laundry and cleaning agents, of course, technical action. Polymer compounds can be used in the field of textile detergents for example as framework substances with the ability to bind of water hardness are used. An example of this are the Polymerver used today to a not inconsiderable extent bonds containing carboxyl groups, which are also in Salt form e.g. B. may be present as an alkali salt. As examples the sodium or potassium salts of homopolymeric and / or copolyme rer called carboxylic acid compounds. Suitable homopolymers are, for example, polyacrylic acid, polymethacrylic acid and polymaleine acid. Suitable copolymers are, for example, those of Acrylic acid, methacrylic acid or copolymers of acrylic acid, Methacrylic acid or maleic acid with vinyl ethers, vinyl esters and / or other comonomers such as acrylamide, methacrylamide, Ethylene, propylene or styrene. But also for completely different ones typesetting purposes, for example, to improve the dirt-carrying capacity Like an aqueous detergent liquor, polymer compounds in active ingredient mixtures of the type concerned here rule moderately used. Examples of these are carboxymethyl cellulose (CMC) and / or methyl cellulose (MC).

In particular, highly concentrated forms of preparation of such in the Usually water soluble, water emulsifiable and / or water dis Pearable polymer compounds stand out just like that previously discussed surfactant preparations by a characterized lubricating character, which in the process stages of Homogenization, compression using high pressures, the molding and if desired rounding off the decisive processing aid gives. At the same time, however, these polymer granules also dry components in the final training of the free-flowing Good things about polymer films, on the one hand, the cohesion of the  Promote grain shape, on the other hand when added in particular aqueous media easily return to the state of the solution or Skip emulsification and / or dispersion.

Comparable state images in the different stages of the inventive method or the use of the inventions Granules produced in accordance with the invention not only show which are usually used in washing and / or cleaning agents put polymer compounds. Practice knows numerous na door and / or synthetic types of polymer, here as well Can be used and ultimately the washing and / or Do not adversely affect the cleaning process. Just as Examples include gelatin and / or starch or their derivatives as a natural product or semi-synthetic material or polyvinyl alcohol as a purely synthetic polymer material.

The lubricants and / or plasticizers used as additives can in turn flow, gel-like or at room temperature be pasty without the use of an additional Liquid phase is required. There are many examples of this Types of those not used in detergents and cleaning agents ionic surfactant compounds. Above all, are suitable but plasticizing and / or lubricant preparations, which under Using limited quantities of auxiliary liquids have been. Water and / or organi come as liquid phases cal liquid phases into consideration, preferably components of the latter type to be water-soluble or water-miscible can. For reasons of procedural security, it can be useful be moderate, comparatively high-boiling organic liquid com components instead of or together with water. Examples for this purpose, higher-boiling, optionally polyfunctional Al alcoholic, at room temperature or moderately elevated temperatures flowable polyalkoxylates and the like.  

The surfactants used as lubricants and / or plasticizers and / or polymer compounds are expediently in the Art concentrated form introduced into the process that the desired quality of the plastic, gliding pressed mass with small amounts of these auxiliary components can be adjusted. At least are particularly suitable about 30% by weight, preferably at least about 40% by weight Surfactant pastes or gels, whereby in a particularly important embodiment tion forms such surfactant preparations with a surfactant content of at least about 50% by weight. 50 to 70 % by weight, in particular aqueous, surfactant gels or surfactant pastes often create a particularly suitable state for the different material stresses or requirements in the successive process steps.

Are due to the sufficient moisture penetration of the granulating goods slightly larger amounts of liquid needed, it is generally appropriate to add these Mix shares as such into the material to be granulated and not the surfactant or poly used as a lubricant Thinner component more dilute. The introduction of such too Additional amounts of fluid can be taken before, during or after the The lubricant component can be incorporated, preferably the addition before incorporation of the effective as a lubricant Proportion of the mixture. In any case are in the invention Plasticizing and processing methods comparatively low Amounts of the liquid phase necessary, so that accordingly subsequent drying of the granules is facilitated.

In carrying out the method of the invention, the raw materials to be processed into granulate or material mix the plasticizing aids and if necessary additionally added small amounts of liquid in such an amount, that at first just a free-flowing mix  powder-like structure is retained. Only with the intensive Homogenization of the mixture of substances using comparative high pressures, for example by kneading, occurs Ver seal of the multi-component mixture, and it will in particular by means of kneading in the multi-component mixture Texture set. At the same time Ensured cutting ability of the homogenized mass. Here the moisturizing and plasticizing parts of the good are so limits that a gluing of the primary granules Verformlings with each other safely before further processing can be prevented. Details on this will be discussed below specified.

An essential element of the teaching according to the invention lies in the following combination of elements: comparatively be limited amounts of liquid phase (s) are used. The The mixture of substances is then comparatively applied high pressures so thoroughly mixed and kneaded that the previously dry-appearing mixture of substances to compact plasticized and form-compressible mass worked up is. The external appearance of this processing step is similar to the plastic processing of rubber containing mixtures or the plasticization of Plastic granules to form a compressible mass. As well as there can also in the homo according to the invention Generation and compression of the primary dry matter seeming mixture of substances to form compressible mass supporting a limited increase in the melt temperature Act. The ability of the limited liquid content in the fabric mix for softening plastification with increasing Temperature too. The intensive mixing process, for example by kneading the desired tempera out of itself lead increase. If necessary, however, additional targeted temperature regulation from the outside  will. However, this desired state is primarily a result of the total liquid used in the mixture proportions and due to the water absorption capacity of the finely divided fixed mixture components determined. The general rule is that highly concentrated surfactant pastes or gels or the ones before mentioned highly concentrated, especially aqueous polymer Preparations in amounts not exceeding about 12% by weight, preferably of at most about 10% by weight, based in each case on the total mixture - can be used. Significantly lower quantities for example on surfactant paste already lead to good results, for example in the field of textile detergent production. For example, a mixture of tower powder / carrier bead can be used or without the addition of sodium perborate (monohydrate and / or Tetrahydrate) with the addition of 2 to 5% by weight of water and 4 to 8 % By weight of a 55 to 60% ABS paste to a mass more suitable Prepared consistency for further shaping will.

The processing procedure is as follows:

First, a premix is made in a manner known per se fixed and the possibly used limited An parts made of liquid components. So on the way the tower powder obtained by spray drying is also quite a fold the selected mixture components as pure substances in finely divided state can be mixed together. Depending on the good and then the required amount of liquid phase the plasticizer and lubricant selected according to the invention as preferably mixed in aqueous paste or gel. If desired can now also other solid components of the Vor mixture can be added. The total mass is added shortly mixes, the respective proportions are selected so that a preferably free-flowing premix is obtained, which is used for loading a homogenizer is suitable.  

Kneaders of any type are preferably used as the homogenizing device Design, for example, 2-screw kneader selected. It can be useful in this step of homogenization the material to be pressed to moderate temperatures at for example, set to 45 to 60 ° C. Under the sherein effect of the kneading device, the premix becomes compacting plasticized and immediately afterwards through perforated nozzles fine strands pressed. These strands are in the extent of their Training in raw granules of the desired particle size cut or split. To perform this procedure According to the invention, two steps are possible in particular suitable:

In the first embodiment, the free-flowing premix preferably continuously a 2-screw kneader / extruder fed, its housing and its extruder pelletizing head to the predetermined extrusion temperature, for example approx. 45 to 50 ° C are heated. Under the shear of The premix is compressed and plasticized by extruder screws and then through the extruder head orifice plate extruded fine strands, which after the nozzle exit by means of a rotating cutting knife to cylindrical pellets be crushed. The hole diameter in the hole nozzle plate and the strand cut length are based on the selected Gra nulatdimension coordinated. In this embodiment of the inventions The inventive method succeeds in the production of granules a substantially uniform predeterminable particle size, the absolute particle sizes being the individual be intended use may be adapted. Absolute part For example, size sizes can range from a few tenths Millimeters, for example about 0.3 mm up to 1 to 2 cm, however, in general the range up to at most approximately 1 cm, preferably up to a maximum of about 0.8 cm particle diameter is preferred. Important embodiments of the invention see here the production of uniform granules  Diameters in the mm range, for example in the range from 0.5 to 5 mm and in particular in the range of about 0.8 to 3 mm.

The length / diameter ratio of the cut raw granule latkorns is in the embodiment shown here preferably in the range of approx. 1 and can expediently rather are slightly below the number 1.

By shock cooling the strand-shaped from the perforated plate entering mass and in particular by blowing cold air in the pelletizing knife area, the pellet is at least above partially cooled flat - for example to temperatures of approx. 40 to 45 ° C - at the same time there is a partial removal of surface water of the pellets formed. To this Way the gluing of the still plasticized pellets in this process step can be reliably prevented.

The pellet blanks formed in this way can as such a drying step, for example a fluidized bed dryers are fed in with the supply air moderately raised temperatures, especially in the range of about 75 to 80 ° C ent speaking moderate product temperatures of for example approx. 55 set to 60 ° C, but then not exceeded. After sufficient drying, the Pro cools down products with cold air, for example.

However, the still plastic raw granules are preferred first a further shaping processing step guided. Here the edges present on the raw granulate rounded so that ultimately spherical or at least approximately spherical granules can be obtained. By using small amounts of dry powder in the This level of final shaping processing can be done undesirable sticking of the granules together  preclude their final drying. For Detergents and cleaning agents can use suitable dry powders pulverulent materials or corresponding inert materials be. A particularly suitable resource in this context are, for example, zeolite powder in detergent quality for example, corresponding zeolite NaA powder.

This final shaping of the still moist granulate the extruder granulation can be done in standard rounding machines batch or continuous. Are suitable for for example corresponding rounding machines with rotating floor slice, by varying the granulate residence time in Rounding device and / or the rotation speed of the devices the desired degree of rounding can be set.

The granulate grain thus finally formed is then also as described above, for example in one drying Fluid bed dryer fed. The resulting very low dust Finally, product can also be removed to remove less formed coarse fractions classified, for example, are screened. The proportion of good grain to be set according to the invention is in generally above 90%, preferably above 95% of the granular material.

Still missing, for example sensitive, especially tem The granulate can be exposed to temperature sensitive ingredients added after its formation, e.g. B. sprayed and / or as separately formed grain to form a multigrain good to be mixed. The granulate can only do so a share - preferably the at least predominant share - Make out the finished washing and / or cleaning agent.

However, the method according to the invention is not limited to Processing of the plasticized raw material via  Extruder screws and perforated plates arranged in the extruder head limited. Also through conventional pellet presses and the like Granulating devices can be inventively plasticized, compressed and homogenized mixtures of substances Granulate granular material. This may then fall a grain-like good rather cylindrical shape and / or inconsistent particle size, which as such dried or also initially a continuing form-giving Processing can be fed and then dried.

The material densities in the grain and thus also the bulk density of the Granules are homogenized by the pressing of the working material used through the perforated plates significantly involved. By building a sufficiently compact basic structure in the mass to be pressed and use correspondingly high pressures can e.g. B. with conventional Tex detergent formulations Bulk weights significantly above 700 g / l, preferably above 750 g / l and especially in the loading Realize from about 800 to approximately 1000 g / l. So are based on commercially available textile detergent formulations Bulk weights in the range of 850 to 970 g / l at the same time good flowability and a preferably homogeneous uniform spherical grain structure adjustable. In similar approaches are free-flowing granules in the dry state with uniform Bulk weights from 950 to 970 g / l with an average Particle size of the spherical granules in the range of about 1 mm has been realized.

The inventive method is characterized by a very low return share. The return share according to you Practice the previously described raw granulate over a 1.6 mm sieve was in the range of at most 3%. Analogous to the convention tional detergent preparation, the remaining emp sensitive formulation components - for example activators for  Bleaching agents, enzymes, defoamers, especially silicone foamer, perfume and the like - added to the raw granules will. Even then, detergent end products are still used obtained with bulk weights in the range of about 900 g / l.

The application properties of the granules, esp in particular their dissolution characteristics, the induction behavior and the residue behavior meets the requirements. The Extruder granulation processes previously described in detail is characterized by a high degree of flexibility.

This increased flexibility due to the technology according to the invention in the manufacture of solid, storage-stable, free-flowing washing and / or cleaning agents for household and commercial use can be seen in a number of other aspects, briefly discussed below had gone.

The compression provided according to the invention is initially rather Active ingredient premix still appearing in powder form plasticized and form-compressible mass under An application of high pressures during homogenization and pressing not only leads to the desired increased bulk weight, at the same time the following effect is realized: The mixture of active ingredients lies in the granule in a dense packing inaccessible to undesirable interaction with any used further components of the total agent. It opened up thus the possibility of each selected and in particular mutually compatible mixture components into the compressed To transfer granulate form and to produce these compacts of the finished product with other components of the overall pro to combine products without undesirable reactions in La and the distribution of the drug would be feared.  

In a particularly important embodiment of the invention the new technical teaching provides for the use of granulate systems, which is a combination of compacts of different composites represent position. In this way, the storage is stable Unification potentially more reactive or at least limited compatible components. An example of this are common Textile detergents, but now in the new preparation form at least two types of compacts in a mixture with each other put. In a first, for example spherical type of granulate the bleach component, especially water of crystallization Perborate and sodium carbonate containing a Share of plasticizers and / or lubricants pelleted, in one The second granulate is separated as the detergent builder Zeolite used, in particular zeolite NaA in detergent Quality pressed with the rest of the detergent ingredients. The Storage stability of the mixed product substantially influencing Interactions between perborate and zeolite - as in powder formal preparations are to be considered - are on this Way excluded. It is obvious that this possibility the use of granulate systems from different Composite compacts in almost any combination Can be used.

This version is particularly helpful for the realization forms of the fact that - starting from an almost dry-appearing powdery mixture - only limited by application of pressure and if desired in any case strictly controllable temperature increase arbitrarily composite compacts can be produced. The invention The pressure range used is usually little at least about 10 bar, preferably at least about 25 to 30 bar in the compression and extrusion step. Press in the area from about 50 to 150 bar or even higher pressures be particularly suitable here. It is consistently  but a work tool that is more common for processing Ingredients of washing and cleaning agents for household and Commercial is to be regarded as harmless. Which derives from it tending to facilitate the combination of reactive in itself and / or unstable active ingredient components by means of such a press ling systems is obvious.

The flexibility and relief provided by the invention in the preparation of active ingredient mixtures of those affected Art is also derived from completely different considerations. To Adjustment of the composition of the mass that can be compressed under pressure limited liquid components are required in the system. In particular special water is a suitable auxiliary liquid. At least one Share of these necessary for the implementation of the procedure The amount of water can over the components to be compressed, especially the corresponding solid components be introduced. The following example shows this possibility clear: sodium zeolite NaA falls as water-containing master batch, which is customary today Process of manufacturing textile detergents Drying, in particular spray drying. According to the invention, it becomes possible to use the zeolite or at least Zeolite fractions in the form of the undried master batch or one only partially dried and thus only limited in the water content of the enriched material Add premix.

From a completely different point of view, this is already happening The flexibility of the process that has been mentioned several times can be seen: The steps of homogenization according to the invention, the Compression and compression of the active agent used mixtures of substances only require very short periods of time. Usually periods in the minute range, for example a maximum of 10 Minutes, preferably less than 5 minutes and often no more  than 3 minutes needed from premix to compacted plasticized finished granules to come, which then one Drying needs. As described at the beginning, this can drying by treating the compacts with, for example heated air. At least partly, however, that is "Inner drying" of the respective substance mixtures is possible as follows Lich: By using a moisture-binding mixture Components in the material to be compacted can be found in the short process processing time the plasticizing effect of the presented Liquid components are used by binding at least sub substantial portions of these liquid portions by mixed in then the internal drying takes place, so that the external drying can be shortened substantially or entirely not applicable. Suitable mixture components for such an inner Drying are components that are able, for example, To bind water in the form of crystal water. In the area of Detergents and cleaning agents are particularly useful here for example sodium sulfate and / or soda in anhydrous or low water form or also a proportion of water of crystallization instructed detergent-quality zeolite.

A further relief and thus flexibility of the Ver driving can be in the following embodiment: The Bil high as a plasticizer and / or lubricant concentrated pastes of in particular surfactant mixture Ingredients can be in situ in the multi-component mixture to be processed respectively. Such an embodiment can be particularly important in the production of detergent concentrates with clearly increased surfactant content, on their production in the following the following.

Today's textile detergents in the form of pourable Powder and / or granules usually contain a combination nation of anionic and nonionic surfactants  Active washing components. Generally make the anionic surfactant components the larger part and the non-ionic surfactants the small one ren portion of the surfactant mixture. The total surfactant content for Powdery, free-flowing household detergent is around 12 up to a maximum of 15% by weight, based on the total detergent. The also applies to the detergents currently on the market increased bulk density. In contrast, the invention allows Application of the described method for manufacturing in the we Significant non-sticky, pourable and free-flowing storage stable Detergent and cleaning agent concentrates, especially corrections high concentrates for textile detergents with clearly excessive content of detergent surfactants. So can textile detergent concentrates with surfactant contents up to approx. 35 % By weight and preferably in the range from about 15 to 25% by weight be produced without adhesions and / or products divergences would be feared, as they are in the marketable powdery mixtures with such an increase in Surfactant content occur. By combining the measures the compression of the mixtures to high bulk densities and a simultaneous increase in the detergent ingredients, especially the amount of surfactants in the detergent mixed, the goal becomes more space-saving and less packaging Detergent preparations optimally realized without the area free-flowing storage stable and all other requirements having to leave fulfilling detergent preparations.

The preparation of detergents and cleaning agents in the invent method of granulation according to the invention for predeterminable Particle size has a number of advantages:

It has been shown that in the method according to the invention Bleach, especially sodium perborate in the form of  Monohydrate and / or tetrahydrate already in the too plastifi decorative and then processed raw material can be achieved without substantial loss of perborate to step. Each granulate thus contains the predetermined per borate content. The use of spray tower powders with variable Additions are possible. On the other hand, are here position of the raw materials to be compressed neither spray tower Powder still requires pre-formed powder with a bead structure. The use or addition of heavy powder of the individual raw fabrics is not required. Processing in washing and Detergents commonly used nonionic surfactants without any problems, which is usually the case here in spray drying occurring pluming problems are eliminated. The non-ionic surfactants will by incorporation into the mixture before extrusion fed easily, you can even use it as highly concentrated tes aqueous gel or paste valuable process aid in the perform described manner.

There is the production of detergents with an increased proportion any selected surfactants or surfactant mixtures possible has so far not been possible using the spray tower method. The possible incorporation of defoamers in liquid form saves a process for the separate production of defoaming mer solid carrier concentrates. This eliminates the Zumi Creation of defoamer granules in detergent processing tung.

By using extruder nozzle plates with freely selectable Hole nozzle diameters and adjustment of processing pressures there is the possibility of targeted product adaptation. It can bulk densities in the raw granulate, for example, up to 980 g / l can be set.  

The invention relates to a particular embodiment High-performance universal detergent for textiles used in the new Offer form of the free-flowing granules with bulk densities above 750 g / l, especially above 800 g / l, for example in Range from 850 to 950 g / l and in a particular important embodiment by a uniform particle shape and size are marked. The preferred particle shape is the spherical shape. Preferred particle sizes are in the range from about 0.5 to 5 mm ball diameter, especially in loading range from about 0.8 to 2 mm. The recipe components can the type and quantity of today's high-performance Tex detergents correspond. The fol information:

The main components of detergents and cleaning agents can be assigned to the following groups.

Surfactants in the form of anionic, nonionic, zwitterionic and / or cationic surfactant compounds.

So-called builder components, which on the one hand are soluble, on the other hand, as insoluble, finely divided materials come and thereby of an inorganic nature and / or organic Can be nature. Soluble inorganic builder materials are Tripolyphosphates, pyrophosphates and the like, soluble or ganic builder components are the poly mentioned above mer compounds, in particular of the type of acrylic acid homo- and / or copolymers. Insoluble builder components are ins especially the detergent-quality zeolites known today, Insoluble organic builder components are, for example finely divided ion exchange resins.

Soda, water glass and ver similar connections into consideration. Common bleaches are  perborates and / or other active oxygen carrier.

Other common mixture components of washing and cleaning agents are, for example, adjusting agents such as sodium sulfate or other salts, brighteners, enzymes, dirt-carrying agents, bleaching agents tivators, perfumes and the like.

For the composition of detergents and cleaning agents, esp special of textile detergents, both of the type of Special detergent as well as the type of universal detergent referenced to the extensive relevant literature as they results from the patent and other specialist literature.

Examples Examples 1 to 5

For the production of laundry detergents in the form of the Invention According to storage stable free-flowing compacts are in the Mixing ratios shown in Table 1 two previously separates obtained mixture components mixed together and worked up.

The first mixture component is a largely non-ionic surfactant-free tower spray powder based on the following main components (numerical values given in% by weight).
Surfactant mixture approx. 17.5%,
calcined soda approx. 35%,
Zeolite NaA approx. 22%,
Acrylic acid copolymer (Sokalan®) approx. 10%,
Water approx. 10%,
the rest of the usual detergent additives.

The second mixture component is a carrier bead containing high levels of non-ionic surfactant, which is composed of the following main components.
22% surfactant mixture,
Zeolite NaA approx. 55%,
Acrylic acid copolymer (Sokalan®) approx. 3%,
Water approx. 15%,
the rest sodium sulfate and other usual auxiliary substances.

In the procedure described in detail below the two mixture components are crushed and ver mixes, then the required amount of water and that in table  1 specified amount of 55% aqueous paste of alkyl benzenesulfonate pumped in. Finally, in Examples 1 to 3 sodium perborate monohydrate added and briefly added mixes.

The free-flowing material thus obtained becomes the homogenizing one Compaction and plasticization fed. The mass formed is extruded in the form of a strand, to form cylindrical granulate particles chipped, rounded and dried.

The following details apply:

Premix production

In a batch mixer (20 liters) equipped with a measuring device turret powder (TP) / carrier bead (TB) presented from production and approx. 0.5 min. mixed. At running mixer and cutter head chopper will be the required Amount of water and then the entire ABS paste over a Slotted nozzle pumped in (approx. 2.5 min.). In conclusion, he will if necessary, the total amount of Na perborate monohydrate added and approx. 1 min. mixed. The resulting Premix is free-flowing and can be used to load the continuous Kneader / extruder system can be used.

Kneader extruder / granulation

The premix obtained is continuously a two-screw ken kneader / extruder supplied, the housing including the Extruder pelletizing head are tempered to approx. 45 to 50 ° C. Under the shear of the extruder screws, the Vorge mixed plasticized and then through the extruder head Perforated nozzle plate to fine strands (1.0 and 1.2 mm diam ser) extruded, which after the nozzle exit by means of an Ab percussion knife into cylindrical pellets (Length / diameter ratio about 1).  

By blowing cold air into the granulating knife area the granules cooled to about 40 to 45 ° C and at the same time by removing surface water from sticking the Prevents pellets.

Rounding

The moist granulate obtained from the extruder granulation is in a marketable rounding machine of the type Marumerizer batchwise or continuously with the addition of zeolite Na Powder rounded off or deburred as a powder.

By varying the granulate residence time in the rounding machine and the Rotation speed of the device disc becomes the desired one Degree of rounding set.

Granulate drying

The moist granules from the rounding machine are in one Discounted fluidized bed dryer at a supply air temperature of approx. 75 to 80 ° C up to a product temperature of approx. 55 to 60 ° C dried. After cooling the product to approx. 30 ° C with Cold air is obtained as a free-flowing product.

Granulate screening

The very dust-free product is passed through a sieve with the Sieve 1.6 mm. The return share above In all cases, 1.6 mm was in the range of a maximum of 3%. The ge Seventh Gutkorn is used as the basis for mixing of detergent end products used.  

Table 1

Example 6

According to the procedure from Examples 1 to 5, a nio surfactant-free tower powder (ABS approx. 9%, calcined soda approx. 25%, Zeolite NaA approx. 38%, acrylic acid copolymer approx. 8%, water approx. 15%, the rest of the usual detergent ingredients) in one Amount of 88.5 wt .-% with 2.5 wt .-% water, 5 wt .-% Nio surfactant based on fatty alcohol ethoxylate (Dehydol LST 80/20) and 4 % By weight of 55% ABS Na paste added and worked up.

Free-flowing granulate balls with good grain Obtain bulk weights in the range of 900 to 950.

Example 7

An active ingredient mixture of tower powder and carrier bead is analog worked up Examples 1 to 5, but now as Plasti a 40% solution of the acrylic acid copolymer (Commercial product Sokalan CP 5®) in an amount of approx. 4.5 % By weight with the addition of water for plasticization (approx. 6 % By weight) are used, are in turn free-flowing and stable in storage nevertheless well water-soluble granules obtained in spherical form.

Example 8

In the sense of the teaching of Examples 1 to 5, the following are Mixing components used:

Free-flowing tower powder based on the following main components approx. 22% surfactant mixture, approx. 2.5% tallow-based Na soap, approx. 15% soda ash, approx. 7% water glass, approx. 26.5% zeolite NaA, approx. 7.5% acrylic acid copolymer, approx. 12% water, for The rest of the usual co-formulants.  

Carrier bead rich in nonionic surfactants based on the following main composition 22% surfactant mixture, sodium soap based on sebum approx. 2%, Zeolite NaA approx. 55%, acrylic acid copolymer approx. 3%, water approx. 15%.

Cut this according to the work instructions from Examples 1 to 5 The mixed and mixed good is approx. 11% (based on total mixture) of 60% ABS paste and homogenized. The resulting material is plasticized ver by kneading seals and presses to give shape. There are falling and pourable, easily washable pellet pellets with bulk densities in the range of 900 to 950 g / l.

Example 9

A phosphorus-free and pH-neutral special detergent subtower powder with the following composition
16% surfactant mixture,
Soap 2.8%,
Zeolite 16.0%,
Sokalan CP 5® 3.2%,
Na ₂ SO ₄ 58%
Rest of usual small components,
is intensively mixed with 5% by weight ABS paste (40%) and then first plasticized in an extruder and then extruded through a perforated disk with 1.2 mm nozzle bores. The temperature is controlled by tempering the jacket so that product temperatures of 45 to 50 ° C are set. The compressed mass strands emerging from the nozzle plate are cut off by rotating knives and thereby cylindrical particles with a length / diameter ratio of approx. 1 are obtained. The still warm particles are rounded in a Maru merizer with the addition of approx. 2% zeolite NaA powder and dried in a fluidized bed dryer as described above. After drying, products with bulk weights between approx. 850 and 920 g / l are obtained - the respective bulk weight depends on the extent of the rounding.

The preparation with approx. 3% of small detergents common in practice components (perfume, enzyme, optionally colored speckles) leads no significant change in the bulk weights.

Example 10

A mixture of 20% surfactants, 25% soda and 40% zeolite as well several small components are processed in a mixer and then sprayed with approx. 5% of a 55% ABS paste. Required If necessary, there will still be a small amount of additional water given the required moisture to the mixture of substances to give content that is used for densifying plasticization in Meaning of the teaching of the invention is required.

This plasticization with compression and compression of the compacted mass takes place in a pellet press. In more detail proceeded as follows.

The premix prepared as described above is over a Screw conveyor entered in the annulus of the pellet press. The The press consists of a rotating hollow roller into which - over the distributed over the entire circumference - radial holes are drilled. A press roll is arranged eccentrically in this ring die. During the tests, a ring die with a diameter is used of approx. 80 mm and approx. 500 holes. The bore diameter is 1.5 mm.

The screw dosing ensures a continuous feed product reached. In the gap between the roller and  the product is compacted in the die. Upon reaching the by the extrudability of the mass of defined pressure will Product pressed through the radial channels of the die and the entire strand pushed out by the appropriate length. By a knife attached to the outside of the die becomes the Each strand is cut to a length of approx. 1.5 mm. The cylindrical granules thus produced are used in another Process step rounded.

This is done by rolling off in a rounding machine. Depending on the dwell time (between 15 and 120 seconds) Rounding machines are either only rounded at the corners or obtained spherical granules.

In the rounding step, approx. 3% of an inorganic powder fabric - e.g. B. zeolite NaA - added, the strength the granules can still be improved.

By subsequent drying in a fluidized bed the water required for granulation dries again separated.

There are abrasion-stable and very free-flowing granules a bulk density of the dry products at approx. 950 g / l er hold.

Claims (25)

1. A process for the preparation of compacted solid granules of predetermined particle size from mixtures nigstens we partly solid fine-particle ingredients of detergents and / or cleaning products for home and Ge rack, in particular detergents for washing textiles, characterized in that the optionally blended liquid ingredients containing solid mixture with the addition of water-soluble, water-emulsifiable and / or water-dispersible plasticizers and / or lubricants worked up to a homogeneous, form-compressible mass, this mass over hole shapes with opening widths of the predetermined granule dimension extruded in a strand shape, the emerging compressed material strands to the predetermined granule dimension cut to length and, if desired, round off the still plastic granulate particles before they are acted upon by further active ingredients and / or to form granular, free-flowing granules be dried out. 2. The method according to claim 1, characterized in that one as a plasticizer and / or lubricant pasty until flowable preparations based on water-soluble or water emulsifiable polymer compounds and / or tensi Discher components used, with corresponding aqueous and / or water-miscible preparations are preferred. 3. The method according to claim 1 and 2, characterized net that you have conventional polymers or surfactant ingredients of washing and / or cleaning agents in preferably highly concentrated mixing with water and / or water soluble organic liquid phases as plasticizing and / or Lubricant is used, being pasty or gel-like  Formulations with a lubricating character may be preferred can. 4. The method according to claim 1 to 3, characterized in net that nonionic and / or anionic surfactants or Surfactant preparations in particular as highly concentrated Pastes and / or concentrated solutions from Polymerver bindings of natural and / or synthetic origin preferably in the field of textile detergents as plasticizers and / or lubricants are used. 5. The method according to claim 1 to 4, characterized in net that at least about 40 wt .-%, preferably we at least about 50% by weight surfactant pastes or gels, the can also contain soluble polymer compounds as Lubricants and / or plasticizers are used, usually these pastes in amounts not about 12% by weight, preferably at most about 10% by weight - each based on the total mixture - are used. 6. The method according to claim 1 to 5, characterized in net that the plasticizing aids and ge if necessary, additional small amounts of liquid in such Quantity uses that especially by kneading and possibly a moderate temperature increase in the majority material mixture the compacted and compressible cuttable texture set, at the same time its Tackiness is limited so that gluing ver of the primary granules can be prevented. 7. The method according to claim 1 to 6, characterized in net that the homogeneously compacted plasticized mass by extruder screws through perforated die plates and  the emerging material strands by means of high-speed Knife cutting devices cut to length or the homogeneous compacted mass in pellet presses or comparable Granulating devices processed to granulate. 8. The method according to claim 1 to 7, characterized in net that the compression using greatly increased Pressures, preferably at or above 50 bar, in particular those in the range of at least about 100 bar and at moderate raised melt temperatures z. B. in the range of 45 to 60 ° C and by shock cooling - especially using cold air - the emerging plasticized strands at least before and / or during their division cools and dries flat. 9. The method according to claim 1 to 8, characterized in net that in the mixture of substances to be compressed components that are used by immobilizing Binding of liquid components used, e.g. B. by binding of water as crystal water, for internal drying of the compacted granules. 10. The method according to claim 1 to 9, characterized in net that granulate bulk weights of at least 700 g / l, preferably set to at least 750 g / l, the preferred bulk densities of granules for the range of textile detergents at values above 800 g / l z. B. are in the range of about 850 to 1000 g / l. 11. The method according to claim 1 to 10, characterized in net that rounded and / or cylindrical Granules are formed that have a predetermined Size distribution spectrum meet, but preferably one in have substantially uniform size, the z. B. in  Diameter and / or length range from about 0.3 to 20 mm, preferably from about 0.8 to 3 mm. 12. The method according to claim 1 to 11, characterized in net that the pressed plasticized granulate blanks before, during or after rounding off with a finest partial dry powder, the one itself Ingredient of the finished product can be, in the context the production of laundry detergents Zeolite NaA in washing medium quality is preferred as dry powder. 13. The method according to claim 1 to 12, characterized in net that the granulate drying at maximum product temperature temperatures of about 55 to 60 ° C and preferably at one Supply air temperature of a maximum of about 75 to 80 ° C carried out becomes. 14. The method according to claim 1 to 13, characterized in net that sensitive recipe ingredients the granulate added after its formation, e.g. B. sprayed and / or be added. 15. Application of the method according to claims 1 to 14 for the production of essentially adhesive-free, bulk and free-flowing storage-stable detergents and cleaning agents Concentrates, in particular corresponding high concentrates for textile detergents with a significantly excessive content of Detergent ingredients, especially on active detergents Surfactant compounds. 16. Embodiment according to claim 15, characterized in net that textile detergent concentrates with surfactant contents up about 35% by weight, preferably in the range of about 15 to 25 % By weight are produced, in particular blends  of anionic surfactants and nonionic surfactant compounds have as surfactant ingredients. 17. Compacted to bulk densities of at least 700 g / l Free-flowing granules, at least containing Proportionally solid ingredients of washing and / or cleaning agents funds for household and / or trade in intimate Ab mix with dried water-soluble, water emulsifiable and / or water-dispersible mixture components as a concentrated preparation in water and / or water-miscible liquid phase lubricating character have. 18. Compacted compacts according to claim 17, characterized records that it has bulk weights of at least 750 g / l, preferably in the range of at least about 800 g / l exhibit, compacts for use in textile detergents Bulk weights in the range of about 800 to 1000 g / l to sit. 19. Compacted compacts according to claim 17 and 18, characterized characterized in that the water-soluble, water emulsifier baren and / or water-dispersible mixture components have a binder function in the dried compact and are preferably distributed homogeneously in the grain structure. 20. Compacted compacts according to claim 17 to 19, characterized characterized in that they are at least as low-dust compacts with average particle size in the range of about 0.2 to 20 mm, preferably about 0.5 to 5 mm and in particular in Range of about 0.8 to 3 mm are formed. 21. Compacted compacts according to claim 17 to 20, characterized characterized that they were at least partially rounded  Grain shape, preferably cylindrical and / or approximately to complete spherical shape with uniform or difference Lich spherical radius. 22. Compacted compacts according to claim 17 to 21, characterized characterized in that they are used as a dried component Binder character surfactants and / or water-soluble or contain water emulsifiable polymer compounds. 23. Compacted compacts according to claim 17 to 22, characterized characterized in that they consist of ingredients of textile detergents are built up and prefer the little the vast majority - based on total weight - make up the ready-to-use detergent mixture. 24. Detergents and / or cleaning agents for household and commercial use in pourable and pourable granulate form, thereby ge indicates that they at least partially from ver sealed, ingredients of detergents and cleaning agents containing solid granules exist after the Processes of claims 1 to 14 have been produced. 25. Granulated washing and cleaning agents according to claim 24, characterized in that - based on the spatial shape and / or the selection of the In compressed to granules Ingredients - just an essentially uniform one Have granules or at least two under contain different types of granules, which are preferred in homogeneous mixture and especially so are coordinated that spontaneous segregation in Storage and / or distribution are eliminated.