EP0603207A1

EP0603207A1 - Method of producing granular surfactant material.

Info

Publication number: EP0603207A1
Application number: EP92917099A
Authority: EP
Inventors: Volker Bauer; Jochen Jacobs; Ditmar Kischkel; Peter Kraeplin; Andreas Syldath
Original assignee: Henkel AG and Co KGaA
Current assignee: Henkel AG and Co KGaA
Priority date: 1991-08-20
Filing date: 1992-08-11
Publication date: 1994-06-29
Anticipated expiration: 2012-08-11
Also published as: ES2071513T3; EP0603207B1; US5516447A; DE4127323A1; ATE122387T1; DK0603207T3; CA2116104A1; WO1993004162A1; DE59202174D1; JPH06510070A; KR100204549B1

Abstract

PCT No. PCT/EP92/01831 Sec. 371 Date Feb. 22, 1994 Sec. 102(e) Date Feb. 22, 1994 PCT Filed Aug. 11, 1992 PCT Pub. No. WO93/04162 PCT Pub. Date Mar. 4, 1993.A process for the production of washing- and cleaning-active surfactant granules containing 60 to 70% by weight of surfactant and having an apparent density above 500 g/l, wherein a formulation containing a non-surface-active liquid component and having a liquid to paste-like form under normal pressure at temperatures of 20 DEG to 40 DEG C. is introduced to a fluidized bed and granulated and, at the same time, totally or partially freed from the non-surface-active liquid compound, optionally with addition of an inorganic or organic solid, and wherein the granules are discharged from the fluidized bed via a grading step by a countercurrent air-stream which is adjusted so that only particles above a predetermined size are removed from the granules.

Description

"Process for the Production of Surfactant Granules"

The invention relates to a method for converting liquid to pasty preparation forms of washable and cleaning-active surfactant compounds into storage-stable and dust-free granules with increased bulk density.

The economic synthesis of light-colored surfactant powders, in particular anionic surfactants based on fatty alkyl sulfates (FAS) and alkylbenzenesulfonates (ABS), is the current state of technical knowledge. The corresponding surfactant salts are obtained in aqueous preparation forms, water contents being adjustable in the range from about 20 to 80% by weight and in particular from about 35 to 60% by weight. Products of this type have a paste-like to cuttable quality at room temperature, the flowability and pumpability of such pastes being restricted or lost in the range of approximately 50% by weight of active substance at room temperature, so that they are stored and further processed Such pastes, particularly when incorporated into mixtures, for example in detergents and cleaning agents, pose considerable problems. Accordingly, it is an old need to provide detergent surfactants in a dry, especially free-flowing form. In fact, it is also possible to obtain free-flowing surfactant powders, for example free-flowing FAS powders, using the conventional drying technology, in particular in the spray tower. Here, however, there are serious restrictions which in particular call into question the economics of the large-scale use of the powders obtained in this way, in particular such FAS powders. FAS powder dried over the tower, for example, shows a very low bulk density, so that unprofitable conditions occur during the packaging and distribution of these powders, or these powders have to be compacted into heavier granules by granulation. But even in the manufacture of the tower powders, safety-related concerns can make such a restrictive manner of tower drying necessary that practical difficulties arise. Safety-related studies on tower powder based on FAS with 20% by weight or higher active substance contents show that the atomization technique of such formulations is only possible to a very limited extent and, for example, tower inlet temperatures required below 200 ° C. Another disadvantage of the spray drying TechM ^'k is that may occur in the tower caking, resulting in brown staining of the powder.

Comparable or other difficulties arise when converting aqueous, in particular paste-like, preparation forms of numerous other detergent-active and detergent-active compounds to storage-stable solids. Further examples of anionic oleochemical surfactant compounds are the known sulfofatty acid methyl esters (fatty acid methyl ester sulfonates, MES) which are obtained by sulfonating the methyl esters of fatty acids of vegetable or animal origin with predominantly 10 to 20 carbon atoms in the fatty acid molecule and subsequent neutralization to water-soluble mono-salts, in particular the corresponding alkali salts. The ester cleavage gives them the corresponding sulfo fatty acids or their di-salts, which, like mixtures of di-salts and sulfo-fatty acid methyl ester mono-salts, have important washing and cleaning properties. However, comparable problems also occur in other surfactant classes when trying to display the corresponding surfactant raw materials in dry form. Reference is made here to washing and cleaning-active alkyl glycoside compounds. In order to obtain light-colored reaction products, a final bleaching, for example with aqueous hydrogen peroxide, is generally required in their synthesis, so that here, too, today's technology leads to aqueous paste form. Such aqueous alkyl glycoside pastes (APG pastes) are more at risk from hydrolysis or microbial contamination, for example, than corresponding dry products. Here, too, simple drying according to the technologies customary to date presents considerable difficulties. Finally, drying an aqueous paste of the alkali salts of detergent soaps and / or ABS pastes can also cause considerable problems.

Granulation is an alternative to spray drying of surfactant pastes. European patent application EP 403 148 describes a process for producing FAS granules which are dispersible in cold water. This results in a highly concentrated aqueous FAS paste which contains less than 14% by weight of water and less than 20% by weight of further additives contains, mechanically processed at temperatures between 10 and 45 ° C until granules are formed. In this way, FAS granules are obtained which are already dispersed at washing temperatures between 4 and 30 ° C; however, the process temperature to be observed and the relatively low maximum water content of the surfactant paste are critical process parameters. In addition, it is not disclosed what bulk densities the granules produced by this process have.

A method for producing FAS and / or ABS granules is known from European patent application EP 402 112, the neutralization of the anionic surfactants in acid form to give a paste with a maximum of 12% by weight of water with the addition of auxiliaries such as polyethylene glycols, ethoxylated alcohols or alkylphenols, which have a melting point above 48 ° C, and the granulation takes place in a high-speed mixer. Again, the amount of water to be maintained represents a critical process parameter. In addition, it is not disclosed which bulk densities the surfactant granules obtained by this process have.

From European patent application EP 402 111, a process for the production of detergent-active granules with a bulk density of between 500 and 1200 g / l is known, a surfactant preparation form which contains water as the liquid component and can additionally contain organic polymers and builder substances a finely divided solid is added and granulated in a high-speed mixer. Here too, the water content of the surfactant paste is a critical process parameter. If the water content of the surfactant paste is too high, the solid is dispersed so that it can no longer act as a deagglomerating agent. On the other hand, if the solids content exceeds a certain value, the mass does not have the consistency necessary for the granulation.

The object of the invention was to provide a method for producing heavy, free-flowing surfactant granules, in which the content of a non-surfactant liquid component is not a critical process parameter. The invention accordingly relates to a process for the production of detergent-active granules having a bulk density above 500 g / l by granulating a surfactant preparation which has a non-surfactant liquid component, a surfactant preparation form which is used under normal pressure at temperatures between 20 and 40 ° C in liquid to pasty form, if desired granulated with the addition of an inorganic or organic solid and dried at the same time.

The process according to the invention has the advantage that it is not limited to the production of granules of only a few surfactants, but that free-flowing granules of anionic, nonionic, amphoteric, cationic surfactants and mixtures of these can be prepared by this process, the composition the granules can be predetermined. The production of anionic surfactants or nonionic surfactants or of mixtures of anionic surfactants and nonionic surfactants is preferred. In particular, the process according to the invention has advantages over the spray drying process, since the process according to the invention can also be used to produce granules which contain nonionic surfactants which, owing to their known pluming behavior, are not accessible by spray drying. In addition, due to the preferably lower process temperatures and gentle drying, there is no browning of the granules.

In a first embodiment, the surfactant preparation form used according to the invention, which is in liquid to pasty form under normal pressure at temperatures between 20 and 40 ° C., contains a mixture of one or more surfactants and a non-surfactant liquid component, the constituents contains organic and / or inorganic nature. In a further embodiment, the surfactant preparation form consists of at least two separate parts, the first of which is a mixture of one or more surfactants and a non-surfactant liquid component which contains constituents of organic and / or inorganic nature, and the second or the following Share either one or more surfactants present under normal pressure and at temperatures between 20 and 40 ° C in liquid to pasty form, which surfactants are at least partially from the Surfactants of the first part are different, or a further mixture of one or more surfactants, which are at least partially different from the surfactants of the first part, and a non-surfactant liquid component which contains constituents of organic and / or inorganic nature. A further embodiment of the invention provides that at least one component of the non-surfactant liquid component is not incorporated into the surfactant-containing parts of the surfactant preparation form, but is added separately. In the case of the quantitative data given below and related to the surfactant preparation form, however, it is assumed that in the surfactant preparation form both the individual surfactant-containing parts of the surfactant preparation form and components of the non-surfactant liquid composition may be used not included, which are added separately and not in a homogeneous mixture with surfactants.

The non-surfactant liquid component, which can contain one or more constituents, has a boiling point or boiling range under normal pressure, preferably below 250 ° C. and in particular below 200 ° C. The non-surfactant liquid component particularly advantageously contains constituents which boil between 60 and 180 ° C. at normal pressure. Mono- and / or polyfunctional alcohols, for example methanol, ethanol, propanol, isopropanol, butanol, secondary and tertiary butanol, pentanol, ethylene glycol, 1, are preferably used as an optional organic component of the non-tensi¬ dic liquid component. 2-propanediol, glycerol or mixtures of these are used. The proportion of the mono- and / or polyfunctional alcohols used as the non-surfactant liquid component is preferably 0.5 to 10% by weight, based on the surfactant preparation form.

In particular, however, it is preferred to use water as the inorganic component of the non-surfactant liquid component, optionally together with organic components such as ethanol, 1,2-propanediol or glycerol. The proportion of water is preferably 25 to 80% by weight, based on the surfactant preparation form. The total proportion of the non-surfactant liquid component is preferably 30 to 70 % By weight and in particular 45 to 60% by weight, based in each case on the surfactant preparation form.

Anionic surfactants used are, for example, those of the sulfonate and sulfate type. Suitable surfactants of the sulfonate type olefin sulfonates, ie mixtures of alkene and hydroxyalkanesulfonates and also disulfonates, as obtained, for example an internal of Ci2-CI8 Mon-_ ^'] efinen _m jt _enc j_ _un d double bond are preferably C-_i3 alkylbenzenesulfonates, by Sulphonation with gaseous sulfur trioxide and subsequent alkaline or acid hydrolysis of the sulfonation products is considered. Also suitable are alkanesulfonates which can be obtained from C 1 -C 18 -alkanes by sulfochlorination or sulfoxidation and subsequent hydrolysis or neutralization. In particular, esters of α-sulfofatty acids (ester sulfonates) which, by oc-sulfonation of the methyl esters of fatty acids of vegetable and / or animal origin with 10 to 20 C atoms in the fatty acid molecule and subsequent neutralization, are converted into water-soluble mono-salts by the process according to the invention. for example the o-sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids, and the oc-sulfofatty acids or their di-salts obtainable by ester cleavage. The preparation of mixtures of the mono-salts and di-salts with further surfactants, for example with alkylbenzenesulfonates, is also preferred.

Suitable surfactants of the sulfate type are the sulfuric acid monoesters from primary alcohols of natural and synthetic origin, in particular from fatty alcohols, for example from coconut fatty alcohols, tallow fatty alcohols, oleyl alcohol, lauryl, myristyl, palmityl or stearyl alcohol, or the Cιn-C20-0x ° ^a lkoholen and those of secondary alcohols of this length Ketten¬. The sulfuric acid monoesters of the alcohols ethoxylated with 1 to 6 mol of ethylene oxide, such as 2-methyl-branched Cg-Cji alcohols with an average of 3.5 mol of ethylene oxide, are also suitable. Sulfated fatty acid monoglycerides are also suitable. In particular, however, is the production of surfactant granules which (FAS) or Ciss-Cig alkyl sulfates (TAS) alone or together with other surfactants, preferred. Other anionic surfactants which can be prepared in granular form by the process according to the invention include soaps made from natural or synthetic, preferably saturated or ethylenically unsaturated, fatty acids. Soap mixtures derived from natural fatty acids, for example coconut, palm kernel or tallow fatty acids, are particularly suitable. Preferred are those which are composed of 50 to 100% saturated C12-Ci8 fatty acid soaps and 0 to 50% oleic acid soaps. In particular, granules are produced by the process according to the invention which contain soap mixed with other surfactants.

The anionic surfactants can be used in the form of their sodium, potassium, calcium and ammonium salts and as water-soluble salts of organic bases, such as mono-, di- or triethanolamine. They are preferably used in the form of aqueous preparations, in particular in the form of about 30 to 60% by weight aqueous preparations in which the anionic surfactants are obtained in the course of their preparation by neutralizing the corresponding acids.

Granules produced by the process according to the invention preferably contain nonionic surfactants, in particular together with anionic surfactants, for example alkylbenzenesulfonate and / or fatty alkyl sulfate. The nonionic surfactants are preferably derived from liquid ethoxylated, in particular primary alcohols with preferably 9 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide per mole of alcohol, in which the alcohol residue can be linear or methyl-branched in the 2-position, or can contain linear and methyl-branched radicals in the mixture, as are usually present in oxo alcohol radicals. In particular, however, linear residues of alcohols of native origin with 12 to 18 carbon atoms, such as, for example, coconut oil, tallow fat or oleyl alcohol, are preferred. The degrees of ethoxylation given represent statistical averages, which can be an integer or a fraction for a specific product. Preferred alcohol ethoxylates have a restricted homolog distribution (narrow ranks ethoxylates, nre). In particular, alcohol ethoxylates are preferred which have an average of 2 to 8 ethylene oxide groups. The preferred ethoxylated alcohols include, for example, Cg-Cu Oxo alcohol with 7 EO, Ci3-Ci5-0xo alcohol with 3 EO, 5 EO or 7 EO and in particular Ci2-Ci4 alcohol with 3 EO or 4 EO, Ci2-Ci8 alcohols with 3 EO, 5 EO or 7 EO and Mixtures of these, such as mixtures of Ci2-Ci4 alcohol with 3 EO and Cχ2-Ci8 alcohol with 5 EO.

Furthermore, the granules produced by the process according to the invention can be used as nonionic surfactants, alkyl glycosides of the general formula R-0- (G) _x , in which R is a primary straight-chain or aliphatic radical branched in the 2-position with 8 to 22, preferably 12 to 18 Atoms means G is a symbol which stands for a glycose unit with 5 or 6 C atoms, and the degree of oligomerization x is between 1 and 10, preferably between 1 and 2 and in particular is significantly less than 1.4.

The proportion of the surfactants is preferably 20 to 75% by weight and in particular 35 to 70% by weight, in each case based on the surfactant preparation form.

The surfactant preparation form preferably contains, as further constituents, additives which are ingredients of detergents and cleaning agents. In particular, surfactant preparations which contain additives in amounts of 0.001 to 15% by weight, based on the surfactant preparation form, are used in the process according to the invention. Particularly preferred additives are dyes, foam inhibitors, bleaches and / or constituents which improve solubility.

Suitable dyes are temperature-stable dyes, preferably pigment dyes, which are advantageously used in amounts of 0.001 to 0.5% by weight, based on the surfactant preparation form.

Suitable foam inhibitors are, for example, soaps of natural and synthetic origin which have a high proportion of Ci8-C24 " ^Fe " t acids. Suitable non-surfactant-like foam inhibitors are organopolysiloxanes and their mixtures with microfine, optionally silanized silica, paraffins, waxes, microcrystalline waxes and their mixtures with silanized silica. Bisacylamides derived from Ci2-C20-alkylamines and C2-Cδ-dicarboxylic acids can also be used. Be an advantage too Mixtures of various foam inhibitors are used, for example those made from silicones and paraffins or waxes. The foam inhibitors are preferably bound to a granular, water-soluble or dispersible carrier substance. The content of foam inhibitors in the surfactant preparation form is preferably 0.01 to 0.5% by weight.

Among the compounds which serve as bleaching agents and supply H2O2 in water, sodium perborate tetrahydrate and sodium perborate monohydrate are of particular importance. Other useful bleaching agents are, for example, peroxy carbonate, peroxypyrophosphate, citrate perhydrate, peroxaphthalate, diperazelaic acid or diperdodecanedioic acid. In particular, it is also preferred to use hydrogen peroxide as a bleaching agent in surfactant preparation forms which are used according to the invention. The content of bleach in the surfactant preparation form is preferably 0.5 to 15% by weight, in particular the content of hydrogen peroxide is 0.5 to 5% by weight.

The constituents which improve the solubility include liquid, pasty and solid compounds which are soluble or dispersible in the other constituents of the surfactant preparation form. Preferred solubility-improving constituents are polyethylene glycols with a relative molecular weight between 200 and 20,000 and highly ethoxylated fatty alcohols with 14 to 80 ethylene oxide groups per mole of alcohol, in particular Ci2-Ci8 fatty alcohols with 20 to 60 ethylene oxide groups, for example tallow fatty alcohol with 30 E0 or 40 E0 used. The use of polyethylene glycols with a relative molecular weight between 200 and 600 is particularly preferred. These polyethylene glycols are advantageously used as a separate constituent of the non-surfactant liquid component. The content of the surfactant preparation form in these constituents which improve the solubility of the finished granules is preferably 1 to 15% by weight and in particular 2 to 10% by weight.

The surfactant preparation form is granulated and dried at the same time. "Drying" is understood to mean the partial or complete removal of the non-surfactant liquid component. If desired, residual values of free, i.e. unbound water and / or mono- and / or polyfunctional alcohols as long as the finished ones

Granules are free-flowing and non-sticky. However, one is preferred

Free water content of 10% by weight and in particular from 0.1 to 2

% By weight, based in each case on the finished granules, not exceeded.

According to the invention, the surfactant granules can be produced in all devices in which granulation can be carried out with simultaneous drying. Examples of this are heatable mixers and granulators, in particular granulators of the Turbo dryer (R) type (device from Vomm, Italy). In a preferred embodiment, however, the invention provides that the combination of these two process steps is carried out in a batch or continuous fluidized bed. It is particularly preferred to carry out the process continuously in the fluidized bed. The surfactant preparation form or the individual parts of the surfactant preparation form can be introduced into the fluidized bed simultaneously or in succession via one, for example via a nozzle with several openings or via several nozzles. It is also possible to add a component of the non-surfactant liquid component which has not been incorporated into the surfactant preparation form simultaneously and separately. The nozzle or the nozzles and the direction of spraying of the products to be sprayed can be arranged as desired. Vortex layer apparatuses used with preference have base plates with dimensions of at least 0.4. In particular, fluidized bed apparatuses are preferred which have a base plate with a diameter between 0.4 and 5 m, for example 1.2 m or 2.5. However, fluidized bed apparatuses are also suitable which have a base plate with a diameter greater than 5 m. A perforated base plate or a Conidur plate (commercial product from Hein & Lehmann, Federal Republic of Germany) is preferably used as the base plate. The process according to the invention is preferably carried out at swirl air speeds between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s. The granules are advantageously discharged from the fluidized bed by grading the size of the granules. This classification can take place, for example, by means of a sieving device or by means of an opposed air flow (classifier air) which is regulated in such a way that only particles of a certain particle size out the fluidized bed is removed and smaller particles are retained in the fluidized bed. In a preferred embodiment, the inflowing air is composed of the heated or unheated classifier air and the heated soil air. The soil air temperature is preferably between 80 and 400 ° C, in particular between 90 and 350 ° C. The fluidized air cools down through heat losses and through the heat of vaporization of the constituents of the non-surfactant liquid component. In a particularly preferred embodiment, the temperature of the vortex air is approximately 5 cm above the base plate 60 to 120 ° C., preferably 65 to 90 ° C. and in particular 70 to 85 ° C. The air outlet temperature is preferably between 60 and 120 ° C, in particular below 100 ° C and particularly advantageously between 70 and 85 ° C. In the process which is preferably carried out in the fluidized bed, it is necessary for a starting mass to be present at the start of the process and which serves as an initial carrier for the sprayed-in surfactant preparation form. Ingredients of detergents and cleaning agents are particularly suitable as starting mass, in particular those which can also be used as solids in the process according to the invention and which have a particle size distribution which corresponds approximately to the particle size distribution of the finished granules. In particular, however, it is preferred to use as the starting mass surfactant granules which have already been obtained in a previous process.

The components of the non-surfactant liquid component evaporate partially or completely in the fluidized bed. Dried to dried germs are formed, which are coated with further quantities of the surfactant preparation form, granulated and in turn dried at the same time.

A particularly important embodiment provides that the surfactant preparation form is granulated with the addition of an inorganic or organic solid and dried at the same time, it being possible for the solid to be pneumatically dusted in via blow lines. This solid, which serves as a carrier for the surfactant preparation form, preferably consists of ingredients from washing and cleaning agents. Suitable solids are, for example, surfactants or surfactant mixtures which by granulation, by spray drying or according to the invention

Processes have been prepared and recycled to increase the surfactant concentration in the finished granules. In particular, the use of spray-dried and / or obtained by the inventive method

Preferred surfactant granules. As solids - as an alternative to incorporation into the surfactant preparation form - it is also advantageous to use highly ethoxylated ones

Fatty alcohols with, for example, 20 to 80 EO, preferably 20 to 60 E0 and in particular tallow fatty alcohol with 30 or 40 E0 can be used.

In a further preferred embodiment, non-surfactant ingredients of detergents and cleaning agents, preferably one or more constituents from the group of the alkali carbonates, alkali sulfates, crystalline and amorphous alkali silicates and layered silicates, and zeolite, in particular zeolite NaA in detergent quality, are used as solids, Salts of citric acid, solid peroxy bleaching agents and optionally bleach activators and solid polyethylene glycols with a relative molecular weight greater than or equal to 2,000, in particular between 4,000 and 20,000, are used.

Preference is given to using finely divided materials as solids, which can either be produced directly in this state, are commercially available, or are converted into this finely divided state by conventional comminution methods, for example by grinding with conventional mills. Preferred solids have, for example, no more than 5% by weight of particles with a diameter above 2 mm and preferably no more than 5% by weight of particles with a diameter above 1.6 mm. In particular, solids are preferred which consist of at least 90% by weight of particles with a diameter below 1.0 mm. Examples of these are alkali carbonates with more than 90% by weight of particles with a diameter of less than or equal to 0.5 mm and zeolite NaA powder in detergent quality, which contains at least 90% by weight of particles with a diameter below 0 , 03 mm contains. The added solids are used with particular advantage in amounts of 10 to 50% by weight and in particular 20 to 45% by weight, based in each case on the sum of the surfactant preparation form and the solid. In a further embodiment, the surfactant granules which can be produced by the process according to the invention are claimed. Preferred surfactant granules have a surfactant content of 10 to 100% by weight, in particular 30 to 80% by weight and with particular advantage between 40 and 70% by weight, in each case based on the finished granules. Pure surfactant granules are obtained when the non-surfactant liquid component is completely evaporated and the granules are thus dried completely and the solid that may be added consists of a pure surfactant material. In this case, surfactant granules which have been produced by the process according to the invention and now serve as a solid in the process according to the invention are optionally comminuted to the desired particle size distribution and recycled. The content of surfactants in the granules can be adjusted to any of the desired values.

The surfactant granules obtained by the process according to the invention preferably have a bulk density of between 550 and 1000 g / 1, in particular between 550 and 850 g / 1, and are dust-free, ie they contain in particular no particles with a particle size below 50 μm. Otherwise, the particle size distribution of the surfactant granules corresponds to the usual particle size distribution of a heavy detergent of the prior art. In particular, the surfactant granules have a particle size distribution in which a maximum of 5% by weight, preferably a maximum of 3% by weight of the particles have a diameter above 2.5 mm and a maximum of 5% by weight, with particular advantage a maximum of 3% by weight. % of the particles have a diameter below 0.1 mm. The surfactant granules are distinguished by their light color and their free-flowing properties. A further measure to prevent the surfactant granules produced according to the invention from sticking together is not necessary. If desired, however, a process step can be followed, the surfactant granules being powdered in a known manner with finely divided materials, for example with zeolite NaA, soda, in order to further increase the bulk density. This powdering can be carried out, for example, during a rounding step. However, preferred surfactant granules already have such a regular, in particular approximately spherical, structure that a Rounding step is generally not necessary and is therefore also not preferred.

B e i s p i e l e

In Examples 1 to 10, a surfactant preparation form, which could consist of one or more separate parts, was granulated through a nozzle and a system for granulation drying (AGT) from Glatt, Bundesrepubli Germany, together with a solid and simultaneously dried. A surfactant granulate was used as the starting mass, since a previous batch had been used (under the same process conditions) and had approximately the same composition as the finished granules from Examples 1 to 10. The process conditions can be found in Table 1.

The following substances were used in the surfactant preparation form:

Sulfopon ( ^R ) T 55, containing 54% by weight tallow fatty alcohol sulfate and approx. 41

Wt .-% water (commercial product of Anmdelders) OO Texapon LS 35, containing 34 wt .-% Ci2 ^_ C_4 fatty alcohol sulfate and ca.

64% by weight of water (commercial product of the applicant) Dehydol 00 LT 7, containing 99% by weight with 7 E0

(Applicant's commercial product) Texin ( ^R ) ES 68, containing 53% by weight sodium mono salt of

Tallow fatty acid methyl ester, 11% by weight disodium salt of

Sulfotalg fatty acid and approx. 33% by weight water

(Applicant's commercial product) PEG 400, polyethylene glycol with a molecular weight of

400

These parts were introduced into the fluidized bed separately and simultaneously via a nozzle.

The following were used as solids:

Soda, sodium carbonate with a bulk density of 620 g / 1

(Commercial product from Matthes & Weber, Federal Republic of Germany) Wessalith OO P, zeolite powder (commercial product from Degussa,

Federal Republic of Germany) Carrier bead, zeolite granules, containing 67% by weight of zeolite

(calculated anhydrous), 11 wt .-% of a poly eren

Polyacrylate, 1.85% by weight taig fatty alcohol with 5 EO, 2

% By weight sodium sulfate and 17% by weight water citrate, trisodium citrate EP powder (dihydrate, commercial product of

Jungbunzlauer, Federal Republic of Germany) Sulfopon OO T, tallow fatty alcohol sulfate powder (commercial product of

B 5, ground product of Example 5 (particle size distribution corresponding to sulfopone 00 T)

Dust-free and non-sticky granules with high surfactant contents were obtained in all examples (see Table 2). The proportion of granules with a grain size above 2.5 m was below 5% by weight in all examples.

Table 1: Process parameters

Examples 3_ "4 8 10

fluidized bed

- Diameter in mm 400 1200 1200 400 400 400 400 400 400 400

- Area in m ² 0.13 1.13 1.13 0.13 0.13 0.13 0.13 0.13 0.13 0.13

Vortex air velocity in m / s 5.1 2.35 2.62 2.8 2.6 2.6 2.7 2.6 2.6 2.6 (under operating conditions)

I.

71 75 82 70 73 71

Airflow in π-Vh 2341 9563 10685 1300 1180 1180 1220 1180 1190 1190

(under operating conditions)

Continued Table 1 Air load (g H θ / kg air) 3.8 14 13

Throughput of surfactant preparation in kg / h

Sulfopon OO T 55 20 50

Texapon OO LS 35 Dehydol OO LT 7 Texin OO ES 68 30 PEG 400

Throughput of solids in kg / h

00 soda 12 60 370 19 5.4 I

WessalithOO p 13.6 carrier bead 25 citrate 15

Sulfopon OO T 20 20 B 5 19

Starting mass in kg 25 120 120 20 20 20 20 20 20 20

Table 2: Characteristics of the products

Examples 3 4 8 10

Total surfactant content in% by weight water content in% by weight

Bulk density in g / 1 790 615 580 630 512 540 655 505 675 685 sieve analysis in% by weight

2.5 mm 1.9 - - - - - ~

1.6 mm 97.2 6.1 17.1 9.8 24.9 27.0 0.3 13.1 0.7 4.8 0.8 mm 2.8 6.2 14.0 44.4 72. 8 64.0 38.1 86.0 51.3 23.0 0.6 mm 0.0 7.9 57.7 23.6 1.0 5.4 48.4 0.8 38.6 14.7 0.4 mm - 23.7 8.4 16.4 0.6 2.8 12.0 0.1 8.6 18.7 I 0.2 mm - 40.2 0.9 4.8 0.4 0.6 0.9 - 0.6 22.0 0.1 mm - 14.0 - 1.0 0.3 0.2 0.2 - 0.2 14.3

0.05 mm - 1.8 0.1 2.5

<0.05 mm - - - - - - - - - -

* including water from zeolite

Claims

Patent claims

1. A process for the production of detergent-active and surfactant granules with a bulk density above 500 g / 1 by granulation of a surfactant preparation form which has a non-surfactant liquid component, characterized in that a surfactant preparation form which is under normal pressure at temperatures between 20 and 40 ° C is in liquid to pasty form, if desired granulated with the addition of an inorganic or organic solid and dried at the same time.

2. The method according to claim 1, characterized in that the surfactant preparation form surfactants or surfactant mixtures from the group of anionic, nonionic, amphoteric and cationic surfactants, preferably anionic surfactants, especially fatty alkyl sulfates, Cg-Ci3-alkylbene benzenesulfonates and sulfofatty acid methyl esters, and / or nonionic surfactants, in particular liquid ethoxylated fatty alcohols containing 2 to 8 ethylene oxide groups per mole of alcohol.

3. The method according to claim 1 or 2, characterized in that the surfactant preparation form consists of at least two separate parts, of which the first part is a mixture of one or more surfactants and a non-surfactant liquid component, the components of organic and / or contains inorganic nature, and the second part or the following parts each have either one or more surfactants present in liquid to pasty form under normal pressure and at temperatures between 20 and 40 ° C. which are at least partially different from the surfactants of the first part, or a further mixture of one or more surfactants which are at least partially different from the surfactants of the first part and a non-surfactant liquid component which contains constituents of an organic and / or inorganic nature.

4. The method according to claims 1 to 3, characterized in that the non-surfactant liquid component under normal pressure boils below 250 ° C, preferably below 200 ° C and in particular between 60 and 180 ° C. 5. The method according to claim 4, characterized in that as non-ten¬ liquid liquid component mono- and / or polyfunctional alcohols, preferably in amounts of 0,

5 to 10 wt .-%, based on the surfactant preparation form, are used.

6. The method according to claim 4 or 5, characterized in that water is used as the non-surfactant liquid component, preferably in amounts of 25 to 80 wt .-%, based on the surfactant preparation form.

7. The method according to any one of claims 1 to 6, characterized in that the surfactant preparation form additives, which are ingredients of detergents and cleaning agents, preferably in amounts of 0.001 to 15 wt .-%, based on the surfactant preparation form .

8. The method according to claim 7, characterized in that dyes, defoamers, bleaches and / or solubility-improving constituents, in particular polyethylene glycols with a relative molecular weight between 200 and 600, are used as additives.

9. The method according to any one of claims 1 to 8, characterized in that the granulation and simultaneous drying in a fluidized bed is carried out batchwise or continuously, preferably continuously.

10. The method according to claim 9, characterized in that the surfactant preparation form or the individual parts of the surfactant preparation form is introduced into the fluidized bed simultaneously or successively via one or more nozzles.

11. The method according to claim 9 or 10, characterized in that the vortex air velocity is between 1 and 8 m / s, preferably between 1.5 and 5.5 m / s.

12. The method according to any one of claims 9 to 11, characterized in that the granules are discharged from the fluidized bed via a size classification of the granules.

13. The method according to any one of claims 9 to 12, characterized in that the Bodenluftte temperature between 80 and 400 ° C, preferably between 90's and 350 ° C, the temperature of the vortex air about 5 cm above the base plate between 60 and 120 ° C, preferably between 65 and 90 ° C and in particular between 70 and 85 ° C, and the air outlet temperature between 60 and 120 ° C, preferably below 100 ° C and in particular between 70 and 85 ° C.

14. The method according to any one of claims 1 to 13, characterized in that the solids are surfactants or surfactant mixtures, preferably spray-dried surfactants and / or surfactant granules and / or highly ethoxylated fatty alcohols containing 20 according to one of claims 1 to 11 up to 80 ethylene oxide groups.

15. The method according to any one of claims 1 to 14, characterized in that the solids are non-surfactant ingredients of detergents and cleaning agents, preferably one or more constituents from the group of alkali metal carbonates, alkali metal sulfates, crystalline and amorphous alkali metal silicates and sheet silicates, and zeolite, salts citric acid, solid peroxy bleaching agents and optionally bleach activators and solid polyethylene glycols with a relative molecular mass greater than or equal to 2,000, in particular between 4,000 and 20,000, are used.

16. The method according to any one of claims 1 to 15, characterized in that the added solids in an amount of 10 to 50 wt .-% and in particular from 20 to 45 wt .-%, each based on the sum of the surfactant preparation form and Solid, can be used.

17. surfactant granules, produced according to one of claims 1 to 16, characterized in that it is 10 to 100 wt .-%, preferably 30 to Contains 80 wt .-% and in particular 40 to 70 wt .-%, each based on the finished granules, of surfactants.

18. surfactant granules according to claim 17, characterized in that it has a bulk density between 550 and 1000 g / 1, preferably between 550 and 850 g / 1.

19. Surfactant granules according to claim 17 or 18, characterized in that it contains no particles with a particle size below 50 microns.

20. surfactant granules according to any one of claims 17 to 19, characterized gekenn¬ characterized in that it has a regular structure, in particular an approximately spherical shape.