EP0603207B1 - Method of producing granular surfactant material - Google Patents

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

The invention relates to a process for the production of detergent granules which are active in washing and cleaning, and to a surfactant granulate produced by the process according to claim 17. The storage-stable and dust-free granules have an 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 now a state of the art. 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 cutable quality at room temperature, the flowability and pumpability of such pastes being restricted or lost at around 50% by weight of active substance at room temperature, so that during storage and further processing of such pastes, Considerable problems arise in particular when they are incorporated into mixtures, for example in detergents and cleaning agents. 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 powder, using conventional drying technology, especially in the spray tower. Here, however, there are serious restrictions which in particular call into question the economics of the industrial use of the powders obtained in this way, in particular such FAS powders. FAS powder dried over the tower, for example, has a very low bulk density, so that unprofitable conditions occur in 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, for example tower inlet temperatures required below 200 ° C. Another disadvantage of spray drying technology is that caking can occur in the tower, which leads to brown discolouration of the powder.

Comparable or other difficulties arise in the conversion of aqueous, in particular pasty, 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 by α-sulfonation of the methyl esters of fatty acids of plant or animal origin with predominantly 10 to 20 carbon atoms in the fatty acid molecule and subsequent neutralization to form water-soluble mono salts, in particular the corresponding alkali salts. The ester cleavage gives them the corresponding sulfofatty acids or their di-salts, which, like mixtures of di-salts and sulfofatty 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 should be made here to detergent-active and alkylglycoside 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 the 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 hitherto 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. For example, European patent application EP 403 148 describes a process for producing FAS granules which are dispersible in cold water. A highly concentrated aqueous FAS paste is used 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 and ethoxylated alcohols or alkylphenols, which have a melting point above 48 ° C., and the granulation is carried out in a high-speed mixer. Again, the amount of water to be maintained is a critical process parameter. In addition, it is not disclosed what 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 and granular surfactants with a bulk density between 500 and 1200 g / l is known, whereby a surfactant preparation form which contains water as a 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.

From European patent application EP-A-0 364 881 a process for the production of free-flowing, surfactant-containing granules with a bulk density of 650 to 1000 g / l is known, a surfactant preparation containing water [ie, a non-surfactant liquid component] , is first granulated and then (optionally) dried. In this known surfactant preparation form, which is necessarily present under normal pressure at temperatures between 20.degree. C. and 40.degree. C. in liquid to pasty form, the drying stage takes place at different times from the granulation and not at the same time as this last.

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 with a bulk density above 500 g / l by granulation of 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 of the granules can be predetermined. The production of anionic surfactants or nonionic surfactants or 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 of organic and / or contains 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. Another 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 mentioned, but is added separately. However, in the case of the amounts indicated below and based on the surfactant preparation form, it is assumed that the individual surfactant-containing parts of the surfactant preparation form as well as constituents of the non-surfactant liquid component, which are separate and not, are included in the surfactant preparation form be added 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, 1,2-propanediol, glycerol or, are preferably used as the optional organic constituent of the non-surfactant liquid component 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, in each case based on the surfactant preparation form.

Anionic surfactants used are, for example, those of the sulfonate and sulfate type. Preferred surfactants of the sulfonate type are C₉-C₁₃ alkylbenzenesulfonates, olefin sulfonates, i.e. Mixtures of alkene and hydroxyalkanesulfonates and disulfonates, such as those obtained, for example, from C₁₂-C₁₈ monoolefins with terminal and internal double bonds by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acidic hydrolysis of the sulfonation products, are considered. Also suitable are alkanesulfonates which are obtainable from C₁₂-C₁₈ alkanes by sulfochlorination or sulfoxidation and subsequent hydrolysis or neutralization. In particular, esters of α-sulfofatty acids (ester sulfonates) which, by α-sulfonation of the methyl esters of fatty acids of plant 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, for example, by the process according to the invention the α-sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids, and the α-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 oil alcohols, tallow fatty alcohols, oleyl alcohol, lauryl, myristyl, palmityl or stearyl alcohol, or the C₁₀-C₂₀ oxo alcohols, and those and this chain length. The sulfuric acid monoesters of alcohols ethoxylated with 1 to 6 moles of ethylene oxide, such as 2-methyl-branched C₉-C₁₁ alcohols with an average of 3.5 moles of ethylene oxide, are suitable. Sulfated fatty acid monoglycerides are also suitable. In particular, however, the production of surfactant granules containing C₁₂-C₁₈ alkyl sulfates (FAS) or C₁₆-C₁₈ alkyl sulfates (TAS) alone or together with other surfactants is preferred.

Other anionic surfactants that can be produced in granular form by the process according to the invention include soaps made from natural or synthetic, preferably saturated or ethylenically unsaturated, fatty acids. Natural fatty acids, e.g. Soap mixtures derived from coconut, palm kernel or tallow fatty acids. Preferred are those which are composed of 50 to 100% of saturated C₁₂-C₁₈ fatty acid soaps and 0 to 50% of oleic acid soaps. In particular, the process according to the invention produces granules 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 during 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 radical can be linear or methyl-branched in the 2-position, or linear and may contain methyl-branched radicals in the mixture, as are usually present in oxo alcohol radicals. However, linear residues of alcohols of native origin with 12 to 18 carbon atoms, such as, for example, coconut oil, tallow oil or oleyl alcohol, are particularly 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 range 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, C₉-C₁₁ oxo alcohol with 7 EO, C₁₃-C₁₅ oxo alcohol with 3 EO, 5 EO or 7 EO and in particular C₁₂-C₁₄ alcohol with 3 EO or 4 EO, C₁₂-C₁₈ alcohols with 3 EO, 5 EO or 7 EO and mixtures of these , such as mixtures of C₁₂-C₁₄ alcohol with 3 EO and C₁₂-C₁₈ 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 RO- (G) _x , in which R is a primary straight-chain or aliphatic radical with 8 to 22, preferably 12 to 18, carbon atoms in the 2-position , G is a symbol which stands for a glycose unit with 5 or 6 carbon 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 C₁₈-C₂₄ fatty 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 C₁₂-C₂₀ alkylamines and C₂-C₆ dicarboxylic acids are also useful. Be an advantage too Mixtures of various foam inhibitors are used, for example those made from silicone and paraffins or waxes. The foam inhibitors are preferably bound to a granular, water-soluble or dispersible carrier substance. The foam inhibitor content of the surfactant preparation form is preferably 0.01 to 0.5% by weight.

Of the compounds used as bleaching agents which 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. 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 C₁₂-C₁₈ fatty alcohols with 20 to 60 ethylene oxide groups, for example tallow fatty alcohol with 30 EO or 40 EO, are preferably used as constituents which improve solubility . 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 component 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, ie unbound water and / or mono- and / or polyfunctional alcohols are present as long as the finished granules are free-flowing and non-sticky. However, a free water content of 10% by weight and in particular 0.1 to 2% by weight, based in each case on the finished granules, is preferably 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. Fluidized bed apparatuses which are preferably used have base plates with dimensions of at least 0.4 m. 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 m. 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 fluidizing air speeds between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s. The granules are discharged from the fluidized bed advantageously by means of a size classification 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 vortex air cools down due to heat losses and the heat of vaporization of the components 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 beginning 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 surfactant granules as starting mass 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 dusted pneumatically 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 were produced by granulation, by spray drying or by the process according to the invention and are recycled to increase the surfactant concentration in the finished granulate. In particular, the use of spray-dried and / or surfactant granules obtained by the process according to the invention is preferred. Highly ethoxylated fatty alcohols with, for example, 20 to 80 EO, preferably 20 to 60 EO and in particular tallow fatty alcohol with 30 or 40 EO can also advantageously be used as solids - as an alternative to incorporation into the surfactant preparation form.

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, salts of citric acid, are used as solids, 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 . 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 completely dried and the solid that may be added consists of a pure surfactant material. In this case, surfactant granules which have been prepared by the process according to the invention and now serve as a solid in the process according to the invention are preferably comminuted to the desired particle size distribution and recycled. The content of surfactants in the granules can be set to any of the desired values.

The surfactant granules obtained by the process according to the invention preferably have a bulk density between 550 and 1000 g / l, in particular between 550 and 850 g / l, and are dust-free, that is to say in particular they contain 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 characterized 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 usually not necessary and is therefore not preferred.

Examples

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

Sulfopon ^(R) T 55,

enthaltend 54 Gew.-% Talgfettalkoholsulfat und ca. 41 Gew.-% Wasser (Handelsprodukt des Anmdelders)

Texapon ^(R) LS 35,

enthaltend 34 Gew.-% C₁₂-C₁₄-Fettalkoholsulfat und ca. 64 Gew.-% Wasser (Handelsprodukt des Anmelders)

Dehydol ^(R) LT 7,

enthaltend 99 Gew.-% C₁₂-C₁₈-Fettalkohol mit 7 EO (Handelsprodukt des Anmelders)

Texin ^(R) ES 68,

enthaltend 53 Gew.-% Natriummonosalz des Talgfettsäuremethylesters, 11 Gew.-% Dinatriumsalz der Sulfotalgfettsäure und ca. 33 Gew.-% Wasser (Handelsprodukt des Anmelders)

PEG 400,

Polyethylenglykol mit einer relativen Molekülmasse von 400

Diese Teile wurden jeweils separat und gleichzeitig über eine Düse in die Wirbelschicht eingebracht.The following substances were used in the surfactant preparation form:

Sulfopone ^(R) T 55,

containing 54% by weight tallow fatty alcohol sulfate and approx. 41% by weight water (commercial product of the applicant)

Texapon ^(R) LS 35,

containing 34% by weight of C₁₂-C₁₄ fatty alcohol sulfate and approx. 64% by weight of water (commercial product of the applicant)

Dehydol ^(R) LT 7,

containing 99% by weight C₁₂-C₁₈ fatty alcohol with 7 EO (commercial product of the applicant)

Texin ^(R) ES 68,

containing 53% by weight sodium mono salt of tallow fatty acid methyl ester, 11% by weight disodium salt of sulph tallow fatty acid and approx. 33% by weight water (commercial product of the applicant)

PEG 400,

Polyethylene glycol with a molecular weight of 400

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

Soda,

Natriumcarbonat mit einem Schüttgewicht von 620 g/l (Handelprodukt der Firma Matthes & Weber, Bundesrepublik Deutschland)

Wessalith ^(R) P,

Zeolith-Pulver (Handelsprodukt der Firma Degussa, Bundesrepublik Deutschland)

Trägerbead,

Zeolith-Granulat, enthaltend 67 Gew.-% Zeolith (wasserfrei gerechnet), 11 Gew.-% eines polymeren Polyacrylats, 1,85 Gew.-% Talgfettalkohol mit 5 EO, 2 Gew.-% Natriumsulfat und 17 Gew.-% Wasser

Citrat,

Trinatriumcitrat-EP-Pulver (Dihydrat, Handelsprodukt der Firma Jungbunzlauer, Bundesrepublik Deutschland)

Sulfopon ^(R) T,

Talgfettalkoholsulfat-Pulver (Handelsprodukt des Anmelders)

B 5,

gemahlenes Produkt des Beispiels 5 (Korngrößenverteilung entsprechend Sulfopon ^(R) T)

In allen Beispielen wurden staubfreie und nicht klebende Granulate mit hohen Tensidanteilen erhalten (siehe Tabelle 2). Der Anteil der Granulate mit einer Korngröße oberhalb 2,5 mm lag in allen Beispielen unter 5 Gew.-%.

The following were used as solids:

Soda,

Sodium carbonate with a bulk density of 620 g / l (commercial product from Matthes & Weber, Federal Republic of Germany)

Wessalith ^(R) P,

Zeolite powder (commercial product from Degussa, Federal Republic of Germany)

Carrier bead,

Zeolite granules containing 67% by weight of zeolite (calculated as anhydrous), 11% by weight of a polymeric polyacrylate, 1.85% by weight of tallow fatty alcohol with 5 EO, 2% by weight of sodium sulfate and 17% by weight of water

Citrate,

Trisodium citrate EP powder (dihydrate, commercial product from Jungbunzlauer, Federal Republic of Germany)

Sulfopone ^(R) T,

Tallow fatty alcohol sulfate powder (commercial product of the applicant)

B 5,

milled product of Example 5 (particle size distribution corresponding to sulfopone ^(R) 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 mm was below 5% by weight in all examples.

Claims (20)

1. A process for the production of washing- and cleaning-active surfactant granules having an apparent density above 500 g/l by granulation of a surfactant formulation which contains a non-surface-active liquid component and which is present in liquid to paste-like form under normal pressure at temperatures of 20 to 40°C, characterized in that the surfactant formulation is granulated and, at the same time, dried, optionally with addition of an inorganic or organic solid, drying being understood to be the partial or complete removal of the non-surface-active liquid component.
2. A process as claimed in claim 1, characterized in that the surfactant formulation contains surfactants or surfactant mixtures from the group consisting of anionic, non-ionic, amphoteric and cationic surfactants, preferably anionic surfactants, more particularly fatty alkyl sulfates, C₉₋₁₃ alkyl benzenesulfonates and sulfofatty acid methyl esters, and/or nonionic surfactants, more particularly liquid ethoxylated fatty alcohols containing 2 to 8 ethylene oxide groups per molecule.
3. A process as claimed in claim 1 or 2, characterized in that the surfactant formulation consists of at least two separate parts of which the first contains a mixture of one or more surfactants and a non-surface-active liquid component containing organic and/or inorganic constituents while the second or following parts either contain one or more surfactants present in liquid to paste-like form under normal pressure at temperatures of 20 to 40°C, which are at least partly different from the surfactants of the first part, or another mixture of one or more surfactants, which are at least partly different from the surfactants of the first part, and a non-surface-active liquid component containing organic and/or inorganic constituents.
4. A process as claimed in claims 1 to 3, characterized in that the non-surface-active liquid component boils below 250°C, preferably below 200°C and, more particularly, between 60 and 180°C under normal pressure.
5. A process as claimed in claim 4, characterized in that mono- and/or polyhydric alcohols are used as the non-surface-active liquid component, preferably in quantities of 0.5 to 10% by weight, based on the surfactant formulation.
6. A process as claimed in claim 4 or 5, characterized in that water is used as the non-surface-active liquid component, preferably in quantities of 25 to 80% by weight, based on the surfactant formulation.
7. A process as claimed in any of claims 1 to 6, characterized in that the surfactant formulation contains additives which are ingredients of detergents, preferably in quantities of 0.001 to 15% by weight, based on the surfactant formulation.
8. A process as claimed in claim 7, characterized in that dyes, foam inhibitors, bleaches and/or solubility improvers, more particularly polyethylene glycols having a relative molecular weight of 200 to 600, are used as the additives.
9. A process as claimed in any of claims 1 to 8, characterized in that granulation and drying are carried out together in a fluidized bed either in batches or continuously, preferably continuously.
10. A process as claimed in claim 9, characterized in that the surfactant formulation or the individual parts of the surfactant formulation is/are simultaneously or successively introduced into the fluidized bed through a single nozzle or through several nozzles.
11. A process as claimed in claim 9 or 10, characterized in that the flow rate of the fluidizing air is between 1 and 8 m/s and preferably between 1.5 and 5.5 m/s.
12. A process as claimed in any of claims 9 to 11, characterized in that the granules are discharged from the fluidized bed via a grading stage.
13. A process as claimed in any of claims 9 to 12, characterized in that the air temperature at the base plate is between 80 and 400°C and preferably between 90 and 350°C, the temperature of the fluidizing air approx. 5 cm above the base plate is between 60 and 120°C, preferably between 65 and 90°C and, more preferably, between 70 and 85°C and the air exit temperature is between 60 and 120°C, preferably below 100°C and, more preferably, between 70 and 85°C.
14. A process as claimed in any of claims 1 to 13, characterized in that surfactants or surfactant mixtures, preferably spray-dried surfactants and/or surfactant granules produced by the process claimed in any of claims 1 to 11 and/or highly ethoxylated fatty alcohols containing 20 to 80 ethylene oxide groups are used as the solids.
15. A process as claimed in any of claims 1 to 14, characterized in that non-surface-active ingredients of detergents and cleaning preparations, preferably one or more constituents from the group consisting of alkali metal carbonates, alkali metal sulfates, crystalline and amorphous alkali metal silicates and layer silicates, and also zeolite, salts of citric acid, solid peroxy bleaches and, optionally, bleach activators and solid polyethylene glycols having a relative molecular weight of, or more than, 2000 and, more particularly, in the range from 4000 to 20,000 are used as the solids.
16. A process as claimed in any of claims 1 to 15, characterized in that the added solids are used in a quantity of 10 to 50% by weight and, more particularly, in a quantity of 20 to 45% by weight, based on the sum total of surfactant formulation and solid.
17. Surfactant granules produced by the process claimed in any of claims 1 to 16, characterized in that they contain 10 to 100% by weight, preferably 30 to 80% by weight and, more preferably, 40 to 70% by weight, based on the final granules, of surfactants.
18. Surfactant granules as claimed in claim 17, characterized in that they have an apparent density of 550 to 1000 g/l and preferably 550 to 850 g/l.
19. Surfactant granules as claimed in claim 17 or 18, characterized in that they do not contain any particles smaller than 50 »m in size.
20. Surfactant granules as claimed in any of claims 17 to 19, characterized in that they have a regular structure, more particularly a substantially spherical form.