EP0538294B1 - Procede de production d'agents tensio-actifs granules de lavage et de nettoyage - Google Patents

Procede de production d'agents tensio-actifs granules de lavage et de nettoyage Download PDF

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Publication number
EP0538294B1
EP0538294B1 EP91912101A EP91912101A EP0538294B1 EP 0538294 B1 EP0538294 B1 EP 0538294B1 EP 91912101 A EP91912101 A EP 91912101A EP 91912101 A EP91912101 A EP 91912101A EP 0538294 B1 EP0538294 B1 EP 0538294B1
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EP
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Prior art keywords
granules
water
surfactant
weight
surfactants
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German (de)
English (en)
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EP0538294A1 (fr
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Volker Bauer
Wilfried Rähse
Andreas Syldath
Ditmar Kischkel
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets

Definitions

  • the invention relates to a method for converting aqueous preparation forms of detergent active in washing and cleaning into storage-stable granules.
  • oleochemical surfactant compounds in detergents and cleaning agents is of great and increasing importance.
  • the considerations in the foreground are based on the one hand on the fact that surfactant compounds of this type are obtained from renewable vegetable and / or animal raw materials, but on the other hand it is the high ecological compatibility of selected components of this type which is of crucial importance.
  • Examples of such a class of oleochemical surfactant compounds are the known fatty alcohol sulfates, which are produced by sulfating fatty alcohols of vegetable and / or animal origin with predominantly 10 to 20 carbon atoms in the fatty alcohol molecule and subsequent neutralization to form water-soluble salts, in particular the corresponding alkali metal salts.
  • Tallow alcohol sulfates with predominantly saturated C16-C18 residues in fatty alcohol are already of considerable importance for the production of laundry detergents, particularly in solid form, but also fatty alcohol sulfates (FAS) with a further range in the C chain number are important washing properties .
  • fatty alcohol sulfates of the C12-C18 range with a high proportion of the lower fatty alcohols in this range can be important anionic surfactants for use in detergents and cleaning agents.
  • anionic surfactants for use in detergents and cleaning agents.
  • European patent application 342 917 also describes detergents in which the anionic surfactants consist predominantly of C12-C18 alkyl sulfates.
  • anionic oleochemical surfactant compounds are the known sulfofatty acid methyl esters (fatty acid methyl ester sulfonates, MES), which by ⁇ -sulfonation of the methyl esters of fatty acids of plant and / or animal origin with predominantly 10 to 20 carbon atoms in the fatty acid molecule and subsequent neutralization to water-soluble mono-salts, especially the corresponding alkali salts.
  • MES fatty acid methyl ester sulfonates
  • 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 inherent to the substance.
  • comparable problems also occur in other surfactant classes when trying to display the corresponding surfactant raw materials in dry form.
  • 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 of the surfactant.
  • APG pastes aqueous alkyl glycoside pastes
  • ABS pastes alkylbenzenesulfonates
  • European application EP 191 396 describes the production of a free-flowing granulate containing nonionic surfactants by mixing a powdery and a liquid, optionally aqueous, component in a mixing granulator.
  • the wet granules obtained in this way are coarsened by increasing the temperature and can optionally be coated with a powdery component.
  • the optionally coated granulate is then converted into the desired dry product by lowering the treatment temperature. A return of the granules obtained in this way to the granulation stage is not provided.
  • nonionic surfactants Another method for producing granules containing nonionic surfactants is described in European application EP 364 881.
  • the property of the nonionic surfactants is of the polyglycol ether derivative type exploited to form highly viscous gels with water.
  • the nonionic, water-insoluble solid-containing surfactant is mixed with water until a viscous gel phase is formed and mechanically processed by adding further solid until a dry, free-flowing granulate is formed. A return of the granules to the granulation stage is not described.
  • European application EP 349 200 describes a process for producing concentrated surfactant granules, an aqueous surfactant paste being cooled to temperatures between -65 and 25 ° C. and then being granulated at this temperature. A return of coarse and fine-grained fractions is described.
  • Swiss patent specification CH 324 201 describes a process for producing a powdered detergent and cleaning agent, the approach being to convert an aqueous, pasty washing and cleaning agent into a powder, in part by cold atomization or spray drying, and to agglomerate with the other part of the aqueous mixture. A return of coarse and fine-grained fractions is planned.
  • British application GB 2 116 200 discloses a process for making granular detergents wherein the desired detergents are made by agglomerating an intimate mixture of an anionic surfactant with an ethoxylated surfactant and a neutral or alkaline salt. A return of the product is not described.
  • US Pat. No. 3,472,784 describes a process for the preparation of free-flowing solid detergent compositions which contain anionic surfactants and tripolyphosphate.
  • an anionic surfactant is neutralized in the acid form with alkaline inorganic salts, so that a dough-like mixture is formed, which is converted into a free-flowing powder in a mixer after the addition of solid, hydratable tripolyphosphate.
  • a return of the granules obtained in this way to the mixing or granulating stage is not described.
  • the invention is based on the object of demonstrating a simple alternative processing option for the aqueous, in particular paste-like, surfactant preparations to give dry, in particular free-flowing and concentrated surfactant granules.
  • the invention is described in detail below using the example of converting aqueous FAS pastes into free-flowing granules.
  • the measures and process parameters described in detail here are appropriate taking into account the general chemical specialist knowledge, it can also be widely used for other aqueous, in particular pasty, surfactant preparations of the type concerned here.
  • the aqueous FAS mixtures which are preferably used are the comparatively strongly water-containing reaction products from the sulfation and the subsequent aqueous-alkaline neutralization of the particular fatty alcohol used. In general, these are mixtures of corresponding FAS types of different chain lengths with a preferably straight-chain fatty alcohol residue within the specified range of C12-C18.
  • the water content of these FAS mixtures is preferably in the range from about 20 to 80% by weight and in particular in the range from about 30 to 50% by weight, it being particularly expedient to work with flowable and / or pumpable aqueous FAS pastes can.
  • As the working temperature temperature of the surfactant paste
  • room temperature or moderately elevated temperatures up to a maximum of about 60 to 70 ° C. are preferred, it being appropriate to coordinate the working temperature and water content of the surfactant paste in such a way that the safe dosing of the water-containing FAS mixture used is ensured.
  • the granulation process is as follows:
  • a suitable mixing and granulating device for example in appropriate systems of the type of an Eirich mixer, a Lödige mixer, for example a ploughshare mixer from the Lödige company, or a mixer from the Schugi company, at peripheral speeds of the mixing elements, preferably between 2 and 7 m / s (ploughshare mixer) or 5 to 50 m / s (Eirich, Schugi), in particular between 15 and 40 m / s the aqueous FAS mixture on the one hand and on the other hand water-soluble and / or water-insoluble solids in such proportions and mixed in such intensely with one another, that a free-flowing granulate is formed.
  • a Lödige mixer for example a ploughshare mixer from the Lödige company, or a mixer from the Schugi company
  • peripheral speeds of the mixing elements preferably between 2 and 7 m / s (ploughshare mixer) or 5 to 50 m / s (Eirich, Schugi), in particular between 15 and
  • a predeterminable grain size of the granulate can be set in a manner known per se.
  • the mixing process takes only a very short period of time, for example about 0.5 to 10 minutes, in particular about 0.5 to 5 minutes (Eirich mixer, Lödige mixer) to homogenize the mixture to form the free-flowing granulate.
  • the mixing ratios of the components and in particular the proportions of the added solid are to be matched to the water content entered via the FAS mixture in such a way that the homogenized mixture of aqueous surfactant preparation form and added solid can form the free-flowing granulate.
  • the still moist granulate is transferred to the drying stage, which in the preferred embodiment is designed as a fluidized bed drying. Drying is advantageous because it leads to surfactant granules with an increased surfactant content.
  • low-concentration surfactant mixtures which contain, for example, more than 50% by weight and in particular more than 60% by weight of water, it may be necessary to dry the granules formed primarily in order to achieve the desired minimum content of 20% by weight of surfactant in the To obtain granules. Drying can be continued in the granulate to the desired final value of unbound or bound water.
  • non-dried granules are mixed with partially or completely dried granules in any ratio.
  • “Completely dried” is understood to mean the state in which the unbound water and possibly portions of the bound water have been removed from the granules.
  • Fluidized bed drying is a preferred type of drying, since rapid drying of the outer surface of the granules occurs with simultaneous intensive movement and mixing of the granules, so that undesirable caking of the still moist granules is counteracted in this way.
  • the invention provides for the still moist granules to be powdered - expediently immediately after the granules are produced - with a dusty or pulverulent auxiliary and for the granules stabilized in this way to be added to the drying stage.
  • the state of the free-flowing granulate is then quickly reached there even under comparatively mild drying conditions.
  • the drying in particular the fluidized bed drying, is preferably carried out at temperatures of the gas phase below 200 ° C. and in particular at temperatures in the range from approximately 70 to 160 ° C., for example in the range from approximately 90 to 150 ° C. These temperatures relate primarily to the gas phase; in a preferred embodiment, the final temperature of the granules which is established is kept at comparatively low temperatures and here, for example, does not exceed 80 to 90 ° C., preferably it is not higher than 75 ° C.
  • the solids used in the granulation for the partial drying of the aqueous surfactant preparation form can be corresponding ingredients from conventional formulations of detergents and / or cleaning agents, but they can also be foreign substances as long as they are compatible with the intended use of the surfactants. It will generally be preferred to use ingredients from washing and / or cleaning agents here. It is a particular advantage of the process according to the invention that there is very great freedom in the selection of these solid mixture components. The reason for this is the fact that the granulation method according to the invention with the preferably connected drying provides such comparatively mild working conditions that undesired secondary reactions in the granulation and / or drying step are only to be feared in special cases. General technical knowledge applies here.
  • temperature-sensitive mixture constituents for example textile detergents, such as those used as bleaching agents of the perborate type
  • textile detergents such as those used as bleaching agents of the perborate type
  • water-soluble and / or water-insoluble solids which can be mixed with the water-containing surfactant preparation forms, granulated and then dried under the specified working conditions.
  • suitable water-soluble solids are inorganic salts, for example soda, alkali silicates, in particular water glass powder, sodium sulfate and / or phosphate salts such as sodium pyrophosphate and sodium tripolyphosphate.
  • the teaching of the invention also provides for the use of corresponding insoluble, preferably finely divided materials.
  • the grain size of the preferred solids is less than 1 mm and in particular less than 100 ⁇ m, for example not more than 30 ⁇ m.
  • Typical examples from the field of washing and / or cleaning agents are additives which are used as so-called builder substances to bind the alkaline earth metal ions and thus to remove the water hardness.
  • Examples include finely divided crystalline zeolites, in particular sodium zeolite NaA in detergent quality, which preferably consists of at least 80% of particles of a size of less than 10 ⁇ m.
  • Other examples of preferred solids are hydrotalcites, water-insoluble and crystalline phyllosilicates, abrasives such as stone powder and the like.
  • a special feature according to the invention is the use of dried and again finely divided granules from ongoing production as a solid component of the mixture for working up further amounts of the aqueous surfactant preparation forms.
  • This embodiment also provides for complete circulation of the granules produced by the process according to the invention in the process cycle. Details of this particular embodiment are described below.
  • the mixing ratios of the surfactants to be used in the mixing and granulating stage on the one hand and on the other hand of the solids it may be expedient to adapt these mixture components to the corresponding requirements of the components in the final washing and / or cleaning agents to be created.
  • the ratio of anionic surfactants to the finely divided solids that are used, for example, in textile detergents can provide clues for the composition of the mixture to be granulated.
  • the need to use various solid detergent constituents, advantageously also in coordinated proportions, can be derived from such considerations.
  • the content of water glass in laundry detergents is comparatively low in the full formulation, for example it can be in the range from 2 to 5% by weight of the total formulation. In contrast, however, it may be desirable to mix in much larger amounts of anionic surfactant based on fatty alcohol sulfate, with amounts in the order of 20 to 30% by weight, based on the formulation of the finished detergent, being suitable. If a comparatively water-rich FAS surfactant mixture is used to carry out the process according to the invention, if water glass powder alone is used as a solid, substantially larger amounts of water glass would have to be mixed in in order to adjust the state of the free-flowing powder in the mixing and granulation stage than in the recipe of finished means are desired. It will therefore be advisable to use other dry detergent ingredients, such as soda and / or sodium sulfate.
  • the desired percentage composition of the granules according to the invention can be combined with the proportional mixture prescribed by the full detergent formulation.
  • Typical examples of this are mixtures of the water-containing surfactant pastes with sodium zeolite, soda and / or sodium sulfate.
  • the invention provides for the already mentioned complete circulation of the granulate back into the mixing and granulating stage.
  • the process in particular in a continuous process, can be carried out in such a way that the entire solid phase added in the mixing and granulating stage is formed from a recycled material of this type, which consists of granules which have already been dried and thus already has considerable proportions, namely preferably more than 25% by weight. , based on this dry granulate used as a solid, contains.
  • the dried granulate used as a solid in the mixing and granulating stage is first crushed under the action of the mixing tools. This return can take place once, but also several times, for example 2 to 8 times.
  • the surfactant can be accumulated in the granulate up to predetermined values. Due to the comparatively low melting points of detergents important for washing, e.g. B. FAS compounds and in particular corresponding FAS mixtures, the enrichment of the granules will have a minor importance for practical work to an almost 100% surfactant mass. However, considerably higher surfactant contents can be set in the granules in this process than when the aqueous mixture passes through the mixing and granulating zone only once. In the embodiment with granulate recycling, FAS contents in the granulate of at least 30% by weight and preferably of at least 35% by weight can be set easily.
  • the corresponding surfactant content it is possible according to the invention to raise the corresponding surfactant content to at least 45% by weight or even to at least 50% by weight.
  • the aforementioned powdering with solid dry mixture components for example with dried zeolite NaA in detergent quality, can become significant.
  • the grain size range of the resulting granulate and the average grain size are adjusted in a manner known per se by adapting the working conditions in the granulation stage.
  • granules with a grain size range of approximately 0.01 to 3 mm (sieve analysis) and in particular those with a range of approximately 0.05 to 2 mm can be produced with ease.
  • An important embodiment of the invention provides for the classification of the dried granules by separating undesired fine-grain and coarse-grain fractions in a manner known per se. In an important embodiment of the invention, these separated fractions can even be returned to the mixing and granulating stage and used as a solid if no recycling of the granulated and dried granules is otherwise provided.
  • the physical properties of the granules can also be largely predetermined in another way.
  • suitable auxiliary substances the hardness of the granulate and in particular its abrasion hardness can be modified and, for example, increased.
  • An example of this is the polyacrylates and polyacrylate copolymers known as builder substances, which can be used, for example, with relative molecular weights in the range from 30,000 to 100,000.
  • Auxiliaries of this type can already be added to the mixture in the mixing and granulating stage, but it is also possible to apply them subsequently to the preformed granules before or during the drying process.
  • the method according to the invention can also be modified in a completely different form and used to facilitate the production of granules of the type described.
  • This modification can be understood from the following example:
  • zeolite NaA is obtained in the form of an aqueous suspension (masterbatch) which can contain more than 50% by weight of water and is usually pulverulent in the spray tower Dry product is worked up.
  • the zeolite can be introduced into the mixing and granulating stage at least in part in the form of this suspension or as a product which has not been completely dried, in order then to be dried up in the granulate in the mixture with the surfactant and the added dry solids.
  • Such an embodiment can be of particular interest if the dried granules are circulated and the portion required as a solid is introduced into the mixing and granulating stage via the desired end product.
  • Zeolite materials of the last-mentioned type but also other typical additives of detergents and cleaning agents, are in turn capable of partially binding water.
  • auxiliaries of this type are anhydrous soda and anhydrous sodium sulfate, which can bind considerable amounts of water in the form of water of crystallization.
  • One embodiment of the invention uses this ability of internal water binding for additional drying (internal drying) of the granules formed in the process according to the invention.
  • the water content in the drying step is reduced to such an extent that the bound water present as crystal water is at least partially discharged.
  • the water contents of the dried granules preferred according to the invention are accordingly comparatively low.
  • the proportion of unbound water is preferably below 5% by weight, in particular below 3% by weight, based on the dried granules.
  • Water bound in crystal form or integrated into the molecular structure may be present in the substance mixture in limited amounts, but the storage stability of the granules becomes higher, the lower the proportion of water of crystallization in the end product in particular is reduced.
  • this embodiment is of lesser importance if rapid further processing of the surfactant granules is intended. If these granules are to be used as a form of trading in raw materials trading, the considerations discussed last should be given greater importance. Granules, on the other hand, which are processed quickly and do not require drying, can have a significantly higher free water content. However, this should not exceed 30% by weight, based on the undried granules.
  • the granules according to the invention can have an increased bulk density, in particular in comparison with corresponding spray-dried materials.
  • Typical granules within the meaning of the invention normally have a bulk density of at least about 350 g / l, preferably of at least about 500 g / l. Bulk weights between 600 and 800 g / l are particularly preferred.
  • the process according to the invention can be used in a wide range with regard to the aqueous surfactant mixtures.
  • mixtures of surfactants which are present in the region of room temperature as sufficiently dimensionally stable solids and which are present in the course of their preparation and / or workup as aqueous pastes which contain the surfactants dispersed in the aqueous phase are recorded.
  • An important example of such surfactants are the sulfofatty acid methyl ester mono salts and / or the so-called di-salts.
  • the mono-salts of the sulfofatty acid methyl esters (MES) are obtained in their large-scale production as a mixture with limited amounts of di-salts, which are known to result from partial ester cleavage with the formation of the corresponding ⁇ -sulfo-fatty acids or their di-salts.
  • the di-salt content of such MES-based surfactants is usually below 50 mol% of the anionic surfactant mixture, for example in the range up to about 30 mol%.
  • the teaching according to the invention is suitable for its application to such surfactant mixtures based on MES as well as to corresponding blends with higher di-salt contents up to the pure di-salts.
  • a preferred aqueous MES feedstock are the comparatively strongly water-containing reaction products from the sulfonation and the subsequent aqueous-alkaline neutralization of the respective fatty acid methyl ester.
  • these are mixtures of corresponding MES types of different chain lengths with preferably straight-chain fatty acid residues within the specified range of C12-C18.
  • the water content of these raw MES products can be in the range from about 20 to 80% by weight and in particular in the range from about 30 to 60% by weight, it being particularly expedient to work with flowable and / or pumpable aqueous MES pastes can.
  • Surfactant compounds based on alkyl glycosides and their preparation, in particular in the form of water-containing bleached pastes, are described in detail, for example, in international patent application WO 90/03977.
  • Surfactant reaction products of this type are a further example of the applicability of the process according to the invention for the production of dry granules based on surfactants.
  • a free-flowing granulate with a water content of 7.7% by weight and a bulk density of 603 g / l was obtained.
  • the drying time could be reduced to 20 minutes or 10 minutes.
  • the product had a tallow fatty alcohol sulfate content of 33.5% by weight and a water content of less than 1% by weight.
  • the bulk density was 650 ⁇ 30 g / l depending on the fine grain and coarse grain content.
  • Example 1a 1.5 kg each of the tallow-based fatty alcohol sulfate mixture (Sulfopon (R) T55) were mixed with 1.5 kg soda, 1.5 kg zeolite NaA and 3 kg crystalline layered silicate (commercial product SKS-6 (R) from. Hoechst) granulated and dried.
  • SKS-6 (R) commercial product SKS-6 (R) from. Hoechst
  • Powdering the 7 times recycled material (carrier soda) with 100 g soda prevented the granules from sticking in a subsequent further mixing process.
  • Such powdering and subsequent further application of surfactant paste made it possible to achieve a shell-like structure of the granules.
  • a free-flowing granulate with 2.4% by weight of water and a bulk density of 721 g / l was obtained.
  • the washing active substance content (sulph tallow fatty acid methyl ester and di-salt content) of these granules was 37.2% by weight, the disalting content was 6.5% by weight (increase in the disalting content by ester cleavage of the mono-salt).
  • WAS detergent substances
  • a corresponding test using sodium sulfate as the carrier material gave, after drying for 20 minutes at an air inlet temperature of 70 ° C., granules with 0.8% by weight of water, 39% by weight of WAS, of which 7% by weight was di-salt.
  • the bulk density of the granules was 664 g / l.
  • Example 2a 1.5 kg of the water-containing sulfotalg fatty acid methyl ester paste were granulated with 1.5 kg of soda in the mixer and dried. A further 250 g of the aqueous sulph tallow fatty acid methyl ester paste were then applied to the resulting granules. The resulting granules with an increased anionic surfactant content were again dried in a fluidized bed.
  • the end product had a WAS content of 44% by weight and a bulk density of 670 g / l with a water content of less than 1% by weight.
  • APG paste 55 wt .-% C12-C14 alkyl glucoside paste
  • soda 2000 g
  • APG paste 55 wt .-% C12-C14 alkyl glucoside paste
  • soda 2000 g
  • APG paste 55 wt .-% C12-C14 alkyl glucoside paste
  • soda 2000 g
  • soda a 55 wt .-% C12-C14 alkyl glucoside paste
  • soda 2000 g of soda were worked up in the manner given in the previous examples in a Eirich mixer to give granules with a bulk density of 800 g / l.
  • another 500 g of APG paste could be applied to these granules in the Eirich mixer and dried to a granulate with an increased surfactant content.

Claims (8)

  1. Procédé de fabrication d'agents tensioactifs granulés de lavage et de nettoyage par granulation d'un mélange constitué d'une forme aqueuse de préparation tensioactive et d'une ou de plusieurs matières solides solubles et/ou insolubles dans l'eau, permettant d'obtenir un granulé coulant, qui renferme au moins 20 % en poids de tensioactifs, caractérisé en ce que
    a) des composés tensioactifs au moins largement solides à température ambiante, appartenant à la classe des surfactifs anioniques, non ioniques, zwitterioniques et/ou cationiques sont mis en oeuvre sous la forme aqueuse de préparation tensioactive,
    b) le granulé obtenu et séché est recyclé en circuit dans l'étape de mélangeage et de granulation et,
    c) présenté et granulé pour le mélangeage ultérieur avec une forme aqueuse de préparation tensioactive conforme à a), la totalité de la phase solide mise en oeuvre dans l'étape de granulation c) étant constituée du granulé recyclé conforme à b) et la concentration en tensioactif de ces granulés, le cas échéant après séchage, étant augmentée par rapport à celle des granulés recyclés.
  2. Procédé selon la revendication 1, caractérisé en ce que l'on met en oeuvre sous la forme aqueuse de préparation tensioactive des tensioactifs faisant partie du groupe des sulfates d'alcools gras en C₁₀-C₂₀, des alkylbenzènesulfonates, des esters méthyliques d'acides gras α-sulfonés en C₁₀-C₂₀, des sels dimétalliques d'acides gras α-sulfonés en C₁₀-C₂₀, des alkylglycosides et des savons.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que le granulé coulant est séché dans un lit fluidisé, ce qui permet d'obtenir des granulés tensioactifs contenant au moins 20 % en poids de tensioactifs.
  4. Procédé selon une des revendications 1 à 3, caractérisé en ce que l'on transforme des pâtes tensioactives aqueuses fluides et/ou pompables possédant une teneur en eau de 20 à 80 % en poids, de préférence de 30 à 50 % en poids, en granulés tensioactifs avec une concentration en tensioactifs d'au moins 25 % en poids, de préférence de 30 à 75 % en poids, par rapport au granulé séché, le séchage consistant de préférence en un séchage en lit fluidisé et étant opéré à des températures de la phase gazeuse inférieures à 200 °C, de préférence comprises dans l'intervalle de 70 à 160 °C.
  5. Procédé selon une des revendications 1 à 4, caractérisé en ce que les granulés non séchés sont mélangés avec des granulés totalement ou complètement séchés, dans un rapport quelconque.
  6. Procédé selon une des revendications 1 à 5, caractérisé en ce que des matières solides, qui sont des constituants de produits de lavage et de nettoyage, sont mises en oeuvre dans l'étape de mélangeage et de granulation, de la soude, des silicates de métaux alcalins ou du sulfate de sodium étant utilisés comme matière solides solubles dans l'eau et de la zéolithe NaA, de l'hydrotalcite ou des matières abrasives, telles que poudres de friction et matières similaires ou des silicates stratifiés cristallins étant mis en oeuvre comme matières solides insolubles dans l'eau.
  7. Procédé selon une des revendications 1 à 6, caractérisé en ce que pour accroître la dureté du granulé, en particulier pour augmenter sa résistance à l'abrasion, des composés polymères, qui sont habituellement mis en oeuvre dans les produits de lavage et de nettoyage, sont co-utilisés pour la fabrication du granulé.
  8. Procédé selon une des revendications 1 à 7, caractérisé en ce que le recyclage dans l'étape de mélangeage et de granulation a lieu 2 à 8 fois.
EP91912101A 1990-07-05 1991-06-26 Procede de production d'agents tensio-actifs granules de lavage et de nettoyage Expired - Lifetime EP0538294B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4021476 1990-07-05
DE4021476A DE4021476B4 (de) 1990-07-05 1990-07-05 Verfahren zur Überführung wäßriger Zubereitungsformen wasch- und reinigungsaktiver Tensidverbindungen in lagerstabile Trockengranulate
PCT/EP1991/001190 WO1992001036A1 (fr) 1990-07-05 1991-06-26 Procede de production d'agents tensio-actifs granules de lavage et de nettoyage

Publications (2)

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EP0538294A1 EP0538294A1 (fr) 1993-04-28
EP0538294B1 true EP0538294B1 (fr) 1996-02-28

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US (1) US5597794A (fr)
EP (1) EP0538294B1 (fr)
JP (1) JP3027413B2 (fr)
KR (1) KR0170424B1 (fr)
AT (1) ATE134704T1 (fr)
DE (2) DE4021476B4 (fr)
ES (1) ES2083579T3 (fr)
WO (1) WO1992001036A1 (fr)

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DE4127323A1 (de) * 1991-08-20 1993-02-25 Henkel Kgaa Verfahren zur herstellung von tensidgranulaten
DE4209339A1 (de) * 1992-03-23 1993-09-30 Henkel Kgaa Verfahren zur Herstellung rieselfähiger Wasch- und Reinigungsmittelgranulate und/oder -teilgranulate
CA2152090A1 (fr) * 1992-12-23 1994-07-07 David Parris Procede de granulation
GB9322530D0 (en) * 1993-11-02 1993-12-22 Unilever Plc Process for the production of a detergent composition
DE4406592A1 (de) * 1994-03-01 1995-09-07 Henkel Kgaa Verbesserte Mehrstoffgemische auf Basis wasserlöslicher Alkalisilikatverbindungen und ihre Verwendung, insbesondere zum Einsatz als Builder in Wasch- und Reinigungsmitteln
BR9509051A (pt) * 1994-09-29 1998-06-23 Unilever Nv Processo para a obtençao de uma composiçao detergente e composiçao detergente particulada
DE4443644A1 (de) * 1994-12-08 1996-06-13 Henkel Kgaa Feste, rieselfähige Zubereitungen
WO1996025482A1 (fr) * 1995-02-13 1996-08-22 The Procter & Gamble Company Procede pour produire des agglomerats detergents a classe granulometrique controlee
US5574005A (en) * 1995-03-07 1996-11-12 The Procter & Gamble Company Process for producing detergent agglomerates from high active surfactant pastes having non-linear viscoelastic properties
DE19524464C2 (de) * 1995-07-10 2000-08-24 Cognis Deutschland Gmbh Verfahren zur Herstellung von Zuckertensidgranulaten
DE19534371C1 (de) * 1995-09-15 1997-02-20 Henkel Kgaa Verfahren zur Herstellung wasser- und staubfreier Zuckertensidgranulate
GB9604000D0 (en) * 1996-02-26 1996-04-24 Unilever Plc Production of anionic detergent particles
GB9604022D0 (en) * 1996-02-26 1996-04-24 Unilever Plc Anionic detergent particles
JP3305327B2 (ja) * 1996-10-04 2002-07-22 ザ、プロクター、エンド、ギャンブル、カンパニー 非塔式製造法による低密度洗剤組成物の製造法
US6248709B1 (en) * 1997-02-27 2001-06-19 The Procter & Gamble Company Process for making a detergent composition by adding co-surfactants
DE19721885A1 (de) † 1997-05-26 1998-12-03 Henkel Kgaa Verfahren zur Herstellung kationtensidhaltiger Granulate
DE19911040A1 (de) * 1999-03-12 2000-09-21 Cognis Deutschland Gmbh Tensidgranulate
US20040077518A1 (en) * 2000-11-08 2004-04-22 Makoto Nishikawa Granular surfactant and process for producing the same
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Publication number Publication date
JPH05508431A (ja) 1993-11-25
ATE134704T1 (de) 1996-03-15
ES2083579T3 (es) 1996-04-16
JP3027413B2 (ja) 2000-04-04
KR930701584A (ko) 1993-06-12
EP0538294A1 (fr) 1993-04-28
DE4021476B4 (de) 2005-03-10
WO1992001036A1 (fr) 1992-01-23
DE59107488D1 (de) 1996-04-04
DE4021476A1 (de) 1992-01-09
KR0170424B1 (ko) 1999-01-15
US5597794A (en) 1997-01-28

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