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WO1996003488A1 - Procede de fabrication de granules de tensioactif - Google Patents

Procede de fabrication de granules de tensioactif Download PDF

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Publication number
WO1996003488A1
WO1996003488A1 PCT/EP1995/002777 EP9502777W WO9603488A1 WO 1996003488 A1 WO1996003488 A1 WO 1996003488A1 EP 9502777 W EP9502777 W EP 9502777W WO 9603488 A1 WO9603488 A1 WO 9603488A1
Authority
WO
WIPO (PCT)
Prior art keywords
acid
granulation
spray
surfactant
anionic
Prior art date
Application number
PCT/EP1995/002777
Other languages
German (de)
English (en)
Inventor
Thomas LÜDER
Bernhard Gutsche
Gilbert Roegel
Christoph Wissenmeyer
Karl-Heinz Schmid
Ditmar Kischkel
Andreas Syldath
Original Assignee
Henkel Kommanditgesellschaft Auf Aktien
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel Kommanditgesellschaft Auf Aktien filed Critical Henkel Kommanditgesellschaft Auf Aktien
Priority to DE59502656T priority Critical patent/DE59502656D1/de
Priority to EP95926892A priority patent/EP0772674B1/fr
Priority to DK95926892T priority patent/DK0772674T3/da
Publication of WO1996003488A1 publication Critical patent/WO1996003488A1/fr

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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
    • C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
    • 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
    • C11D11/02—Preparation in the form of powder by spray drying

Definitions

  • the invention relates to a process for the production of detergent granules with high bulk density and good dissolving behavior in water, the granulate size being controllable at least in such a way that dust-free or at least low-dust granules are produced.
  • Surfactant granules can be produced, for example, by conventional drying techniques for surfactant-containing solutions and pastes, especially in the spray tower.
  • European patent application EP-A-0 319819 discloses a process for the preparation of surfactant granules by spray drying, an anionic surfactant in its acid form and a highly concentrated aqueous alkaline component being acted upon separately with a gaseous medium, then combined in stoichiometric amounts, in neutralized with a multi-component nozzle and sprayed at a high propellant pressure in the drying tower.
  • the products obtained are solid or pasty, solid products mostly being relatively dusty, having a relatively high water content and a low bulk density.
  • Granulation is an alternative to spray drying of surfactant pastes.
  • European patent application EP-A-0430 148 describes a process for producing fatty alcohol sulfate granules which are dispersible in cold water.
  • a highly concentrated aqueous paste holsulfat fatty alcohols containing less than 14 wt .-% of water and less than 20 wt .-% is further additives, at temperatures between 10 and 45 C ⁇ so long me ⁇ mechanically processed until granules are formed .
  • a surfactant preparation containing water as a liquid component and additionally organic polymer and Bu lder substances can contain, mixed with a finely divided solid and granulated in a high-speed mixer.
  • the water content of the surfactant paste also represents a critical process parameter here. If the water content of the surfactant paste is too high, the solid is dispersed so that it can no longer act as a deagglomeration agent. On the other hand, if the solids content exceeds a certain value, the mass will not have the consistency required for granulation.
  • the object of the invention was to develop a method which does not have the disadvantages of the above-mentioned methods.
  • low-dust granules with increased bulk density should be produced, which nevertheless have good dissolving behavior in water.
  • the invention accordingly relates to a process for the preparation of surfactant granules by spray drying, an anionic surfactant or more anionic surfactants in its / its acid form and a highly concentrated aqueous alkaline component being separately charged with a gaseous medium, combined, neutralized in a multi-component nozzle and at a high rate Propellant gas pressure are sprayed in the drying tower, the combination of the acidic and alkaline components in almost stoichiometric amounts and the solid, one-piece products obtained in a mechanisc working mixer are transferred in which the fine particles are agglomerated into granules having a bulk density of at least 400 g / l.
  • the first process step, spray neutralization can be carried out, for example, according to the teaching of European patent application EP-A-0319819. At this point, reference is expressly made to the disclosure in European patent application EP-A-0319819.
  • a preferred embodiment of the present invention provides that the acidic and alkaline reactant streams separately charged with a gaseous medium are brought together via a single multi-component nozzle, for example via a 2-component nozzle or a 3-component nozzle, and dry ⁇ nungsraum be sprayed. It is also possible to bring the gas-charged reactant streams together before the nozzle. It should be noted, however, that the distance between the location of the junction from the spraying device depends on the process conditions and the material systems used, but is preferably kept as small as possible in order to avoid clogging of the nozzle due to premature neutralization reactions.
  • the first-mentioned variant of combining the reactant streams in the nozzle is to be preferred, since in this case the neutralization takes place essentially in the nozzle or directly when it emerges from the nozzle.
  • the combined acidic and alkaline reactant streams it is also possible for the combined acidic and alkaline reactant streams to be sprayed into the drying chamber via a plurality of multi-component nozzles. This is particularly preferred when products are to be produced from different types of anionic surfactants and thus different, combined acidic and alkaline reactant streams are to be sprayed.
  • the starting materials are introduced, for example using piston pumps, in almost stoichiometric metered amounts into one or two non-modified commercial nozzle (s) or one or two spray tube (s).
  • the gaseous medium (propellant) is mixed in directly in front of the nozzle. This means that the gaseous medium is mixed into the reactant streams before they meet in front of or in the nozzle.
  • the flow rate of the reactant streams or the pressure at which the reaction mixture is sprayed into the drying room can be found in European patent application EP-A-0319819.
  • almost stoichiometric amounts mean that the ratio of the number of acidic groups to alkaline groups is preferably in the range from 1.1: 1 to 0.8: 1 and in particular from 1: 1 to 0.9 : 1 lies.
  • the anionic surfactants in their acid form can be carboxylic acids, sulfuric acid semesters and sulfonic acids, preferably fatty acids, alkylarylsulfonic acids, ⁇ -sulfofatty acid esters and the sulfuric acid semiesters of optionally alkoxylated, especially ethoxylated alcohols and fatty alcohols and / or sulfosuccinic acid.
  • fatty acid esters in particular fatty acid methyl esters, can also be used, in which case the ester group is not saponified, but instead is saponified.
  • Suitable anionic surfactants in their acid form are therefore in particular either an anionic surfactant in its acid form or a mixture of the group of anionic surfactants in their acid form, optionally in combination with nonionic, amphoteric and / or cationic surfactants.
  • Preferred anionic surfactants in their acid form are C ⁇ -C ⁇ alkylsulfonic acids, Cg-Ci3-alkylbenzenesulfonic acid, usually called dodecylbenzenesulfonic acid, and ⁇ -sulfofatty acid methyl ester in its acid form.
  • Particularly preferred alkylsulfonic acids are the sulfuric acid monoesters from primary alcohols of natural and synthetic origin, in particular from fatty alcohols, e.g.
  • esters of ⁇ -sulfofatty acids which, by 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, for example the ⁇ -sulfonated methyl esters of the hydrogenated coconut oil, , Palm kernel or tallow fatty acids, as well as those caused by the ester cleavage available ⁇ -sulfo fatty acids (diacids) used.
  • diacids ⁇ -sulfofatty acids
  • alkanesulfonic acids which are obtainable from Ci2-Ci8-alkanes by sulfochlorination or sulfoxidation.
  • ingredients can be used, which are preferably derived from the group of ingredients that are usually used in spray-dried washing or cleaning agents.
  • nonionic surfactants but also builder substances such as phosphates and zeolites or polycarboxylic acids or their salts and polymeric polycarboxylates, and also inorganic salts such as carbonates, bicarbonates, silicates, sulfates and bisulfates are suitable.
  • Solid substances can be blown into the spray drying room, for example, while liquid components can additionally be introduced into the spray drying room in combination with one of the reactant streams.
  • anionic surfactant and / or nonionic, surfactant pastes are also introduced into the spray drying room in addition to the reactant streams.
  • an anionic surfactant in its acid form or a mixture of anionic surfactants in its acidic form is used in combination with anionic, nonionic, amphoteric and / or cationic surfactants.
  • Suitable anionic surfactants which can be introduced into the process in paste form in particular, are all salts which are concordant with the acid forms mentioned above.
  • Nonionic surfactants preferably used in combination with these anionic surfactants in acid form are derived from liquid alkoxylated, advantageously ethoxylated, in particular primary alcohols with preferably 9 to 18 carbon atoms and an average of 1 to 40 moles of ethylene oxide per mole of alcohol, in which the alcohol residue may be linear or methyl-branched in the 2-position, or may contain linear and methyl-branched residues in the mixture, as is usually present in oxo alcohol residues.
  • linear residues from alcohols of native origin with 12 to 18 carbon atoms are preferred, such as from coconut, tallow or oleyl alcohol.
  • the degrees of ethoxylation given represent statistical mean values, which can be an integer or a fractional number for a special product.
  • Alcohol ethoxylates with a narrow homolog distribution are also suitable.
  • alcohol ethoxylates are preferred which have an average of 2 to 8 ethylene oxide groups.
  • the preferred ethoxylated alcohols include, for example, Cg-Cn-oxo alcohol with 7 EO, Ci3 ⁇ Ci5-0xoalcohol with 3 EO, 5 EO or 7 EO and in particular Ci2-C j 4-alcohol with 3 EO or 4 EO, Ci2- Ci8 alcohols with 3 EO, 5 EO or 7 EO and mixtures thereof, such as mixtures of Ci2-Ci4 alcohol with 3 EO and C ⁇ 2-Ci8 alcohol with 5 EO.
  • alcohols are preferred which have more than 10 EO per molecule of alcohol, for example 11 EO, 14 EO, 20 EO, 25 EO, 30 EO or also 40 E0 such as tallow fatty alcohol with 40 E0.
  • nonionic surfactants which can be used are alkylglycosides of the general formula R- 0- (G) x , in which R is a primary straight-chain or aliphatic radical which is methyl-branched in the 2-position and has 8 to 22, preferably 12 to 18, atoms, G is a symbol , which stands for a glycose unit with 5 or 6 carbon atoms, and the degree of oligo erization x is between 1 and 10, preferably between 1 and 2 and in particular is significantly less than 1.4.
  • R is a primary straight-chain or aliphatic radical which is methyl-branched in the 2-position and has 8 to 22, preferably 12 to 18, atoms
  • G is a symbol , which stands for a glycose unit with 5 or 6 carbon atoms
  • the degree of oligo erization x is between 1 and 10, preferably between 1 and 2 and in particular is significantly less than 1.4.
  • the neutralization or saponification reaction is preferably carried out with concentrated aqueous alkaline solutions, for example solutions of hydroxides, carbonates or hypochlorites of sodium or potassium, in particular with a concentrated aqueous sodium hydroxide solution and / or potassium hydroxide solution, concentrations around 45 to 55% by weight are particularly preferred. A further dilution of the reactant streams with water is not necessary.
  • Suitable gaseous medium are, in particular, gases such as air or nitrogen which are inert to the starting and end materials.
  • gases such as air or nitrogen which are inert to the starting and end materials.
  • water vapor is also suitable here, in particular if one of the reactant streams or the reactant streams is to be heated before the merging.
  • Such solid products can now be transferred to any of the known mechanically operating mixers or granulators, with the aid of which the powders are granulated and at the same time recompacted to bulk densities of at least 400 g / 1, preferably of about 420 to 650 g / 1 can.
  • Such mixers are, for example, ploughshare mixers or annular layer mixers, such as those sold by the companies Lödige, Imcatec or Drais, but also mixer types from Schugi (Flexomi ⁇ (R)) or Niro (ZigZag mixer ( R ) or HEC granulator ( R )). Both batch and continuous mixer types can be used, with the continuously operating mixer types being preferred.
  • this granulation is carried out at a temperature at which the solid product softens and can thus be shaped.
  • a temperature at which the solid product softens and can thus be shaped In the lower temperature range, granules with an only slightly increased bulk density are formed; however, this increases at higher temperatures. If the temperatures are too high, however, the mixture to be granulated is softened to a great extent and the mixer becomes blocked by pasty caking on walls and tools. With a given chemical composition, the preferred temperature range also shifts downward with increasing water content.
  • drying or moistening, cooling or heating the spray-neutralized product before or during the granulation can be advantageous.
  • the spray-neutralized powders are subjected to a treatment in a fluidized bed before the granulation, and the powders can be dried and / or cooled.
  • cooling or initially drying and then cooling of the products is carried out, preferably such Product temperatures are set which have proven to be advantageous in the granulation, so that direct further processing of the product is made possible.
  • the powdery products produced in the spray chamber are even further processed directly, that is to say without intermediate storage and without treatment in the fluidized bed, in the mechanically working mixer.
  • the granulation in the mixer is carried out at product temperatures between 30 and 80 ° C., preferably between 40 and 70 ° C.
  • solid and / or liquid additional components in this process stage, it is not necessary.
  • the granulation of the dusty products succeeded without the addition of liquid components, which usually had to be added as a granulating liquid.
  • advantageous low-dust granules with controllable particle size and high bulk density are obtained, which also show very good flow behavior, so that granulation of the spray-dried powder without the addition of liquid components is a preferred embodiment.
  • the applicant assumes that the relatively high water content of the sprayed and dusty products from the first process stage serves as a "liquid reserve", which enables granulation. It is precisely the parameter that leads to the manifold disadvantages of the powdery products in the first process stage that results in particularly advantageous products after the second process stage.
  • additives can of course be added at this point, as is customary in conventional granulation, even at these temperatures liquid to pasty additives such as nonionic surfactants (see above), but also anionic surfactant pastes (see above).
  • nonionic surfactants see above
  • anionic surfactant pastes see above.
  • liquid components are added during the granulation and the proportion of the added liquid components exceeds 5% by weight, to further solids
  • Add usual ingredients of washing or cleaning agents are also peroxy bleaching agents, such as perborate and percarbonate, but also conventional graying inhibitors and substances which prevent the fabric from being soiled again.
  • Enzymes can also be granulated at this stage; however, it is preferred to add these to the end product in granular form.
  • water and aqueous solutions are less preferred: on the one hand, the water - as stated above - is not required as a granulating liquid and, on the other hand, a subsequent drying would have to be connected in most cases, but this is not preferred.
  • Such drying of the granules and thus a concentration of the granules following the second process stage can, in principle, be carried out, for example, in a so-called long-term dryer, for example in a fluidized bed or a vacuum dryer. Just like drying, cooling the granules, as is known from the prior art, is also possible.
  • customary processing steps such as sieving and, if appropriate, recycling fine and coarse-grained fractions into the mixer can follow.
  • finely divided solids for example zeolites, in particular zeolite A and / or zeolite P, silicates, silicas, sulfates, calcium stearates and mixtures thereof, are advantageously added at the end of the granulation step in order to improve the storage stability of the granules.
  • soaps, alkyl sulfates and / or fatty acid isethionates are also added as solid additional components in the granulation stage. It has been shown that the dissolution behavior of the granular end products produced according to the invention in water, which in themselves have good values, by adding these solids, for example in amounts of 0.5 to 15% by weight, preferably in amounts of 1 to 10 wt .-%, can still be increased.
  • the products obtained according to the invention, which are quickly soluble in water, are low-dust granules.
  • the grain sizes or certain grain size ranges can be controlled via the process parameters of the mechanically operating mixers or granulators used. Bulk weights between 400 and 600 g / l and particle size ranges are preferably set, less than 5% by weight having a particle diameter below 0.1 mm and at least 85% by weight having a maximum particle diameter of 1.6 mm.
  • surfactant granules having the following composition are produced which contain more than 40% by weight, preferably 50 to 95% by weight and in particular 80 to 90% by weight, of anionic surfactants, preferably C8-C22- Have alkyl sulfates, in particular C12-Ci ⁇ -alkyl sulfates, Cjs-Cis-alkyl sulfates or cuts with higher proportions of C12 and d j4.
  • Example 1 analogously to the disclosure of EP-A-0 319 819, half-sulfuric acid (FAS1 and FAS2) were spray-neutralized with 50% by weight sodium hydroxide solution via a multi-component nozzle.
  • the spray-neutralized products FAS1 and FAS2 obtained had the composition given below (Table 1).
  • the spray-neutralized, relatively dusty products were transferred directly, ie without intermediate storage, to the mixers specified below.
  • granules with a bulk density of at least 400 g / l were produced which had good dissolving behavior in water.
  • Baten B B mean 1 2 1.5 1.5 ⁇ 0.5
  • Example 1 Spout diameter of radially symmetrical stainless steel bunkers after 24-hour storage according to the Jenike shear test (AW Jenike, Gravity Flow of Bulk Solids, Bulletin of the University of Utah No. 108, Vol. 52 (No.29), October 1961 and AW Jenike, Storage and Flow of Solids, Bulletin of the University of Utah No. 123, Vol. 53 (No.26), November 1964)
  • Example 1 was repeated with the FAS 2 type. The composition, bulk density and grain size distribution were in the same size range as for FAS 1.
  • Examples 2 and 3 show the effects of the residence time on the particle size distribution and the bulk density.
  • Examples 4 and 5 show the effects of the granulation temperature on the bulk density.
  • the improved flow properties of the products 2 to 6 produced according to the invention can be read off from the value of the required outlet diameter of a bunker: for a further processing of a relatively dusty, only spray-neutralized product according to Example 1 after storage in a bunker, this would have to have an outlet diameter of 3 , 1 m, while for products according to one of the examples 2 to 6 outlet diameters of less than 1 m are sufficient.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Materials For Medical Uses (AREA)
  • Compounds Of Unknown Constitution (AREA)

Abstract

L'invention concerne un procédé de fabrication de granulés de tensioactif à faible teneur en poussière, présentant une masse volumique apparente élevée mais une bonne solubilité dans l'eau. Ce procédé consiste à exposer séparément au moins un tensioactif anionique sous sa forme acide et un constituant alcalin aqueux extrêmement concentré, à l'action d'une substance gazeuse, à les combiner, à les neutraliser dans un ajutage à plusieurs constituants puis à les pulvériser dans une tour de séchage avec une pression de gaz propulseur élevée. Les constituants acides et alcalins sont combinés dans des proportions pratiquement st÷chiométriques et les produits solides obtenus, à fines particules, sont transportés dans un mélangeur mécanique où les fines particules sont agglomérées pour donner des granulés présentant une masse volumique apparente d'au moins 400 g/l.
PCT/EP1995/002777 1994-07-25 1995-07-14 Procede de fabrication de granules de tensioactif WO1996003488A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE59502656T DE59502656D1 (de) 1994-07-25 1995-07-14 Verfahren zur herstellung von tensidgranulaten
EP95926892A EP0772674B1 (fr) 1994-07-25 1995-07-14 Procede de fabrication de granules de tensioactif
DK95926892T DK0772674T3 (da) 1994-07-25 1995-07-14 Fremgangsmåde til fremstilling af tensidgranulater

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP4425968.9 1994-07-25
DE4425968A DE4425968A1 (de) 1994-07-25 1994-07-25 Verfahren zur Herstellung von Tensidgranulaten

Publications (1)

Publication Number Publication Date
WO1996003488A1 true WO1996003488A1 (fr) 1996-02-08

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1995/002777 WO1996003488A1 (fr) 1994-07-25 1995-07-14 Procede de fabrication de granules de tensioactif

Country Status (6)

Country Link
EP (1) EP0772674B1 (fr)
AT (1) ATE167700T1 (fr)
DE (2) DE4425968A1 (fr)
DK (1) DK0772674T3 (fr)
ES (1) ES2117433T3 (fr)
WO (1) WO1996003488A1 (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6683042B1 (en) 1998-09-29 2004-01-27 Henkel Kommanditgesellschaft Auf Aktien (Henkel Kgaa) Granulation method
WO2009158449A1 (fr) * 2008-06-25 2009-12-30 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2009158221A1 (fr) * 2008-06-25 2009-12-30 The Procter & Gamble Company Procédé de séchage par pulvérisation
US7811980B1 (en) 2009-06-09 2010-10-12 The Procter & Gamble Company Spray-drying process
WO2011075520A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2011075434A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2011075504A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2011075521A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
US8435936B2 (en) 2009-12-18 2013-05-07 The Procter & Gamble Company Spray-drying process

Families Citing this family (8)

* Cited by examiner, † Cited by third party
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DE19617085A1 (de) * 1996-04-29 1997-10-30 Bayer Ag Verfahren zur Herstellung von feinstteiligen Kristallisationsprodukten
DE19820943A1 (de) 1998-05-11 1999-11-18 Henkel Kgaa Alkylsulfat-Granulate
DE19844523A1 (de) 1998-09-29 2000-03-30 Henkel Kgaa Granulationsverfahren
DE19855380A1 (de) * 1998-12-01 2000-06-08 Henkel Kgaa Granulationsverfahren
DE19910789A1 (de) * 1999-03-11 2000-09-14 Henkel Kgaa Granulationsverfahren
DE10003124A1 (de) 2000-01-26 2001-08-09 Cognis Deutschland Gmbh Verfahren zur Herstellung von Tensidgranulaten
DE10163603B4 (de) 2001-12-21 2006-05-04 Henkel Kgaa Verfahren zur Herstellung builderhaltiger Tensidgranulate
DE102004005761A1 (de) * 2004-02-05 2005-06-02 Henkel Kgaa Neutralisationsverfahren

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DE2203552A1 (de) * 1971-02-01 1972-08-10 Colgate Palmolive Co Neutralisations-Verfahren fuer in Saeureform vorliegende Tenside
CH555888A (it) * 1966-03-18 1974-11-15 Micol Anstalt Procedimento e dispositivo per la produzione di detergenti sintetici in forma granulare.
EP0319819A1 (fr) * 1987-12-07 1989-06-14 Henkel Kommanditgesellschaft auf Aktien Procédé d'obtention de produits solides ou pâteux
WO1994005767A1 (fr) * 1992-09-08 1994-03-17 Unilever Plc Composition de detergent et procede de production
JPH06166898A (ja) * 1992-12-01 1994-06-14 Lion Corp 高嵩密度洗剤組成物の製造方法
DE4304062A1 (de) * 1993-02-11 1994-08-18 Henkel Kgaa Verfahren zur Herstellung von Tensidgranulaten

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH555888A (it) * 1966-03-18 1974-11-15 Micol Anstalt Procedimento e dispositivo per la produzione di detergenti sintetici in forma granulare.
DE2203552A1 (de) * 1971-02-01 1972-08-10 Colgate Palmolive Co Neutralisations-Verfahren fuer in Saeureform vorliegende Tenside
EP0319819A1 (fr) * 1987-12-07 1989-06-14 Henkel Kommanditgesellschaft auf Aktien Procédé d'obtention de produits solides ou pâteux
WO1994005767A1 (fr) * 1992-09-08 1994-03-17 Unilever Plc Composition de detergent et procede de production
JPH06166898A (ja) * 1992-12-01 1994-06-14 Lion Corp 高嵩密度洗剤組成物の製造方法
DE4304062A1 (de) * 1993-02-11 1994-08-18 Henkel Kgaa Verfahren zur Herstellung von Tensidgranulaten

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6683042B1 (en) 1998-09-29 2004-01-27 Henkel Kommanditgesellschaft Auf Aktien (Henkel Kgaa) Granulation method
JP2011525215A (ja) * 2008-06-25 2011-09-15 ザ プロクター アンド ギャンブル カンパニー 噴霧乾燥プロセス
WO2009158449A1 (fr) * 2008-06-25 2009-12-30 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2009158221A1 (fr) * 2008-06-25 2009-12-30 The Procter & Gamble Company Procédé de séchage par pulvérisation
EP2138565A1 (fr) * 2008-06-25 2009-12-30 The Procter and Gamble Company Procédé de séchage par atomisation
EP2138566A1 (fr) * 2008-06-25 2009-12-30 The Procter and Gamble Company Procédé de séchage par atomisation
US7842657B2 (en) 2008-06-25 2010-11-30 The Procter & Gamble Company Spray-drying process
US7811980B1 (en) 2009-06-09 2010-10-12 The Procter & Gamble Company Spray-drying process
WO2011075434A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2011075504A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
WO2011075521A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
EP2338968A1 (fr) * 2009-12-18 2011-06-29 The Procter & Gamble Company Procédé de séchage par atomisation
EP2338969A1 (fr) * 2009-12-18 2011-06-29 The Procter & Gamble Company Procédé de séchage par atomisation
EP2341124A1 (fr) * 2009-12-18 2011-07-06 The Procter & Gamble Company Procédé de séchage par atomisation
EP2341123A1 (fr) * 2009-12-18 2011-07-06 The Procter & Gamble Company Procédé de séchage par atomisation
WO2011075520A1 (fr) * 2009-12-18 2011-06-23 The Procter & Gamble Company Procédé de séchage par pulvérisation
US8361357B2 (en) 2009-12-18 2013-01-29 The Procter & Gamble Company Spray-drying process
US8435936B2 (en) 2009-12-18 2013-05-07 The Procter & Gamble Company Spray-drying process
US8568629B2 (en) 2009-12-18 2013-10-29 The Procter & Gamble Company Spray-Drying process
RU2499038C1 (ru) * 2009-12-18 2013-11-20 Дзе Проктер Энд Гэмбл Компани Способ сушки распылением

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EP0772674B1 (fr) 1998-06-24
DE59502656D1 (de) 1998-07-30
EP0772674A1 (fr) 1997-05-14
ATE167700T1 (de) 1998-07-15
DK0772674T3 (da) 1999-04-06
DE4425968A1 (de) 1996-02-01
ES2117433T3 (es) 1998-08-01

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