EP0859048B1 - Procédé pour la fabrication de granules tensioactifs - Google Patents

Procédé pour la fabrication de granules tensioactifs Download PDF

Info

Publication number
EP0859048B1
EP0859048B1 EP98100768A EP98100768A EP0859048B1 EP 0859048 B1 EP0859048 B1 EP 0859048B1 EP 98100768 A EP98100768 A EP 98100768A EP 98100768 A EP98100768 A EP 98100768A EP 0859048 B1 EP0859048 B1 EP 0859048B1
Authority
EP
European Patent Office
Prior art keywords
weight
granules
surfactant
cleaning
process according
Prior art date
Legal status (The legal status 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 status listed.)
Expired - Lifetime
Application number
EP98100768A
Other languages
German (de)
English (en)
Other versions
EP0859048A3 (fr
EP0859048A2 (fr
Inventor
Georg Dr. Assmann
Hans-Friedrich Kruse
Volker Dr. Bauer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0859048A2 publication Critical patent/EP0859048A2/fr
Publication of EP0859048A3 publication Critical patent/EP0859048A3/fr
Application granted granted Critical
Publication of EP0859048B1 publication Critical patent/EP0859048B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/662Carbohydrates or derivatives
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/83Mixtures of non-ionic with anionic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082Special methods for preparing compositions containing mixtures of detergents 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
    • C11D11/0088Special methods for preparing compositions containing mixtures of detergents 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 the liquefied ingredients being sprayed or adsorbed onto solid particles
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0034Fixed on a solid conventional detergent ingredient
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065High-density particulate detergent compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • C11D3/2082Polycarboxylic acids-salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • C11D3/2086Hydroxy carboxylic acids-salts thereof

Definitions

  • the invention relates to a process for the production of concentrated surfactant granules Active substance content of more than 45 wt .-%, based on the granules, which a low hygroscopicity, a significantly improved silage capacity and an increased Have bulk density.
  • Granulation is an alternative to spray drying surfactant pastes describes EP-B-0 603 207 (Henkel) a process for the production of washing and cleaning active Surfactant granules with a bulk density above 500 g / l by simultaneous Granulation and drying in all devices in which granulation can be done with simultaneous drying.
  • a surfactant preparation form which is a non-surfactant liquid component (usually water) has, if desired granulated with the addition of a solid component and dried at the same time.
  • the simultaneous spraying also provides of active substance and carrier component solution through one and the same nozzle here is a possible but not a mandatory process parameter.
  • the object of the invention was to provide a method for producing heavy, free-flowing, to provide highly concentrated surfactant granules with bulk densities above 600 g / l, the granules obtained have advantages in terms of ensiling ability and Show hygroscopicity.
  • the process according to the invention has the advantage that the resulting grain is conditional due to the inclusion of surfactant phases in phases of the carrier material, an increased mechanical Stability and an extremely reduced water absorption during storage.
  • the granules obtained by the process according to the invention are accordingly very easy to pour and ensilage and stick together due to their low tendency to absorb water. With separate injection of active substance and carrier paste in the granulation unit is the product even at low surfactant concentrations sticky and cakes on drying, adding the products are hygroscopic and stick in the course of heavy water absorption.
  • the solutions of the active substance and the carrier substance are carried out according to the invention one and the same nozzle atomized.
  • the solutions can only be mixed in the nozzle mixed, i.e. fed to the nozzle via separate storage containers and feed lines but also a mixture of both solutions from a single storage container can be injected through a nozzle.
  • the non-surfactant solvent which may contain one or more components, has a boiling point or boiling range preferably below normal pressure 250 ° C and especially below 200 ° C. With particular advantage, it contains components which boil between 60 and 180 ° C at normal pressure.
  • organic constituents of the non-surfactant solvent are preferably mono- and / or polyfunctional alcohols, for example methanol, ethanol, propanol, Isopropanol, butanol, secondary and tertiary butanol, pentanol, ethylene glycol, 1,2-propanediol, Glycerin or mixtures of these are used.
  • the inorganic component of the non-surfactant Solvent water optionally together with organic components such as ethanol, 1,2-propanediol or glycerin.
  • the share is of the water preferably 25 to 80 wt .-%, based on the total amount of non-surfactant solvent.
  • the solutions of surfactants and carrier materials in Non-surfactant solvents can be used in a wide range of concentrations are taken into account, with only a viscosity that is still suitable for atomization got to.
  • the proportion of the non-surfactant is Solvent 30 to 70 wt .-% and in particular 45 to 60 wt .-%.
  • alkylbenzenesulfonates ABS
  • alkylpolyglycosides APG
  • APG alkylpolyglycosides
  • APG alkylpolyglycosides
  • R is one primary, straight-chain or in the 2-position methyl branched aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms
  • G is a symbol which represents a glucose unit with 5 or 6 carbon atoms
  • the degree of oligomerization x between 1 and 10, preferably between 1 and 2 and in particular is significantly smaller than 1.4.
  • ABS and / or APG surfactants in addition to the ABS and / or APG surfactants also other anionic, nonionic, cationic or amphoteric surfactants can be used in combination with the former. While the process is mainly used to manufacture ABS and / or APG compounds suitable are additions of up to 20% by weight of other surfactants, based on the total amount of surfactant, possible without losing the advantages of the method according to the invention.
  • the carrier materials used in the process according to the invention can be inorganic and / or organic in nature.
  • they consist of amorphous alkali silicates of the formula (SiO 2 ) m (M 2 O) n1 (so-called water glasses) and / or crystalline layered silicates of the formula (SiO 2 ) m ((M 2 O) n2 (H 2 O ) x , where M is lithium, sodium or potassium, m and n1 are integers or fractional numbers greater than 0, n2 is 1 and x is 0 or integers from 1 to 20.
  • inorganic salts or organic polycarboxylates into consideration.
  • sodium carbonate is among the inorganic salts preferred, while as polycarboxylates preferably citric acid / citrates and / or Acrylic acid / maleic acid copolymers are used.
  • the detergent granules which are active in washing and cleaning, have, based on the finished granulate, Carrier material contents of 10 to 50 wt .-%. Because highly concentrated surfactant granules Preferred for economic reasons are carrier material contents from below 40, in particular below 30% by weight, is preferred. In addition to the so-called over-dried Water glasses can also be found in preferred embodiments of the invention Sodium carbonate, acrylic acid / maleic acid copolymers and trisodium citrate as carrier materials Use. Mixtures of the carrier substances are also preferred, in particular Carbonate / silicate mixtures as well as citrate / silicate mixtures.
  • the surfactant preparation form is granulated and dried, using the method according to the invention.
  • Process granulate particles are obtained in which the active substance is partially enclosed by the carrier. Under drying, this becomes partially or completely remove the non-surfactant solvent.
  • the non-surfactant solvent is preferably removed almost completely.
  • the preparation of the surfactant granules can be carried out by the process according to the invention in all devices take place in which a granulation under drying conditions can be carried out.
  • Examples include heated mixers and granulators, especially high-speed ring mix dryers such as Turbo dryer® granulators (Device from Vomm, Italy).
  • the Invention however, that the combination of the two process steps in a batch or continuously running fluidized bed is carried out. It is special preferred to carry out the process continuously in the fluidized bed.
  • there the surfactant preparation form is introduced into the fluidized bed from a common nozzle.
  • the mixture of the two liquid to pasty components of the surfactant preparation form can be done beforehand or only in the nozzle.
  • Fluid bed apparatuses used have base plates with dimensions of at least 0.4 m.
  • fluidized bed apparatuses are preferred which have a base plate have a diameter between 0.4 and 5 m, for example 1.2 m or 2.5 m.
  • fluidized bed apparatuses are also suitable which have a base plate with a have a diameter greater than 5 m.
  • a perforated base plate is preferably used as the base plate or a Conidur plate (commercial product from Hein & Lehmann, Federal Republic Germany).
  • the method according to the invention is preferred at vortex air speeds between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s performed.
  • the granules are discharged from the fluidized bed advantageously via a size classification of the granules.
  • This classification can for example with a screening device or through an opposed air flow (Classifier air), which is regulated so that only particles above a certain particle size removed from the fluidized bed and smaller particles retained in the fluidized bed become.
  • Classifier air opposed air flow
  • the inflowing settles Air from the heated or unheated classifier air and the heated soil air together.
  • 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 loss and by the heat of vaporization of the components of the non-surfactant solvent from.
  • the temperature of the fluidizing air is about 5 cm above the base plate 60 to 120 ° C, preferably 65 to 90 ° C and especially 70 to 85 ° C.
  • the air outlet temperature is preferably between 60 and 120 ° C, especially below 100 ° C and with particular advantage between 70 and 85 ° C.
  • the evaporate Components of the non-surfactant solvent partially or completely, the dried-on to dry germs with additional amounts of surfactant preparation be encased in such a way that the carrier substance is the active substance envelops.
  • This special structure of the granulate which can only be achieved by simultaneous injection Obtain active substance and carrier material solution through one and the same nozzle is the result of the evaporating non-surfactant solvent in the evaporation process Backing material from the freshly condensed layer on the grain carries and deposits on the surface of the grain when evaporating.
  • a powdering agent preferably zeolite or sodium carbonate Fluidized bed
  • these powdering agents reduce the amount of granulation the stickiness of the moist granules and thus promote turbulence and drying to the desired product.
  • this variant can be advantageous is, however, not absolutely necessary to carry out the invention.
  • the process according to the invention results in surfactant granules which dissolve easily in cold water without being hygroscopic.
  • the granules have high mechanical stability and therefore excellent flow and silage properties.
  • Leave with organic solvents that do not destroy the grain structure only small amounts of active substance dissolve from the uncrushed granules, while most of the active substance can be extracted from the ground granules is.
  • the washing and cleaning active produced by the inventive method Surfactant granules have bulk densities above 600 g / l. They are ideal as components suitable for the production of detergents and cleaning agents, preferred Detergents and cleaning agents which are produced by the process according to the invention detergent-active and surfactant granules in amounts of more than 10% by weight, in particular in amounts above 20 wt .-%, based on the total washing and Detergent included.
  • a bulk density according to the invention Process produced washing and cleaning active surfactant granules above of 700 g / l, in particular above 800 g / l, is preferred.
  • the process according to the invention can advantageously be active in washing and cleaning Surfactant granules are produced, the total surfactant content, based on the total granulate is more than 40% by weight.
  • Surfactant contents above 50% by weight and in particular above 60% by weight are preferred.
  • ABS alkylbenzenesulfonate
  • APG alkylpolyglycoside
  • the process is suitable for the production of highly concentrated surfactant granules and has particular advantages if the surfactants to be processed are sticky per se Are natural, as is the case with alkylbenzenesulfonates and alkylpolyglycosides.
  • the proportion of other surfactants is 20% by weight, based on the total surfactant content, does not exceed in the granules according to the invention.
  • composition [% by weight] E1 E2 E3 E4 E5 E6 E7 E8 SECTION 45 - - - 60 50 - 61 APG - 67 80 50 - - 62 - silicate 21 22 17.5 10 13 15 - - Sokalan CP5® - - - - - - 33 - sodium citrate - - - - - - - 14 sodium 28 - - 35 - - - - zeolite - - - - 22 30 - 20 water 6 11 2.5 5 5 5 5 5 5 bulk weight [G / l] 632 641 612 651 702 734 611 633 Sokalan CP5 ® is an acrylic acid-maleic acid copolymer from BASF
  • solubilities of E1 and E2 were determined by adding 5 g each of the agent to a 1 l vessel containing 500 ml of demineralized water which was stirred by a propeller stirrer at 900 rpm. The conductivity was detected via a conductivity measuring cell and recorded on a recorder. The measurement was carried out until no increase was ascertainable. The time to reach the conductivity of the agent was set to 100%, the corresponding other dissolving times were calculated. solubility E1 E2 95% solved [min] 2.59 2.57 90% solved [min] 2.27 2.25 80% solved [min] 1.45 1.48 Residue after 1.5 min [% by weight] 2 5 Residue after 5 min [% by weight] 0 0 0
  • All compounds E1 to E8 produced according to the invention can be stored in the air without sticking or losing their free-flowing properties.
  • a comparison test between ES and a commercially available comparable ABS compound with a bulk density of 400 g / l and an active substance content of 85% by weight showed the following values after 8 hours of storage (55% relative luminous humidity): Hygroscopicity (8-hour storage trial) E5 comparison Water absorption [% by weight] 5 20 Remarks pourable bonding
  • ABS / APG compounds produced according to the invention are ideal additives suitable for detergents since they give the detergents improved solubility.

Landscapes

  • 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)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Molecular Biology (AREA)
  • Detergent Compositions (AREA)

Claims (12)

  1. Procédé de fabrication de granulats tensioactifs ayant une action lavante et nettoyante, qui présentent une densité apparente supérieure à 600 g/l, par granulation d'une préparation tensioactive, caractérisé en ce que l'on pulvérise des solutions
    a) de tensioactifs à base d'alkylbenzènesulfonates et/ou d'alkylpolyglycosides, et
    b) de substances de support, choisies parmi les polycarboxylates et les sels inorganiques, en particulier les silicates amorphes,
    dans un solvant non tensioactif, simultanément, par l'intermédiaire d'une seule et même buse et on les soumet à un séchage dans un dispositif usuel, de préférence un lit fluidisé ou un sécheur-mélangeur circulaire à vitesse de rotation élevée, une séparation entre les deux liquides ayant lieu pendant le séchage, de sorte que la substance active collante, fortement hygroscopique se trouve enfermée au moins en partie dans la substance de support non collante.
  2. Procédé selon la revendication 1, caractérisé en ce que comme solvant non tensioactif, on utilise des mono- et/ou polyalcools, de préférence dans des proportions de 0,5 à 10 % en poids, par rapport à la totalité de la solution à pulvériser.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que comme solvant non tensioactif, on utilise de l'eau, de préférence dans des proportions de 25 à 80 % en poids, par rapport à la totalité du solvant non tensioactif.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que pour maintenir le procédé de granulation en lit fluidisé, on introduit en continu dans le lit fluidisé un agent de pulvérisation, de préférence une zéolithe ou du carbonate de sodium.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que comme substance de support, on utilise un mélange silicate/citrate.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que la teneur en alkylbenzènesulfonate (ABS) du granulat tensioactif ayant une action lavante et nettoyante est supérieure à 40 % en poids, de préférence supérieure à 50 % en poids et en particulier, supérieure à 60 % en poids par rapport au granulat.
  7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que la teneur en alkylpolyglycoside (APG) du granulat tensioactif ayant une action lavante et nettoyante est supérieure à 50 % en poids, de préférence supérieure à 60 % en poids et en particulier, supérieure à 70 % en poids par rapport au granulat.
  8. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que la teneur totale en tensioactif du granulat tensioactif ayant une action lavante et nettoyante est supérieure à 40 % en poids, de préférence supérieure à 50 % en poids et en particulier, supérieure à 60 % en poids par rapport au granulat.
  9. Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce que le granulat tensioactif ayant une action lavante et nettoyante contient jusqu'à 20 % en poids d'autres tensioactifs, par rapport à la quantité d'ABS et d'APG.
  10. Granulat tensioactif ayant une action lavante et nettoyante, présentant une densité apparente supérieure à 600 g/l, préparé par un procédé selon l'une quelconque des revendications 1 à 9, contenant plus de 60 % en poids d'alkylbenzènesulfonate.
  11. Granulat tensioactif ayant une action lavante et nettoyante, présentant une densité apparente supérieure à 600 g/l, préparé par un procédé selon l'une quelconque des revendications 1 à 9, contenant plus de 60 % en poids, de préférence plus de 70 % en poids d'alkylpolyglycoside.
  12. Produit de lavage et de nettoyage, contenant au moins 10 % en poids, de préférence au moins 20 % en poids d'un produit d'un procédé selon l'une quelconque des revendications 1 à 9.
EP98100768A 1997-01-27 1998-01-17 Procédé pour la fabrication de granules tensioactifs Expired - Lifetime EP0859048B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19702845A DE19702845A1 (de) 1997-01-27 1997-01-27 Verfahren zur Herstellung von Tensidgranulaten
DE19702845 1997-01-27

Publications (3)

Publication Number Publication Date
EP0859048A2 EP0859048A2 (fr) 1998-08-19
EP0859048A3 EP0859048A3 (fr) 1999-09-08
EP0859048B1 true EP0859048B1 (fr) 2003-10-29

Family

ID=7818463

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98100768A Expired - Lifetime EP0859048B1 (fr) 1997-01-27 1998-01-17 Procédé pour la fabrication de granules tensioactifs

Country Status (4)

Country Link
EP (1) EP0859048B1 (fr)
AT (1) ATE253107T1 (fr)
DE (2) DE19702845A1 (fr)
ES (1) ES2210601T3 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11214763B2 (en) 2018-01-26 2022-01-04 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a carrier
US11377628B2 (en) 2018-01-26 2022-07-05 Ecolab Usa Inc. Solidifying liquid anionic surfactants
US11655436B2 (en) 2018-01-26 2023-05-23 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19824742A1 (de) * 1998-06-03 1999-12-09 Henkel Kgaa Herstellung Alkylpolyglycosid-haltiger Granulate
DE19923626A1 (de) * 1999-05-22 2000-11-23 Henkel Kgaa Verfahren zur Herstellung von Tensidgranulaten
DE19951598A1 (de) * 1999-10-27 2001-05-03 Cognis Deutschland Gmbh Verfahren zur Herstellugn von festen Zuckertensiden
DE19961333B4 (de) * 1999-12-17 2006-12-14 Henkel Kgaa Verfahren zur Herstellung von Zuckertensidgranulaten
DE10018812A1 (de) 2000-04-15 2001-10-25 Cognis Deutschland Gmbh Verfahren zur Herstellung von nichtionischen Tensidgranulaten
US20110005002A1 (en) * 2009-07-09 2011-01-13 Hiroshi Oh Method of Laundering Fabric

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2712529A (en) * 1948-10-21 1955-07-05 Procter & Gamble Detergent composition
US3055835A (en) * 1958-11-18 1962-09-25 Colgate Palmolive Co Drying process for detergents
US3733278A (en) * 1971-03-22 1973-05-15 Philadelphia Quartz Co Detergent slurry process
CA995092A (en) * 1972-07-03 1976-08-17 Rodney M. Wise Sulfated alkyl ethoxylate-containing detergent composition
ZA776946B (en) * 1976-12-02 1979-06-27 Colgate Palmolive Co Free flowing high bulk density particulate detergent softener
JPH0384100A (ja) * 1989-08-28 1991-04-09 Lion Corp 高嵩密度洗剤組成物の製造方法
DE4211699A1 (de) * 1992-04-08 1993-10-14 Henkel Kgaa Verfahren zur Erhöhung des Schüttgewichts sprühgetrockneter Waschmittel
DE4408502A1 (de) * 1994-02-18 1995-08-24 Henkel Ecolab Gmbh & Co Ohg Sprühgetrocknetes Granulat mit hohem Schüttgewicht
DE19524287A1 (de) * 1995-07-06 1997-01-09 Henkel Kgaa Von Staub- und Feinanteilen freie granulare Wasch- und Reinigungsmittel hoher Schüttdichte

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11214763B2 (en) 2018-01-26 2022-01-04 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a carrier
US11377628B2 (en) 2018-01-26 2022-07-05 Ecolab Usa Inc. Solidifying liquid anionic surfactants
US11655436B2 (en) 2018-01-26 2023-05-23 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier
US11834628B2 (en) 2018-01-26 2023-12-05 Ecolab Usa Inc. Solidifying liquid anionic surfactants
US11976255B2 (en) 2018-01-26 2024-05-07 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier
US12006488B2 (en) 2018-01-26 2024-06-11 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a carrier

Also Published As

Publication number Publication date
ES2210601T3 (es) 2004-07-01
EP0859048A3 (fr) 1999-09-08
DE59809988D1 (de) 2003-12-04
DE19702845A1 (de) 1998-07-30
ATE253107T1 (de) 2003-11-15
EP0859048A2 (fr) 1998-08-19

Similar Documents

Publication Publication Date Title
EP0603207B1 (fr) Procede de fabrication de granulats tensioactifs
DE69019574T2 (de) Detergens-Zusammensetzungen und Verfahren zu ihrer Herstellung.
EP0642576B1 (fr) Procede de fabrication continue d'un detergent et/ou d'un nettoyant granulaire
EP0663946B1 (fr) Produits d'interet et melanges de produits d'interet pour agents mouillants, detergents et/ou nettoyants sous une nouvelle forme de preparation
EP0541608B1 (fr) Procede de production de granules actifs de lavage et de nettoyage
DE69225679T2 (de) Teilchenförmige Waschmittelzusammensetzungen
DE69220773T2 (de) Verfahren zur Herstellung von Detergenskörnchen durch Neutralisation von Sulfonsäuren
DE4435743C2 (de) Verfahren zur Herstellung eines Mehrkomponenten-Granulates
WO1995022592A1 (fr) Produit de lavage a adjuvants au silicate amorphes
EP0632826B1 (fr) Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels
WO1993015180A1 (fr) Procede pour fabriquer des produits solides de lavage et de nettoyage de densite apparente elevee et presentant une vitesse de dissolution amelioree
EP0663005B1 (fr) Procede de fabrication de granules tensioactifs
EP0859048B1 (fr) Procédé pour la fabrication de granules tensioactifs
DE4021476A1 (de) Verfahren zur ueberfuehrung waessriger zubereitungsformen wasch- und reinigungsaktiver tensidverbindungen in lagerstabile trockengranulate
DE3838086A1 (de) Verfahren zur herstellung zeolithhaltiger granulate hoher dichte
DE4304062A1 (de) Verfahren zur Herstellung von Tensidgranulaten
WO1997003165A1 (fr) Procede de preparation de granules tensioactifs de saccharose
DE69314056T3 (de) Verwendung ethoxylierter aliphatischer alkohole als lösungsvermittler
DE68924373T2 (de) Verfahren zur Herstellung konzentrierter Granulatkörner von oberflächenaktiven Mitteln.
EP0560802B2 (fr) Procede de fabrication de granulats de zeolite
WO1994014946A1 (fr) Produits granules de lavage et/ou de nettoyage
EP0605436B1 (fr) Procede de preparation de granules de zeolithe
DE19601841A1 (de) Niotensidreiche Granulate und Verfahren zu ihrer Herstellung
EP0874684B1 (fr) Procede de production d'un additif granule
EP0473622B1 (fr) Additif granulaire sans phosphates contenant des agents tensio-actifs non ioniques pour produit a lessive

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19980117

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE DE ES FI FR GB IT NL PT SE

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

PUAL Search report despatched

Free format text: ORIGINAL CODE: 0009013

AK Designated contracting states

Kind code of ref document: A3

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

AKX Designation fees paid

Free format text: AT BE DE ES FI FR GB IT NL PT SE

17Q First examination report despatched

Effective date: 20020830

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE DE ES FI FR GB IT NL PT SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031029

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20031029

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REF Corresponds to:

Ref document number: 59809988

Country of ref document: DE

Date of ref document: 20031204

Kind code of ref document: P

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 20040107

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20040113

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 20040121

Year of fee payment: 7

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20040129

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20040128

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 20040409

Year of fee payment: 7

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2210601

Country of ref document: ES

Kind code of ref document: T3

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20040730

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20050117

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20050131

BERE Be: lapsed

Owner name: *HENKEL K.G.A.A.

Effective date: 20050131

BERE Be: lapsed

Owner name: *HENKEL K.G.A.A.

Effective date: 20050131

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040329

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20131211

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20140115

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20140108

Year of fee payment: 17

Ref country code: IT

Payment date: 20140121

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20140115

Year of fee payment: 17

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 59809988

Country of ref document: DE

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20150117

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150801

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150117

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20150930

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150202

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150117

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20160226

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20150118