[go: up one dir, main page]

EP0632826B1 - Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels - Google Patents

Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels Download PDF

Info

Publication number
EP0632826B1
EP0632826B1 EP93906531A EP93906531A EP0632826B1 EP 0632826 B1 EP0632826 B1 EP 0632826B1 EP 93906531 A EP93906531 A EP 93906531A EP 93906531 A EP93906531 A EP 93906531A EP 0632826 B1 EP0632826 B1 EP 0632826B1
Authority
EP
European Patent Office
Prior art keywords
alkyl
sulfates
ether
granules
sulfonates
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
EP93906531A
Other languages
German (de)
English (en)
Other versions
EP0632826A1 (fr
Inventor
Franz-Josef Carduck
Paul Schulz
Rainer Eskuchen
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 EP0632826A1 publication Critical patent/EP0632826A1/fr
Application granted granted Critical
Publication of EP0632826B1 publication Critical patent/EP0632826B1/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
    • C11D1/66Non-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
    • 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
    • C11D1/29Sulfates of polyoxyalkylene ethers
    • 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
    • C11D1/667Neutral esters, e.g. sorbitan esters
    • 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
    • C11D1/75Amino oxides

Definitions

  • the invention relates to a process for producing free-flowing detergent and cleaning agent granules and / or partial granules, in which aqueous alkyl and / or alkenyl oligoglycoside pastes are dried in a turbine dryer with rotating internals in the presence of surfactants and / or further detergent and cleaning agent ingredients granulated at the same time.
  • Powdered detergents and cleaning agents are usually produced by spray drying.
  • an aqueous slurry (“slurry") of the ingredients, for example surfactants, builders and adjusting agents, is pumped into the spray tower and sprayed through nozzles located in the top of the tower. Rising air with a temperature of 250 to 300 ° C dries the slurry and evaporates the adhering water, so that at the outlet of the tower a practically water-free granular or powdery Product is received. Details of this process are described, for example, in ROEMPP Chemie Lexikon, Thieme Verlag, Stuttgart, Vol. V, 1992 under the keyword “spray drying”.
  • European patent application EP-A 0 411 477 relates to a process for spray drying alkyl glucosides at 160 to 170 ° C., in which aqueous solutions with a very low surfactant content are used and the drying is carried out in the presence of a very large amount of carrier salt.
  • the object of the invention was therefore to develop a new process for the production of detergent and cleaning agent granules and / or partial granules which is free from the disadvantages described.
  • the invention relates to a process for producing free-flowing detergent and cleaning agent granules and / or partial granules, which is characterized in that aqueous alkyl and / or alkenyl oligoglycoside pastes in the presence of anionic and / or nonionic surfactants and / or usual detergent and cleaning agent ingredients in a turbine dryer with rotating internals dewatered to a residual water content of 0.1 to 5 wt .-% and granulated at the same time.
  • Alkyl and / or alkenyl oligoglycosides which are derived from aldoses or ketoses and, in particular, from glucose because of their easy availability are preferred.
  • the preferred alkyl oligoglycosides are thus the alkyl oligo glucoside .
  • Alkyl oligoglycosides with an average degree of oligomerization p of from 1.1 to 3.0 are preferred; those alkyl and / or alkenyl oligoglycosides whose degree of oligomerization is less than 1.7 and in particular between 1.2 and 1.4 are particularly preferred.
  • the radical R 1 can be derived from saturated and / or unsaturated primary alcohols having 8 to 22, preferably 8 to 10 or 12 to 18, carbon atoms.
  • Typical examples are capric alcohol, 2-ethylhexanol, caprylic alcohol, lauryl alcohol, isotridecyl alcohol, myristyl alcohol, cetyl alcohol, palmoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, dieol alcohol, aryl alcohol alcohol, dieolyl alcohol, aryl alcohol, diesyl alcohol, diesyl alcohol alcohol, dieol alcohol alcohol, dieol alcohol alcohol alcohol, dieol alcohol alcohol alcohol
  • alkyl and / or alkenyl oligoglycosides can also be present in the form of their adducts with 1 to 30 moles of ethylene, propylene and / or butylene oxide.
  • Alkyl and / or alkenyl oligoglycosides are known substances which can be obtained by the relevant methods of preparative organic chemistry.
  • a process for their preparation is, for example, the acid-catalyzed acetalization of glucose with fatty alcohols.
  • the alkyl and / or alkenyl oligoglycosides are used in the form of aqueous pastes which can have a water content of 20 to 80, preferably 30 to 50% by weight, based on the paste.
  • the anionic surfactants can be selected, for example, from the group consisting of soaps, alkylbenzenesulfonates, olefin sulfonates, alkanesulfonates, alkyl ether sulfonates, alpha sulfo fatty acids, internal sulfo fatty acids, alpha ester sulfonates, Glycerin ether sulfonates, alkyl sulfates, alkyl ether sulfates with conventional or narrow homolog distribution, glycerin ether sulfates, monoglyceride (ether) sulfates, hydroxy mixed ether sulfates, alkyl oligoglucoside sulfates, isethionates, taurides, sarcosinates, ether carboxylic acids, sulfosuccinates, and sulfonate ether sulfates, is formed.
  • soaps alkylbenz
  • nonionic surfactants such.
  • B substances which are selected from the group formed by fatty alcohol polyglycol ethers with conventional or narrow homolog distribution, alkylphenol polyglycol ethers, mixed ethers, amine oxides, sugar esters, sorbitan esters and polysorbates.
  • Under detergent and cleaner ingredients are, for example, mixing components selected from the group consisting of alkali and alkaline earth metal phosphates and phosphonates of, zeolites, NTA, EDTA, citric acid, polycarboxylic acids, alkali metal and alkaline earth metal carbonates, sulfates, silicates, borates and citrates, Starch, sucrose, polydextrose, active oxygen carriers, bleach activators, optical brighteners and defoamers.
  • alkali and alkaline earth metal phosphates and phosphonates of, zeolites, NTA, EDTA, citric acid, polycarboxylic acids, alkali metal and alkaline earth metal carbonates, sulfates, silicates, borates and citrates, Starch, sucrose, polydextrose, active oxygen carriers, bleach activators, optical brighteners and defoamers.
  • the ratio of the individual components to one another is not critical as long as it is ensured that the feed materials can be metered into the turbine mixer without any problems, ie with the aid of conventional pumps or other conveying means.
  • Turbine dryers are to be understood as cylindrical drying apparatuses, preferably in a horizontal construction, in which rotating internals at high speed ensure a fine distribution of the dry material.
  • these internals are, for example, wings, blades or paddles which are mounted on a rotating shaft (peripheral speed 5 to 25 m / s, preferably 10 to 20 m / s).
  • the actual drying can take place at wall temperatures of 100 to 180 ° C and gas phase temperatures of 150 to 220 ° C, preferably in the presence of air, inert gases such as nitrogen or superheated steam, whereby the heat transfer takes place by convection and the heated wall of the dryer.
  • a temperature of the gas phase of 150 to 220 ° C. has proven to be optimal.
  • the dry goods can be separated off, for example, using a cyclone and / or a bag filter.
  • Special features of the turbine dryers to be used according to the invention are thus the short residence time, the narrow residence time spectrum and the high temperature stabilization, which ensure that the dry material is treated as gently as possible, particularly with regard to its composition and color.
  • the detergent and cleaning agent granules and / or partial granules obtainable by the process according to the invention have a residual water content of 0.1 to 5% by weight and an advantageously narrow particle size distribution. They are suitable, for example, for producing powder detergents, in which they can be present in concentrations of 10 to 100% by weight, based on the detergents.
  • the detergent and cleaning agent granules and / or partial granules were produced in a horizontally arranged turbo dryer (type ES 2050, Vomm, Milan, Italy) with a turbine diameter of 0.34 m and a turbine length of 2.4 m , in which a shaft with blades or vanes rotated at high speed.
  • Components A) and B) were continuously introduced at two metering points of the turbine dryer which follow each other axially in the direction of flow.
  • the mixture was finely distributed in a hot, turbulent air stream and dewatered at the same time.
  • the drying temperature was 160 to 180 ° C and was transferred on the one hand by convection and on the other hand via the heated jacket of the dryer.
  • the granulated dry material was separated from the gas stream at the outlet of the turbine dryer using a cyclone and a bag filter. A light-colored, free-flowing granulate with a narrow particle size distribution was obtained, the residual water content of which was 1.5% by weight.
  • Example 1 was repeated. The following were used as input materials:

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)
  • Molecular Biology (AREA)
  • Detergent Compositions (AREA)

Claims (8)

  1. Procédé de préparation de granulés et/ou de granulés partiels de produits de lavage et de nettoyage,
    caractérisé en ce qu'
    on déshydrate des pâtes aqueuses d'alkyl et/ou alcényloligoglycosides en présence de tensioactifs anioniques et/ou non ioniques et/ou de composants usuels des produits de lavage et de nettoyage dans un sécheur à turbine à pales rotatives jusqu'à une teneur résiduelle en eau de 0,1 à 5 % en poids et on granule simultanément.
  2. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on utilise des alkyl et/ou alcényloligoglycosides de formule (I),

            R1O-(R2O)x-[G]p

    où,
    R1   est un radical hydrocarbure aliphatique de 8 à 22 atomes de carbone et avec 0, 1, 2 ou 3 doubles liaisons,
    R2   est un radical alkylène de 2 à 4 atomes de carbone,
    x   est O ou un nombre de 1 à 30,
    [G]   est un radical sucre de 5 à 6 atomes de carbone et,
    p   est un nombre de 1 à 10.
  3. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on utilise des alkyl et/ou alcényloligoglycosides qui ont une teneur en eau de 20 à 80 % en poids par rapport à la pâte.
  4. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on utilise des tensioactifs anioniques qu'on choisit dans le groupe constitué des savons, sulfonates de benzène d'alkyle, oléfinesulfonates, alcanesulfonates, alkyl éthersulfonates, acides gras alpha sulfoniques, acides gras sulfoniques internes, alpha estersulfonates, éthersulfonates de glycérine, alkylsulfates, alkyléthersulfates à répartition d'homologues classique ou concentrée, éthersulfates de glycérine, (éther)sulfates de monoglycéride, sulfates d'ethers hydroxyles mixtes, sulfates d' alkyloligoglucosides, iséthionates, taurides, sarcosinates, acides éthercarboxyliques, sulfosuccinates, sulfotriglycérides et alkyl(éther)-phosphates.
  5. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on utilise des tensioactifs non ioniques qu'on choisit dans le groupe constitué des poly(éthers de glycol) et d'alcool gras à répartition classique ou resserrée d'homologues, des poly(éthers de glycol) et d'alkylphénol, des éthers mixtes, des oxydes d'amines, des esters de sucres, des esters de sorbitane et des polysorbates.
  6. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on utilise des composants de produits de lavage et de nettoyage qu'on choisit dans le groupe constitué des phosphates et phosphonates alcalins et alcalino-terreux, des zéolithes, de NTA, de EDTA, de l'acide citrique, des acides polycarboxyliques, des carbonates, sulfates, silicates, borates et citrates alcalins et alcalino-terreux, de l'amidon, du saccharose, du polydextrose, des véhicules d'oxygène actif, des activateurs de blanchiment, des azurants optiques et des produits anti-mousse.
  7. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on réalise le séchage ou la granulation à une température de paroi de 100 à 180°C et à une température de phase gazeuse de 150 à 220°C.
  8. Procédé selon la revendication 1,
    caractérisé en ce qu'
    on réalise le séchage ou la granulation en présence d'air, de gaz inerte et/ou de vapeur d'eau surchauffée.
EP93906531A 1992-03-23 1993-03-15 Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels Expired - Lifetime EP0632826B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4209339A DE4209339A1 (de) 1992-03-23 1992-03-23 Verfahren zur Herstellung rieselfähiger Wasch- und Reinigungsmittelgranulate und/oder -teilgranulate
DE4209339 1992-03-23
PCT/EP1993/000593 WO1993019155A1 (fr) 1992-03-23 1993-03-15 Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels

Publications (2)

Publication Number Publication Date
EP0632826A1 EP0632826A1 (fr) 1995-01-11
EP0632826B1 true EP0632826B1 (fr) 1996-09-04

Family

ID=6454760

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93906531A Expired - Lifetime EP0632826B1 (fr) 1992-03-23 1993-03-15 Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels

Country Status (8)

Country Link
US (1) US5536431A (fr)
EP (1) EP0632826B1 (fr)
JP (1) JPH07504931A (fr)
AT (1) ATE142252T1 (fr)
DE (2) DE4209339A1 (fr)
ES (1) ES2090986T3 (fr)
GR (1) GR3021062T3 (fr)
WO (1) WO1993019155A1 (fr)

Families Citing this family (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4321840A1 (de) * 1993-07-01 1995-01-12 Henkel Kgaa Verfahren zur Herstellung von Alkyl- und/oder Alkenyloligoglucosiden
DE4337032C1 (de) * 1993-10-29 1995-05-24 Henkel Kgaa Verwendung von Detergensgemischen zur Herstellung von Toilettensteinen
GB9417354D0 (en) * 1994-08-26 1994-10-19 Unilever Plc Detergent particles and process for their production
GB9417356D0 (en) * 1994-08-26 1994-10-19 Unilever Plc Detergent particles and process for their production
GB9424444D0 (en) * 1994-12-02 1995-01-18 Unilever Plc Detergent compositions
DE4446444A1 (de) * 1994-12-23 1996-06-27 Henkel Kgaa Verfahren zur Herstellung von wasserfreien Tensiden
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
GB9606913D0 (en) * 1996-04-02 1996-06-05 Unilever Plc Surfactant blends processes for preparing them and particulate detergent compositions containing them
DE19641275C1 (de) * 1996-10-07 1998-03-12 Henkel Kgaa Verfahren zur Herstellung wasser- und staubfreier Aniontensidgranulate
US5914308A (en) * 1996-10-23 1999-06-22 Henkel Corporation Process for agglomerating detergent powders
US5733863A (en) * 1997-01-17 1998-03-31 The Procter & Gamble Company Process for making a free-flowing particule detergent admix containing nonionic surfactant
DE19707649C1 (de) * 1997-02-26 1998-10-22 Henkel Kgaa Verfahren zur Herstellung von Waschmittelrohstoffen
EP0861885B1 (fr) * 1997-02-27 2003-04-16 The Procter & Gamble Company Compositions pour trempage
DE19710153C1 (de) 1997-03-12 1998-02-12 Henkel Kgaa Verfahren zur Herstellung neutraler Zuckertensidgranulate
EP1007613A1 (fr) * 1997-08-25 2000-06-14 Cognis Deutschland GmbH Procede de production de granules d'agents de surface anioniques exempts d'eau et de poussiere
DE19806495C1 (de) * 1998-02-17 1999-01-14 Henkel Kgaa Verfahren zur Herstellung wasser- und staubfreier Aniontensidgranulate
US6608021B1 (en) * 1998-09-25 2003-08-19 The Procter & Gamble Co. Granular detergent composition having improved appearance and solubility
DE10018812A1 (de) * 2000-04-15 2001-10-25 Cognis Deutschland Gmbh Verfahren zur Herstellung von nichtionischen Tensidgranulaten
DE10214388A1 (de) * 2002-03-30 2003-10-16 Cognis Deutschland Gmbh Verfahren zur Herstellung fester Mittel
DE102024109023A1 (de) * 2024-03-28 2025-10-02 inprotec GmbH Trocknungsverfahren

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3703772A (en) * 1971-07-27 1972-11-28 Colgate Palmolive Co Drying of detergents
US4536319A (en) * 1983-10-04 1985-08-20 The Procter & Gamble Company Compositions comprising alkylpolysaccharide detergent surfactant
US4675127A (en) * 1985-09-26 1987-06-23 A. E. Staley Manufacturing Company Process for preparing particulate detergent compositions
DE3723826A1 (de) * 1987-07-18 1989-01-26 Henkel Kgaa Verfahren zur herstellung von alkylglykosiden
US4894117A (en) * 1988-04-28 1990-01-16 Colgate-Palmolive Company Process for manufacturing high bulk density particulate fabric softening synthetic anionic organic detergent compositions
DE3925858A1 (de) * 1989-08-04 1991-02-07 Henkel Kgaa Pulverfoermige zubereitungen oberflaechenaktiver alkylglykoside
KR0170424B1 (ko) * 1990-07-05 1999-01-15 호르스트 헤를레,요한 글라슬 세제 및 청정제용 표면 활성제 과립의 제조방법

Also Published As

Publication number Publication date
JPH07504931A (ja) 1995-06-01
ATE142252T1 (de) 1996-09-15
WO1993019155A1 (fr) 1993-09-30
ES2090986T3 (es) 1996-10-16
DE4209339A1 (de) 1993-09-30
DE59303669D1 (de) 1996-10-10
US5536431A (en) 1996-07-16
EP0632826A1 (fr) 1995-01-11
GR3021062T3 (en) 1996-12-31

Similar Documents

Publication Publication Date Title
EP0632826B1 (fr) Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels
EP0663946B1 (fr) Produits d'interet et melanges de produits d'interet pour agents mouillants, detergents et/ou nettoyants sous une nouvelle forme de preparation
DE2050560C3 (fr)
DE69332270T2 (de) Verfahren zum herstellen von kompakten waschmittelzusammensetzungen
DE19524464C2 (de) Verfahren zur Herstellung von Zuckertensidgranulaten
DE19707649C1 (de) Verfahren zur Herstellung von Waschmittelrohstoffen
EP0863979B1 (fr) Procede de fabrication de granules tensioactifs de sucre sans eau ni poussiere
EP0859048B1 (fr) Procédé pour la fabrication de granules tensioactifs
EP0682690A1 (fr) Tensioactifs anioniques a solubilite amelioree.
EP0966516B1 (fr) Procede de production de granules tensioactifs de type sucre neutres
DE19543990C2 (de) Flüssige Vorprodukte für Wasch-, Spül- und Reinigungsmittel
DE19806495C1 (de) Verfahren zur Herstellung wasser- und staubfreier Aniontensidgranulate
DE19961333A1 (de) Verfahren zur Herstellung von Zuckertensidgranulaten
EP0929647B2 (fr) Procede de production de granules de tensioactifs anioniques anhydres et sans poussiere
DE19520105A1 (de) Verfahren zur Herstellung wasserfreier, rieselfähiger Tensidpulver
EP1131400B1 (fr) Procede de production de granules tensioactifs
DE10002709A1 (de) Verfahren zur Herstellung von wasser- und staubarmen Alkyl- und/oder Alkenylphosphat-Granulaten

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: 19940914

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DE ES FR GB GR IT LI NL

17Q First examination report despatched

Effective date: 19950420

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH DE ES FR GB GR IT LI NL

REF Corresponds to:

Ref document number: 142252

Country of ref document: AT

Date of ref document: 19960915

Kind code of ref document: T

ET Fr: translation filed
REF Corresponds to:

Ref document number: 59303669

Country of ref document: DE

Date of ref document: 19961010

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2090986

Country of ref document: ES

Kind code of ref document: T3

ITF It: translation for a ep patent filed
REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2090986

Country of ref document: ES

Kind code of ref document: T3

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

Effective date: 19961106

REG Reference to a national code

Ref country code: GR

Ref legal event code: FG4A

Free format text: 3021062

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

Ref country code: AT

Payment date: 20010313

Year of fee payment: 9

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

Ref country code: CH

Payment date: 20010315

Year of fee payment: 9

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

Ref country code: GR

Payment date: 20010329

Year of fee payment: 9

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

Ref country code: NL

Payment date: 20010330

Year of fee payment: 9

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

Ref country code: BE

Payment date: 20010516

Year of fee payment: 9

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

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: 20020315

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

Ref country code: LI

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

Effective date: 20020331

Ref country code: CH

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

Effective date: 20020331

Ref country code: BE

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

Effective date: 20020331

BERE Be: lapsed

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

Effective date: 20020331

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 NON-PAYMENT OF DUE FEES

Effective date: 20021001

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

Ref country code: GR

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

Effective date: 20021007

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 20021001

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

Ref country code: GB

Payment date: 20030312

Year of fee payment: 11

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

Ref country code: ES

Payment date: 20030328

Year of fee payment: 11

REG Reference to a national code

Ref country code: GB

Ref legal event code: 732E

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

Ref country code: GB

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

Effective date: 20040315

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: 20040316

REG Reference to a national code

Ref country code: FR

Ref legal event code: TP

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

Effective date: 20040315

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20040316

REG Reference to a national code

Ref country code: FR

Ref legal event code: TP

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

Ref country code: IT

Payment date: 20120322

Year of fee payment: 20

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

Ref country code: DE

Payment date: 20120531

Year of fee payment: 20

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

Ref country code: FR

Payment date: 20120419

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 59303669

Country of ref document: DE

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 EXPIRATION OF PROTECTION

Effective date: 20130316