EP0353976A1 - Waschmittel - Google Patents
Waschmittel Download PDFInfo
- Publication number
- EP0353976A1 EP0353976A1 EP89307771A EP89307771A EP0353976A1 EP 0353976 A1 EP0353976 A1 EP 0353976A1 EP 89307771 A EP89307771 A EP 89307771A EP 89307771 A EP89307771 A EP 89307771A EP 0353976 A1 EP0353976 A1 EP 0353976A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- powdered
- free flowing
- high active
- anionic
- detergent composition
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
- C11D11/04—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions 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 ; Methods for using cleaning compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0034—Fixed on a solid conventional detergent ingredient
Definitions
- This invention relates to detergents, and more particularly, to free flowing, high active anionic detergents.
- High active detergents for the purposes of the present invention, may be defined as detergents comprising more than 12% active matter.
- Free flowing for the purposes of the present invention, may be defined as sufficiently mobile as to be capable of being poured or dispensed reproducably as a measured quantity.
- detergent powders exemplify certain characteristics, namely, the detergent powder should be non-dusty, free flowing, easily handled, easily dissolved and stable under normal storage conditions.
- a large proportion of the worldwide detergent market uses high foaming powder surfactants, most of which are based on anionic active matter ingredients.
- a further method of manufacture of detergents in powder form is by so called 'dry neutralisation'. Dry neutralisation and associated agglomeration is normally regarded as a three part process:
- a method of producing a free flowing, high active, anionic detergent comprising the step of adsorbing an anionic surfactant acid onto a powdered or granular material to form an agglomerate without the addition of water in the agglomeration stage.
- the powdered or granular detergent composition derived from this method suprisingly has a substantially uniform particle size and may comprise high levels of surfactant acid successfully exceeding the maximum surfactant acid content of the prior art.
- a free flowing, high active, anionic powdered or granular detergent composition comprising an anionic surfactant acid adsorped onto a powdered or granular material, said detergent composition having a particle size distribution substantially within the range from 248 microns to 1752 microns.
- a free flowing, high active, anionic, powdered or granular detergent composition comprising a surfactant acid adsorped onto a powdered or granular material the surfactant acid being present in the range from 12 to 40% by weight of the total composition and the powdered or granular material being present within the range from 20 to 50% by weight of the total composition.
- the anionic surfactant acid is adsorbed onto heated, dry, powdered, or granular material. In a preferred embodiment of the invention the anionic surfactant acid is adsorbed onto heated dry powdered or granular form preferably in a fluidised bed.
- the agglomerate so formed is then coated by the application of a silicate and/or alkali, preferably in a fluidised bed.
- a silicate and/or alkali preferably in a fluidised bed.
- the temperature of the inital part of the fluidised bed is preferably above 50°C and more preferably in the range from 85 to 95°C.
- Any suitable anionic surfactant acid may be used. Suitable examples of such are as follows: alkyl aryl sulphonic acids, fatty acid sulphonic acids, olefin sulphonic acids, fatty alcohol ether sulphuric acid, fatty methyl ester sulphonic acid, alkane sulphonic acids. More particularly alkyl aryl sulphonic acids containing an alkyl group with 9-20 carbon atoms and a sulphonic acid or sulphuric acid ester group (included in the term alkyl is the alkyl portion of the aryl groups), or fatty acid sulphuric acids obtained by sulphating alcohols with 8-18 carbon atom chains.
- linear straight chain alkyl benzene sulphonic acids in which the average number of carbon atoms in the alkyl group is from 11 to 13.
- the amount of anionic surfactant acid added is preferably in the range 12% to 40%, more preferably from 12% to 35% and even more preferably from 12% to 30% of the final product weight for weight.
- the powdered or granular material may comprise any suitable alkali, or alkalies, alone, or in combination with other additional ingredients.
- suitable alkalies are as follows: Sodium phosphates, for example sodium tripolyphosphate, sodium carbonate, sodium bicarbonate, sodium silicate or other similar alkalies including potassium or magnesium salts.
- the amount of alkali is preferably in the range 10% to 95% and more preferably 60% to 95% final product weight for weight.
- Additional ingredients may include the following: bleaching agents for example Sodium Perborate, corrosion inhibitors or alkaline additives, for example, Sodium Silicates, inert fillers, for example Sodium Sulphate, surfactants, optical brighteners, preventors of soil redeposition, (for example, sodium carboxy-methyl cellulose,) dedusting agents and solubilisers, such as sodium xylene sulphonate, enzymes, chelating agents, perfumes, softening agents, defoamers, bleach activators, soap, and non ionic active material.
- bleaching agents for example Sodium Perborate, corrosion inhibitors or alkaline additives, for example, Sodium Silicates, inert fillers, for example Sodium Sulphate, surfactants, optical brighteners, preventors of soil redeposition, (for example, sodium carboxy-methyl cellulose,) dedusting agents and solubilisers, such as sodium xylene sulphonate, enzymes, chelating agents, perfumes,
- Any suitable apparatus may be used, but this may have to be adapted to run under the appropriate conditions so as to maintain dry conditions during the agglomeration stage. Examples of such apparatus are as follows:
- Sample powdered or granular detergents derived from this method exhibit the following characteristics: Particle Size no more than 3% by weight of the particles are larger than 1700 microns no more than 1% by weight of the particles are less than 250 microns average particle size 1100 to 1300 microns
- Bulk density untapped 600-720 gm/ml tapped: 730-830 gm/ml moisture content : less than 4% W/W angle of repose average: 37 to 38°C with minimum 36° maximum 41° sliding angle : minimum 25° maximum 28° flowrate : 30-41 cc/sec through standard orifice. compressibility : 7-15%
- composition of anionic detergent granulate
- the detergent composition comprises 5 to 40% preferably 10 to 35% and more preferably 12 to 30% by weight of the final composition of an anionic surfactant acid for example Sodium alkyl aryl sulphate.
- the detergent composition comprises 20 to 50% preferably 25 to 45% and more preferably 30 to 40% by weight of the final composition of the powdered or granular material such as the alkaline material sodium tripolyphoshphate.
- the detergent composition may also comprise any of the optical ingredients listed on page 5 including for example any of the following: soda ash, sodium sulphate, sodium carboxy methyl cellulose, optical bleaches, sequestering agents, sodium silicates etc.
- the angle of repose is defined as the angle from the horizontal to the line of slope of a heap of powder, the heap having been formed by directing powder through a funnel into the centre of a circular horizontal surface. The funnel is slowly raised to allow the heap to form immediately beneath it.
- the flow rate of the powder is defined as the rate in cubic centimetres per second that will flow through a 1.25cm diameter orifice with a smooth PVC funnel expanding at 10° to the vertical above the orifice.
- the angle of slide is defined as the minimum angle between the horizontal and an inclined surface when a powder slides by gravity en masse down that surface, the surface being a smooth, wooden unpolished medium.
- the powder is scattered as a layer no more than 20mm deep on the surface. The surface is raised slowly until the sliding condition is achieved
- the compressibility of the powder is defined as the percentage of initial volume lost when a sample is subjected to a compressive load, the compressive load being provided by a 10Kg weight which is applied to a cylinder of powder of 69mm diameter for a period of 3 minutes.
- LIQUID 1 Do Decyl Benzene Sulphonic Acid (DDBSA) at a spray rate of 390g/min.
- LIQUID 2. A solution comprising % W/W a) Sodium Silicate (2:1 SiO2:Na2O) 40.00 b) Pigment blue 15:1 (46% Dispersion 0.18 c) Tetra sodium salt of ethylene diamine tetra acetic acid 3.66 d) Water 56.16
- the product was a dust free, free flowing granular agglomerate.
- composition of the two liquids sprayed along the fluidised bed was as in EXAMPLE 1.
- LIQUID 1 was applied at a spray rate of 600g/min.
- LIQUID 2 was applied at a spray rate of 390g/min
- alkyl aryl sulphonic and silicate solultion equated to a combined percentage liquid addition of 35.0% W/W.
- the powder produced was a dust free, free flowing granular agglomerate.
- the method enabled a liquid addition of 35.0% W/W to the fluid bed which is comfortably in excess of the limit of 20% imposed by known methods.
- Active matter content was as high as 23.9%, which is almost twice the maximum amount of 12% of active matter achieved by known methods, utilising a fluid bed apparatus.
- the present invention provides a cost efficient method of producing a high active, non-dusty, free flowing, stable anionic detergent powder which may be easily handled and easily stored.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT89307771T ATE97951T1 (de) | 1988-08-05 | 1989-07-31 | Waschmittel. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB8818613 | 1988-08-05 | ||
GB888818613A GB8818613D0 (en) | 1988-08-05 | 1988-08-05 | Detergents |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0353976A1 true EP0353976A1 (de) | 1990-02-07 |
EP0353976B1 EP0353976B1 (de) | 1993-12-01 |
Family
ID=10641648
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP89307771A Revoked EP0353976B1 (de) | 1988-08-05 | 1989-07-31 | Waschmittel |
EP89909029A Pending EP0404865A1 (de) | 1988-08-05 | 1989-07-31 | Waschmittel |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP89909029A Pending EP0404865A1 (de) | 1988-08-05 | 1989-07-31 | Waschmittel |
Country Status (14)
Country | Link |
---|---|
EP (2) | EP0353976B1 (de) |
KR (1) | KR920009044B1 (de) |
AT (1) | ATE97951T1 (de) |
CA (1) | CA1323278C (de) |
DE (1) | DE68911053T2 (de) |
ES (1) | ES2047677T3 (de) |
GB (1) | GB8818613D0 (de) |
HK (1) | HK48495A (de) |
IE (1) | IE63797B1 (de) |
IN (1) | IN176172B (de) |
MY (1) | MY105001A (de) |
NZ (1) | NZ230218A (de) |
PT (1) | PT91386A (de) |
WO (1) | WO1990001536A1 (de) |
Cited By (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1994007990A1 (de) * | 1992-09-30 | 1994-04-14 | Henkel Kommanditgesellschaft Auf Aktien | Verfahren zur herstellung von tensidgranulaten |
DE4415369C1 (de) * | 1994-05-02 | 1995-08-31 | Henkel Kgaa | Heterogene Tensidgranulate |
EP0688861A1 (de) * | 1994-06-22 | 1995-12-27 | SOCIETE FRANCAISE HOECHST Société anonyme dite: | Verfahren zur Herstellung von anionische Tenside enthaltenden Zusammensetzungen in Form von Pulvern, Perlen oder Granulaten und Verwendung dieser Zusammensetzungen in Reinigungs- und Pflegeprodukten |
WO1996004359A1 (en) * | 1994-08-05 | 1996-02-15 | Unilever Plc | Granulation in a fluidised bed |
WO1997032005A1 (en) * | 1996-02-26 | 1997-09-04 | Unilever Plc | Anionic detergent particles |
WO1998058046A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
WO1999000475A1 (en) * | 1997-06-27 | 1999-01-07 | Unilever Plc | Production of detergent granulates |
US6077820A (en) * | 1995-12-20 | 2000-06-20 | Lever Brothers Company Division Of Conopco, Inc. | Process for preparing a granular detergent |
WO2000037604A1 (en) * | 1998-12-22 | 2000-06-29 | The Procter & Gamble Company | Process for preparing a granular detergent composition |
WO2000053719A1 (en) * | 1999-03-09 | 2000-09-14 | The Procter & Gamble Company | Detergent particles having coating or partial coating layers |
US6207635B1 (en) * | 1995-05-31 | 2001-03-27 | The Procter & Gamble Company | Process for manufacture of high density detergent granules |
US6274544B1 (en) | 1997-06-16 | 2001-08-14 | Lever Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
US6596683B1 (en) | 1998-12-22 | 2003-07-22 | The Procter & Gamble Company | Process for preparing a granular detergent composition |
US6740632B1 (en) * | 2000-02-18 | 2004-05-25 | Glatt Ingenieurtechnik Gmbh | Process for manufacturing industrial detergent and components thereof |
US6858572B1 (en) | 1999-03-09 | 2005-02-22 | The Procter & Gamble Company | Process for producing coated detergent particles |
US6894018B1 (en) | 1999-06-21 | 2005-05-17 | The Procter & Gamble Company | Process for making granular detergent in a fluidized bed granulator having recycling of improperly sized particles |
US6992055B1 (en) * | 1996-09-06 | 2006-01-31 | Kao Corporation | Process for preparing detergent compositions having high bulk density |
US7022660B1 (en) | 1999-03-09 | 2006-04-04 | The Procter & Gamble Company | Process for preparing detergent particles having coating or partial coating layers |
US7098177B1 (en) * | 1998-10-16 | 2006-08-29 | Kao Corporation | Process for producing detergent particles |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB9001285D0 (en) * | 1990-01-19 | 1990-03-21 | Unilever Plc | Detergent compositions and process for preparing them |
DE4216629A1 (de) * | 1992-05-20 | 1993-11-25 | Henkel Kgaa | Verfahren zur Herstellung aniontensidhaltiger Wasch- und Reinigungsmittel |
US5573697A (en) * | 1995-05-31 | 1996-11-12 | Riddick; Eric F. | Process for making high active, high density detergent granules |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2671797A (en) * | 1951-02-15 | 1954-03-09 | Ruhrchemie Ag | Neutralization of sulfonic acids and sulfuric acid esters |
GB707994A (en) * | 1950-02-13 | 1954-04-28 | Ruhrchemie Ag | Process for the neutralization of sulphonic acids |
GB1369269A (en) * | 1971-02-01 | 1974-10-02 | Colgate Palmolive Co | Method for neutrlization of detergent acid |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA807615A (en) * | 1966-09-30 | 1969-03-04 | W. Poe Russell | Detergent process |
BE750648A (fr) * | 1969-05-21 | 1970-11-20 | Stauffer Chemical Co | Procede de preparation de compositions detergentes |
GB1404317A (en) * | 1971-10-23 | 1975-08-28 | Bell Chemicals Pty Ltd | Manufacture of detergent powders |
DD140987B1 (de) * | 1979-01-05 | 1982-06-30 | Manfred Mittelstrass | Kontinuierliches herstellungsverfahren granulierter wasch-und reinigungsmittel in wirbelschichtapparaten |
DD228458A1 (de) * | 1983-12-21 | 1985-10-16 | Genthin Waschmittelwerk | Verfahren zur kontinuierlichen bestaeubung von waschmittelgranulatprodukten |
GB2166542B (en) * | 1984-11-02 | 1988-10-12 | British Aerospace | Air conditioning systems |
GB2209172A (en) * | 1987-08-28 | 1989-05-04 | Unilever Plc | Preparation of solid particulate components for detergents |
IN170991B (de) * | 1988-07-21 | 1992-06-27 | Lever Hindustan Ltd |
-
1988
- 1988-08-05 GB GB888818613A patent/GB8818613D0/en active Pending
-
1989
- 1989-07-28 MY MYPI89001029A patent/MY105001A/en unknown
- 1989-07-31 IN IN675DE1989 patent/IN176172B/en unknown
- 1989-07-31 WO PCT/GB1989/000873 patent/WO1990001536A1/en not_active Application Discontinuation
- 1989-07-31 CA CA000607122A patent/CA1323278C/en not_active Expired - Fee Related
- 1989-07-31 EP EP89307771A patent/EP0353976B1/de not_active Revoked
- 1989-07-31 KR KR1019900700616A patent/KR920009044B1/ko not_active IP Right Cessation
- 1989-07-31 ES ES89307771T patent/ES2047677T3/es not_active Expired - Lifetime
- 1989-07-31 DE DE89307771T patent/DE68911053T2/de not_active Revoked
- 1989-07-31 AT AT89307771T patent/ATE97951T1/de not_active IP Right Cessation
- 1989-07-31 EP EP89909029A patent/EP0404865A1/de active Pending
- 1989-08-04 NZ NZ230218A patent/NZ230218A/xx unknown
- 1989-08-04 IE IE253089A patent/IE63797B1/en not_active IP Right Cessation
- 1989-08-04 PT PT91386A patent/PT91386A/pt not_active Application Discontinuation
-
1995
- 1995-03-30 HK HK48495A patent/HK48495A/xx unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB707994A (en) * | 1950-02-13 | 1954-04-28 | Ruhrchemie Ag | Process for the neutralization of sulphonic acids |
US2671797A (en) * | 1951-02-15 | 1954-03-09 | Ruhrchemie Ag | Neutralization of sulfonic acids and sulfuric acid esters |
GB1369269A (en) * | 1971-02-01 | 1974-10-02 | Colgate Palmolive Co | Method for neutrlization of detergent acid |
Non-Patent Citations (1)
Title |
---|
A.S. DAVIDSOHN et al.: "SYNTHETIC DETERGENTS" * |
Cited By (26)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1994007990A1 (de) * | 1992-09-30 | 1994-04-14 | Henkel Kommanditgesellschaft Auf Aktien | Verfahren zur herstellung von tensidgranulaten |
US5824633A (en) * | 1994-05-02 | 1998-10-20 | Henkel Kommanditgesellschaft Auf Aktien | Heterogeneous surfactant granules |
DE4415369C1 (de) * | 1994-05-02 | 1995-08-31 | Henkel Kgaa | Heterogene Tensidgranulate |
EP0688861A1 (de) * | 1994-06-22 | 1995-12-27 | SOCIETE FRANCAISE HOECHST Société anonyme dite: | Verfahren zur Herstellung von anionische Tenside enthaltenden Zusammensetzungen in Form von Pulvern, Perlen oder Granulaten und Verwendung dieser Zusammensetzungen in Reinigungs- und Pflegeprodukten |
FR2721616A1 (fr) * | 1994-06-22 | 1995-12-29 | Hoechst France | Compositions de tensioactifs anioniques en poudre, en perles ou en granulés, leur procédé de préparation et leur utilisation dans les produits de nettoyage et d'entretien. |
WO1996004359A1 (en) * | 1994-08-05 | 1996-02-15 | Unilever Plc | Granulation in a fluidised bed |
CN1115403C (zh) * | 1994-08-05 | 2003-07-23 | 尤尼利弗公司 | 流化床造粒 |
AU702808B2 (en) * | 1994-08-05 | 1999-03-04 | Unilever Plc | Granulation in a fluidised bed |
US6207635B1 (en) * | 1995-05-31 | 2001-03-27 | The Procter & Gamble Company | Process for manufacture of high density detergent granules |
US6077820A (en) * | 1995-12-20 | 2000-06-20 | Lever Brothers Company Division Of Conopco, Inc. | Process for preparing a granular detergent |
WO1997032005A1 (en) * | 1996-02-26 | 1997-09-04 | Unilever Plc | Anionic detergent particles |
US6992055B1 (en) * | 1996-09-06 | 2006-01-31 | Kao Corporation | Process for preparing detergent compositions having high bulk density |
WO1998058046A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
US6056905A (en) * | 1997-06-16 | 2000-05-02 | Lever Brothers Company Division Of Conopco, Inc. | Production of detergent granulates |
US6274544B1 (en) | 1997-06-16 | 2001-08-14 | Lever Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
US6429184B1 (en) | 1997-06-16 | 2002-08-06 | Lever & Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
WO1999000475A1 (en) * | 1997-06-27 | 1999-01-07 | Unilever Plc | Production of detergent granulates |
US6133223A (en) * | 1997-06-27 | 2000-10-17 | Lever Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
US7098177B1 (en) * | 1998-10-16 | 2006-08-29 | Kao Corporation | Process for producing detergent particles |
WO2000037604A1 (en) * | 1998-12-22 | 2000-06-29 | The Procter & Gamble Company | Process for preparing a granular detergent composition |
US6596683B1 (en) | 1998-12-22 | 2003-07-22 | The Procter & Gamble Company | Process for preparing a granular detergent composition |
US6858572B1 (en) | 1999-03-09 | 2005-02-22 | The Procter & Gamble Company | Process for producing coated detergent particles |
US7022660B1 (en) | 1999-03-09 | 2006-04-04 | The Procter & Gamble Company | Process for preparing detergent particles having coating or partial coating layers |
WO2000053719A1 (en) * | 1999-03-09 | 2000-09-14 | The Procter & Gamble Company | Detergent particles having coating or partial coating layers |
US6894018B1 (en) | 1999-06-21 | 2005-05-17 | The Procter & Gamble Company | Process for making granular detergent in a fluidized bed granulator having recycling of improperly sized particles |
US6740632B1 (en) * | 2000-02-18 | 2004-05-25 | Glatt Ingenieurtechnik Gmbh | Process for manufacturing industrial detergent and components thereof |
Also Published As
Publication number | Publication date |
---|---|
AU4049289A (en) | 1990-03-05 |
NZ230218A (en) | 1991-11-26 |
IE892530L (en) | 1990-02-05 |
DE68911053T2 (de) | 1994-03-31 |
GB8818613D0 (en) | 1988-09-07 |
CA1323278C (en) | 1993-10-19 |
AU622925B2 (en) | 1992-04-30 |
WO1990001536A1 (en) | 1990-02-22 |
EP0353976B1 (de) | 1993-12-01 |
KR900701997A (ko) | 1990-12-05 |
ES2047677T3 (es) | 1994-03-01 |
HK48495A (en) | 1995-04-07 |
IN176172B (de) | 1996-02-17 |
MY105001A (en) | 1994-07-30 |
KR920009044B1 (ko) | 1992-10-13 |
PT91386A (pt) | 1990-03-08 |
IE63797B1 (en) | 1995-06-14 |
DE68911053D1 (de) | 1994-01-13 |
EP0404865A1 (de) | 1991-01-02 |
ATE97951T1 (de) | 1993-12-15 |
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Legal Events
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PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
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AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): ES GR |
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17P | Request for examination filed |
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