EP1070115B1 - Composition granulaire coloree, a utiliser dans des compositions de detergents particulaires - Google Patents
Composition granulaire coloree, a utiliser dans des compositions de detergents particulaires Download PDFInfo
- Publication number
- EP1070115B1 EP1070115B1 EP99944131A EP99944131A EP1070115B1 EP 1070115 B1 EP1070115 B1 EP 1070115B1 EP 99944131 A EP99944131 A EP 99944131A EP 99944131 A EP99944131 A EP 99944131A EP 1070115 B1 EP1070115 B1 EP 1070115B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- water
- granular composition
- coloured
- flow modifier
- weight
- 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
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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/40—Dyes ; Pigments
- C11D3/42—Brightening agents ; Blueing agents
-
- 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
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0063—Photo- activating compounds
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2082—Polycarboxylic acids-salts thereof
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3769—(Co)polymerised monomers containing nitrogen, e.g. carbonamides, nitriles or amines
- C11D3/3776—Heterocyclic compounds, e.g. lactam
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/40—Dyes ; Pigments
Definitions
- the present invention relates to a fast-dissolving, low-staining granular composition containing a visually distinct, eg coloured or fluorescent, ingredient, for example, a photobleach.
- the invention more particularly relates to granules containing a coloured or fluorescent ingredient which may be incorporated into a detergent composition without encountering the problem of staining of the fabric during the wash.
- Coloured speckles are used in detergent formulations to give a distinct appearance to the product as well as to deliver functional benefits. In the wash process, it is undesirable that these coloured speckles settle onto the fabric surface leading to staining of the fabric. It has also been noticed that these stains do not get washed out in subsequent laundering. Further the uneven concentration of these speckles on the substrate could result in localised higher levels of the active causing fabric damage.
- US 4 097 418 discloses a granular coloured speckle having non-staining qualities comprising an agglomerate of a granular water soluble inorganic alkaline salt with an anionic surfactant which contains a dye or pigment. Mixing of the dye and the anionic surfactant prior to agglomeration prevents the pigment particles from attaching to each other and onto the fabric surface thus preventing staining of the fabric.
- US 4 762 636 (Ciba-Geigy, 1988 ) discloses a process for obtaining granules with defined physical properties that float on an aqueous treatment liquor and release the active ingredient without getting deposited onto the substrate.
- the present invention provides a granular composition suitable for incorporation into a particulate detergent composition, the granular composition comprising
- the water-soluble or water-dispersible barrier material serves to provide a protective layer or coating on the combination of the coloured or fluorescent ingredient and its carrier material, the citric acid. Preferably at least a part of the inorganic flow modifier is also thus protected. Additional inorganic flow modifier that is not protected by the barrier material may also be present.
- the granule composition comprises:
- the granular composition of the invention may be prepared by a process in which the coloured or fluorescent ingredient is dispersed onto the citric acid, which is then mixed with part or all of the inorganic flow modifier and the whole treated with the barrier material, then granulated with any remaining inorganic flow modifier.
- coloured or fluorescent ingredients are photoactivators (also known as photobleaches), especially phthalocyanines; coloured dyes and pigments; fluorescent whitening agents; and mixtures thereof.
- photoactivators also known as photobleaches
- phthalocyanines especially phthalocyanines
- coloured dyes and pigments especially coloured dyes and pigments
- fluorescent whitening agents especially preferred ingredients are the photobleaches, zinc and aluminium phthalocyanine sulphonates.
- the inorganic flow modifier can be selected from china clay, (preferably washed china clay), silica, precipitated silica, precipitated calcium carbonate and diatomaceous/siliceous earth. China clay, silica and mixtures thereof are especially preferred.
- the water-soluble or water-dispersible, preferably water-soluble, barrier material may suitably be selected from water-soluble starches, polyvinyl alcohols, polyethylene glycols and latex. Preferred materials are starches and polyvinyl alcohols.
- the granules of the present invention may be prepared by dispersing the coloured or fluorescent ingredient on the citric acid, for example, in a rotary pan granulator, and subsequently or simultaneously adding a suitable flow modifier.
- the resultant agglomerate is dried and further coated with the water-soluble or water-dispersible barrier material, and optionally granulated with further flow modifier and dried.
- a further subject of the invention is a particulate detergent composition comprising organic detergent surfactants and other detergent ingredients, and comprising a granular composition as defined previously.
- the particulate laundry detergent composition of the invention may suitably comprise from 5 to 60 wt% of organic surfactant, from 10 to 80 wt% of detergency builder, from 0.1 to 10 wt%, preferably from 0.5 to 5 wt%, of a granular composition as defined previously, and optionally other detergent ingredients to 100 wt%.
- Example 1 photobleach granules using citric acid carrier and starch barrier material
- the formulation of the granular material was as follows: Starting material (g) Final formulation (wt%) Aluminium phthalocyanine sulphonate 20 2 Citric acid 8000 80 China clay 800 8 Silica 500 5 Starch 50 0.5 Water to 100% 630 4.5
- Example 2 photobleach granules using citric acid carrier and polyvinyl alcohol barrier material
- Photobleach granules were prepared as in Example 1 but the starch solution was replaced by polyvinyl alcohol solution (concentration 10% by weight).
- the final formulation of the granular material was as follows: Starting material (g) Final formulation (wt%) Aluminium phthalocyanine sulphonate 20 2 Citric acid 8000 80 China clay 800 8 Silica 500 5 Polyvinyl alcohol 50 0.5 Water to 100% 630 4.5
- Granules were prepared by the process of Example 1 but using soda ash instead of citric acid.
- Granules were prepared by the process of Example 1 but using sodium tripolyphosphate instead of citric acid.
- Cotton fabric pieces of dimension 10 inch x 10 inch (25.4 cm x 25.4 cm) were placed in trays, each together with 2 kg of water and one of the following photobleach granular compositions:
- Comparative Example C commercially available blue speckles, Laundrosil (Trade Mark) PRT-2 ex Sud-Chemie, containing aluminium phthalocyanine sulphonate on a bentonite clay carrier.
- Granular detergent compositions were prepared by dry mixing to the following formulations: Linear alkylbenzene sulphonate 30 Sodium carbonate 20 Sodium tripolyphosphate 40 Photobleach granules (see below) 2 Enzymes, perfume, fluorescer, water etc to 100
- the detergent composition of Example 3 contained the photobleach granules of Example 1 (citric acid carrier, starch barrier material).
- the detergent composition of Example 4 contained the photobleach granules of Example 2 (citric acid carrier, polyvinyl alcohol barrier material).
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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)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Molecular Biology (AREA)
- Detergent Compositions (AREA)
Abstract
Claims (12)
- Composition granulaire incorporable dans une composition détergente particulaire, la composition granulaire comprenant(a) un ingrédient coloré ou fluorescent(b) un matériau support pour l'ingrédient coloré ou fluorescent,
caractérisée en ce que le matériau support (b) est de l'acide citrique et que la composition granulaire comprend en outre(c) un matériau-barrière hydrosoluble ou hydrodispersible et,(d) un modificateur d'écoulement inorganique. - Composition granulaire selon la revendication 1, caractérisée en ce que:- l'ingrédient coloré ou fluorescent (a) est dispersé sur, ou sous la forme d'un revêtement sur l'acide citrique (b), celui-ci étant en mélange avec le modificateur d'écoulement inorganique (d) ou une partie de celui-ci, et- le matériau-barrière (c) est sous la forme d'un revêtement sur le mélange d'acide citrique enduit et du modificateur d'écoulement inorganique, le mélange enduit étant en mélange avec tout modificateur d'écoulement inorganique (d) résiduel.
- Composition granulaire selon l'une quelconque des revendications précédentes, caractérisée en ce qu'elle comprend:(a) de 0,5 à 5 % en poids, de préférence de 1 à 2 % en poids, de l'ingrédient coloré ou fluorescent,(b) de 40 à 90 % en poids, de préférence de 60 à 80 % en poids d'acide citrique,(c) de 0,5 à 5 % en poids, de préférence de 1 à 3 % en poids du matériau barrière hydrosoluble ou hydrodispersible,(d) de 10 à 50 % en poids, de préférence de 18 à 40 % en poids du modificateur d'écoulement inorganique.
- Composition granulaire selon l'une quelconque des revendications précédentes, caractérisée en ce que l'ingrédient coloré ou fluorescent (a) est choisi parmi les photo-activateurs (photo-blanchisseurs), les pigments, les colorants et les agents blanchisseurs fluorescents.
- Composition granulaire selon la revendication 4, caractérisée en ce que l'ingrédient coloré ou fluorescent (a) est un sulfonate de phtalocyanine de zinc ou d'aluminium.
- Composition granulaire selon l'une quelconque des revendications précédentes, caractérisée en ce que le matériau barrière hydrosoluble ou hydrodispersible (c) est choisi parmi les amidons hydrosolubles, les alcools polyvinyliques hydrosolubles, les glycols de polyéthylène hydrosolubles et les micelles hydrosolubles.
- Composition granulaire selon la revendication 6, caractérisée en ce que le matériau-barrière (c) est hydrosoluble et est un amidon ou un alcool polyvinylique.
- Composition granulaire selon l'une quelconque des revendications précédentes, caractérisée en ce que le modificateur d'écoulement inorganique (d) est choisi parmi l'argile chinoise, la silice, la silice précipitée, le carbonate de calcium précipité et la terre diatomée ou siliceuse.
- Composition granulaire selon la revendication 8, caractérisée en ce que le modificateur d'écoulement inorganique (d) comprend de l'argile chinoise, de la silice, ou un mélange de celles-ci.
- Composition détergente blanchisseuse particulaire qui comprend de 5 à 60 % en poids de tensioactif organique, de 10 à 80 % en poids d'agent détergent, et éventuellement d'autres ingrédients détergents jusqu'à 100 % en poids, caractérisée en ce qu'elle comprend de 0,1 à 10 % en poids, de préférence de 0,5 à 5 % en poids, d'une composition granulaire selon l'une quelconque des revendications 1 à 11.
- Procédé de préparation d'une composition granulaire selon la revendication 1, caractérisé en ce qu'il comprend les étapes consistant à :(i) disperser l'ingrédient coloré ou fluorescent (a) sur l'acide citrique (b), et le granuler avec tout ou partie du modificateur d'écoulement inorganique (d),(ii) sécher le matériau granulaire ainsi obtenu,(iii) traiter le matériau séché avec le matériau-barrière hydrosoluble ou hydrodispersible (c),(iv) éventuellement, granuler le matériau traité ainsi obtenu avec tout modificateur d'écoulement inorganique (d) résiduel éventuel, et à procéder au séchage.
- Procédé selon la revendication 11, caractérisé en ce que l'étape de séchage (iii) est réalisée à une température située dans la plage allant de 15 à 50°C, de préférence de 20 à 40°C.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GBGB9807477.6A GB9807477D0 (en) | 1998-04-07 | 1998-04-07 | Coloured granular composition for use in particulate detergent compositions |
GB9807477 | 1998-04-07 | ||
PCT/EP1999/000493 WO1999051714A2 (fr) | 1998-04-07 | 1999-01-26 | Composition granulaire coloree, a utiliser dans des compositions de detergents particulaires |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1070115A2 EP1070115A2 (fr) | 2001-01-24 |
EP1070115B1 true EP1070115B1 (fr) | 2008-03-12 |
Family
ID=10830010
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP99944131A Expired - Lifetime EP1070115B1 (fr) | 1998-04-07 | 1999-01-26 | Composition granulaire coloree, a utiliser dans des compositions de detergents particulaires |
Country Status (12)
Country | Link |
---|---|
EP (1) | EP1070115B1 (fr) |
CN (1) | CN1137983C (fr) |
AU (1) | AU5265299A (fr) |
BR (1) | BR9909469A (fr) |
DE (1) | DE69938341T2 (fr) |
EA (1) | EA200001026A1 (fr) |
ES (1) | ES2301245T3 (fr) |
GB (1) | GB9807477D0 (fr) |
ID (1) | ID26094A (fr) |
TR (1) | TR200002800T2 (fr) |
WO (1) | WO1999051714A2 (fr) |
ZA (1) | ZA99839B (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8021436B2 (en) | 2007-09-27 | 2011-09-20 | The Procter & Gamble Company | Cleaning and/or treatment compositions comprising a xyloglucan conjugate |
Families Citing this family (67)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2343456A (en) * | 1998-11-06 | 2000-05-10 | Procter & Gamble | Speckle particles and compositions containing the speckle particles |
WO2000058431A1 (fr) * | 1999-03-29 | 2000-10-05 | Ciba Specialty Chemicals Holding Inc. | Utilisation d'un pigment eclaircissant dans des nettoyants ou des detergents |
GB0110414D0 (en) * | 2001-04-27 | 2001-06-20 | Unilever Plc | Radical initiator composition |
ATE319807T1 (de) | 2001-08-20 | 2006-03-15 | Unilever Nv | Photobleichsprenkel und sie enthaltende waschmittel |
GB0120160D0 (en) | 2001-08-20 | 2001-10-10 | Unilever Plc | Photobleach speckle and laundry detergent compositions containing it |
GB0228354D0 (en) | 2002-12-05 | 2003-01-08 | Unilever Plc | Detergent compositions |
GB0202017D0 (en) | 2002-01-29 | 2002-03-13 | Unilever Plc | Detergent compositions |
BR0306995A (pt) | 2002-01-29 | 2004-12-14 | Unilever Nv | Composição detergente |
EP1976967A2 (fr) | 2006-01-23 | 2008-10-08 | The Procter and Gamble Company | Compositions détergentes |
EP2287281A1 (fr) | 2006-01-23 | 2011-02-23 | The Procter & Gamble Company | Composition comprenant une lipase et un agent de nuançage |
MX2008013357A (es) * | 2006-04-20 | 2008-10-31 | Procter & Gamble | Una composicion detergente para lavanderia particulada solida que comprende particulas de perfume. |
US7629158B2 (en) | 2006-06-16 | 2009-12-08 | The Procter & Gamble Company | Cleaning and/or treatment compositions |
EP2071017A1 (fr) | 2007-12-04 | 2009-06-17 | The Procter and Gamble Company | Composition de détergent |
RU2470070C2 (ru) | 2008-01-04 | 2012-12-20 | Дзе Проктер Энд Гэмбл Компани | Композиции, содержащие фермент и подкрашивающий агент для тканей |
AU2010209328B2 (en) * | 2009-01-30 | 2015-07-02 | Ecolab Inc. | Development of an aluminum hydroxycarboxylate builder |
EP4159833A3 (fr) | 2009-12-09 | 2023-07-26 | The Procter & Gamble Company | Tissu et produits de soins à domicile |
EP3418382B1 (fr) | 2010-05-06 | 2021-01-20 | Danisco US Inc. | Compositions et procédés comprenant des variants de subtilisine |
WO2012142087A1 (fr) | 2011-04-12 | 2012-10-18 | The Procter & Gamble Company | Catalyseurs de blanchiment métalliques |
US20140371435A9 (en) | 2011-06-03 | 2014-12-18 | Eduardo Torres | Laundry Care Compositions Containing Thiophene Azo Dyes |
EP2537918A1 (fr) | 2011-06-20 | 2012-12-26 | The Procter & Gamble Company | Produits de consommation avec particules enrobées comprenant une lipase |
IN2014DN06191A (fr) | 2012-02-03 | 2015-10-23 | Procter & Gamble | |
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WO2015042087A1 (fr) | 2013-09-18 | 2015-03-26 | The Procter & Gamble Company | Composition d'entretien du linge comprenant un colorant carboxylate |
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US20200157476A1 (en) | 2018-11-16 | 2020-05-21 | The Procter & Gamble Company | Composition and method for removing stains from fabrics |
EP3994255A1 (fr) | 2019-07-02 | 2022-05-11 | Novozymes A/S | Variants de lipase et compositions de ceux-ci |
WO2022090361A2 (fr) | 2020-10-29 | 2022-05-05 | Novozymes A/S | Variants de lipase et compositions comprenant de tels variants de lipase |
EP4386035A1 (fr) | 2021-08-10 | 2024-06-19 | Nippon Shokubai Co., Ltd. | Composé à teneur en oxyde de polyalkylène |
WO2023247664A2 (fr) | 2022-06-24 | 2023-12-28 | Novozymes A/S | Variants de lipase et compositions comprenant de tels variants de lipase |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1378923A (en) * | 1971-01-25 | 1974-12-27 | Colgate Palmolive Co | Coloured particles and cleanser composition containing same |
US4762636A (en) * | 1986-02-28 | 1988-08-09 | Ciba-Geigy Corporation | Process for the preparation of granules containing an active substance and to the use thereof as speckles for treating substrates |
AU715795B2 (en) * | 1996-03-15 | 2000-02-10 | Access Business Group International Llc | Free flowing agglomerated nonionic surfactant detergent composition and process for making same |
WO1998016615A1 (fr) * | 1996-10-15 | 1998-04-23 | The Procter & Gamble Company | Compositions particulaires colorees |
-
1998
- 1998-04-07 GB GBGB9807477.6A patent/GB9807477D0/en not_active Ceased
-
1999
- 1999-01-26 DE DE69938341T patent/DE69938341T2/de not_active Expired - Lifetime
- 1999-01-26 WO PCT/EP1999/000493 patent/WO1999051714A2/fr active IP Right Grant
- 1999-01-26 CN CNB998047961A patent/CN1137983C/zh not_active Expired - Fee Related
- 1999-01-26 EA EA200001026A patent/EA200001026A1/ru unknown
- 1999-01-26 EP EP99944131A patent/EP1070115B1/fr not_active Expired - Lifetime
- 1999-01-26 ES ES99944131T patent/ES2301245T3/es not_active Expired - Lifetime
- 1999-01-26 AU AU52652/99A patent/AU5265299A/en not_active Abandoned
- 1999-01-26 ID IDW20002012A patent/ID26094A/id unknown
- 1999-01-26 BR BR9909469-0A patent/BR9909469A/pt not_active Application Discontinuation
- 1999-01-26 TR TR2000/02800T patent/TR200002800T2/xx unknown
- 1999-02-03 ZA ZA9900839A patent/ZA99839B/xx unknown
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8021436B2 (en) | 2007-09-27 | 2011-09-20 | The Procter & Gamble Company | Cleaning and/or treatment compositions comprising a xyloglucan conjugate |
Also Published As
Publication number | Publication date |
---|---|
WO1999051714A3 (fr) | 1999-11-18 |
WO1999051714A8 (fr) | 1999-12-29 |
WO1999051714A2 (fr) | 1999-10-14 |
DE69938341T2 (de) | 2009-04-30 |
AU5265299A (en) | 1999-10-25 |
ID26094A (id) | 2000-11-23 |
ES2301245T3 (es) | 2008-06-16 |
CN1137983C (zh) | 2004-02-11 |
CN1296523A (zh) | 2001-05-23 |
EA200001026A1 (ru) | 2001-04-23 |
DE69938341D1 (de) | 2008-04-24 |
EP1070115A2 (fr) | 2001-01-24 |
ZA99839B (en) | 2000-08-03 |
TR200002800T2 (tr) | 2000-12-21 |
GB9807477D0 (en) | 1998-06-10 |
BR9909469A (pt) | 2002-05-07 |
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