CA2158714A1 - Process for decreasing the build up of inorganic incrustations on textiles and detergent compositions used in such process - Google Patents
Process for decreasing the build up of inorganic incrustations on textiles and detergent compositions used in such processInfo
- Publication number
- CA2158714A1 CA2158714A1 CA002158714A CA2158714A CA2158714A1 CA 2158714 A1 CA2158714 A1 CA 2158714A1 CA 002158714 A CA002158714 A CA 002158714A CA 2158714 A CA2158714 A CA 2158714A CA 2158714 A1 CA2158714 A1 CA 2158714A1
- Authority
- CA
- Canada
- Prior art keywords
- detergent
- builder
- carbohydrate
- build
- washing
- 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.)
- Abandoned
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
- C11D3/16—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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/40—Products in which the composition is not well defined
- C11D7/44—Vegetable products
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Molecular Biology (AREA)
- Emergency Medicine (AREA)
- Detergent Compositions (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
A process for decreasing the build-up of inorganic incrustations on textiles deriving from water hardness and due to repeated washing cycles with detergent compositions comprises the addition to the washing batch of a carbohydrate or carbohydrate derivative having a DE of 0.5 to 20 inclusive as co-builder.
Description
~ ~ 5 8 7 1 ~
Process for decreasing the build up of inorganic incrustations on textiles and detergent composition used in such process The present invention relates to a process for decreasing the build-up of inorganic incrustations on fabrics caused by water hardness and repeated washing cycles with detergent compositlons.
More particularly, the present invention relates to a process for decreasing the build-up of inorganic incrustations wherein a co-builder is added to the washing cycle, and to detergent and/or anti-incrustation compositions containing said co-builder.
It is well known that detergents contain builders in order to support detergent action and to elimin~te calcium and m~gn~.sium ions (hardness ions), which arise partly from the water and sometimes also from soil and fabrics.
In case of multiple washing cycles the washing performance is significantly reduced because of the build up of inorganic incrustations on fabrics and on washing machine components. Such build up of inorganic incrustations on fabrics decreases the flexibility of fibres and consequently shortens the fabric life, in addition to greying the tissue.
A well known builder is sodium tripolyphosphate which has excellent plopellies in the washing process even at low concentrations. Despite its many advantageous properties however, it causes serious ecological problems, namely~eutrophication of stationary or slowly flowing surface waters leading to extreme algal growth which adversely influences marine org~ni~m.~. As a result, the use of phosphate free detergents is of great importance.
Some substitutes of phosphate builders such as zeolites have been adopted. However, zeolites alone in water softening have poor efficiency. Therefore, good anti-incrustation effects are achieved only in the presence of auxiliary compounds called co-builders.
The most widely used co-builders are synthetic polymers and/or co-polymers of olefinic mono- or dicarboxylic acids such as acrylic and maleic acid and copolymers of said 215~71~
monomers with other allylic or vinylic monomers. A common characteristic of these polymeric materials is their minim~31 biodegradability which leads to ecological problems.
There are known other non-polymeric co-builders, such as EDTA
(ethylenediaminetetraacetic acid sodium salt), NTA (nitrilotriacetic acid sodium salt) and phosphonates. As with the polymeric co-builders these substances too are non-biodegradable.
It is therefore an object of the present invention to provide a process for decreasing the build-up of inorganic incrustations on fabrics and on washing machine components by using co-builders which are very efficient in reducing incrustation build up during washing cycles and which are cheap and biodegradable.
Another object of the present invention is to provide detergent and/or anti-incrustation compositions containing said biodegrable co-builders.
It has now surprisingly been found that certain carbohydrates show a high efficiency in reducing incrustation build up when combined with detergents, particularly with zeolite-based detergents.
In European patent application 0 618 286 there is described a co-builder based upon a non-reducing carbohydrate or a non-reducing carbohydrate derivative. Preferred among the non-reducing carbohydrate derivatives are certain sugar alcohols exemplified by maltitol and, especially, by m~nnitoL It has now been found however-that the carbohydrate or carbohydrate derivative need not be fully non-reducing but that some reducing activity is tolerable and that certain compounds showing such activity are as effective co-builders as the sugar alcohols referred to above.
In accordance with one aspect of the present invention therefore there is provided a process for decreasing the build-up of inorganic incrustations on fabrics and on washing machine components during multiple washing cycles with detergent compositions characterized by the addition to the washing cycle of a co-builder based on a carbohydrate or carbohydrate derivative having a DE of 0.5 to 20 inclusive.
21~8714 A range of carbohydrates or carbohydrate derivatives having a DE of 0.5 to 20 inclusive may be used in the process of the invention eg. polydextrose or partially degraded inulin but preferably the carbohydrate or carbohydrate derivative is a maltodextrin having a DE of 0.5 to 20 inclusive, particularly a DE of ~ to 17 inclusive.
"DE" or dextrose equivalent is a measure of the reducing activity of a carbohydrate measured by comparison with dextrose which has a DE of 100.
The co-builders based on such carbohydrates and carbohydrate derivatives having a DE
of 0.5 to 20 inclusive can be incorporated into the detergent compositions or added as such directly to the washing bath.
In accordance with another aspect of the present invention, there are provided detergent and/or anti-incrustation compositions containing the hereinbefore defined co-builders. These compositions may also contain other conventional components such as anionic, non-ionic, cationic or amphoteric surfactants, aL~ali metal salts (e.g. sodium carbonate, sodium silicate), neutral salts (e.g. sodium sulphate), zeolites, bleaching agents, bleaching activators and other minor ingredients.
In accordance with one preferred embodiment of the present invention the novel co-builders are used in combination with zeolite-based detergents.
The co-builders used according to the present in~ention are particularly efficacious in the presence of inorganic persalts, such as sodium perborate tetrahydrate or monohydrate.
The amount of the co-builders used in the process can vary from 1 g/washing cycle to 40 g/washing cycle, and preferably from 2 g/washing cycle to 20 g/washing cycle. This amount is achieved by a range of from 0.5 ~ to 20 ~ and preferably by a range of from 1 ~ to 10 %, expressed as 100 % dry substance of co-builder in the detergent or anti-incrustation compositions.
The co-builders used according to the present invention are naturally derived, _ 4 _ 7 1 4 biodegradable compounds. In combination with detergents they reduce the build up of inorganic incrustations on fabrics and on washing machine components. Such activity is more significant at high temperatures e.g. at 90C.
The present invention is disclosed in still further detail in the following Example, which is supplied for purely illustrative and not limiting purposes.
Example The co-builder activities of the following compositions were evaluated on a laboratory scale using the so-called "Harnpshire" test which measures the Ca~ sequestering capacity of the composition. The test was carried out as follows :-1 gram of the substance under test is dissolved in 100 ml of demineralised water, the solutionfiltered and the filtrate made up to 100 ml with demineralised water. 10 ml of a 2 % by weight aqueous solution of sodium carbonate is then added, the pH adjusted to 11 with sodium hydroxide solution (0.1 N or more concentrated for a large pH adjustment) and the temperature regulated at 20C. The solution is then titrated with a calcium acetate solution (39.59 g/l) at a rate of 1 ml/min until a perm?nent turbidity becomes apparent. The quantity of Ca~ in the calcium acetate solution, determined by a preliminary titration with EDTA, is 10.03 mg Ca~/ml.
The results of the determinations in mg Ca~/g of-test substance were as follows: -Substance Solution with borax Solution without borax (2~/50 ml) Maltodextrin (DE = 12) 40.7 9.7 Mannitol 46.9 7.9 Maltitol 47.~ 9.2
Process for decreasing the build up of inorganic incrustations on textiles and detergent composition used in such process The present invention relates to a process for decreasing the build-up of inorganic incrustations on fabrics caused by water hardness and repeated washing cycles with detergent compositlons.
More particularly, the present invention relates to a process for decreasing the build-up of inorganic incrustations wherein a co-builder is added to the washing cycle, and to detergent and/or anti-incrustation compositions containing said co-builder.
It is well known that detergents contain builders in order to support detergent action and to elimin~te calcium and m~gn~.sium ions (hardness ions), which arise partly from the water and sometimes also from soil and fabrics.
In case of multiple washing cycles the washing performance is significantly reduced because of the build up of inorganic incrustations on fabrics and on washing machine components. Such build up of inorganic incrustations on fabrics decreases the flexibility of fibres and consequently shortens the fabric life, in addition to greying the tissue.
A well known builder is sodium tripolyphosphate which has excellent plopellies in the washing process even at low concentrations. Despite its many advantageous properties however, it causes serious ecological problems, namely~eutrophication of stationary or slowly flowing surface waters leading to extreme algal growth which adversely influences marine org~ni~m.~. As a result, the use of phosphate free detergents is of great importance.
Some substitutes of phosphate builders such as zeolites have been adopted. However, zeolites alone in water softening have poor efficiency. Therefore, good anti-incrustation effects are achieved only in the presence of auxiliary compounds called co-builders.
The most widely used co-builders are synthetic polymers and/or co-polymers of olefinic mono- or dicarboxylic acids such as acrylic and maleic acid and copolymers of said 215~71~
monomers with other allylic or vinylic monomers. A common characteristic of these polymeric materials is their minim~31 biodegradability which leads to ecological problems.
There are known other non-polymeric co-builders, such as EDTA
(ethylenediaminetetraacetic acid sodium salt), NTA (nitrilotriacetic acid sodium salt) and phosphonates. As with the polymeric co-builders these substances too are non-biodegradable.
It is therefore an object of the present invention to provide a process for decreasing the build-up of inorganic incrustations on fabrics and on washing machine components by using co-builders which are very efficient in reducing incrustation build up during washing cycles and which are cheap and biodegradable.
Another object of the present invention is to provide detergent and/or anti-incrustation compositions containing said biodegrable co-builders.
It has now surprisingly been found that certain carbohydrates show a high efficiency in reducing incrustation build up when combined with detergents, particularly with zeolite-based detergents.
In European patent application 0 618 286 there is described a co-builder based upon a non-reducing carbohydrate or a non-reducing carbohydrate derivative. Preferred among the non-reducing carbohydrate derivatives are certain sugar alcohols exemplified by maltitol and, especially, by m~nnitoL It has now been found however-that the carbohydrate or carbohydrate derivative need not be fully non-reducing but that some reducing activity is tolerable and that certain compounds showing such activity are as effective co-builders as the sugar alcohols referred to above.
In accordance with one aspect of the present invention therefore there is provided a process for decreasing the build-up of inorganic incrustations on fabrics and on washing machine components during multiple washing cycles with detergent compositions characterized by the addition to the washing cycle of a co-builder based on a carbohydrate or carbohydrate derivative having a DE of 0.5 to 20 inclusive.
21~8714 A range of carbohydrates or carbohydrate derivatives having a DE of 0.5 to 20 inclusive may be used in the process of the invention eg. polydextrose or partially degraded inulin but preferably the carbohydrate or carbohydrate derivative is a maltodextrin having a DE of 0.5 to 20 inclusive, particularly a DE of ~ to 17 inclusive.
"DE" or dextrose equivalent is a measure of the reducing activity of a carbohydrate measured by comparison with dextrose which has a DE of 100.
The co-builders based on such carbohydrates and carbohydrate derivatives having a DE
of 0.5 to 20 inclusive can be incorporated into the detergent compositions or added as such directly to the washing bath.
In accordance with another aspect of the present invention, there are provided detergent and/or anti-incrustation compositions containing the hereinbefore defined co-builders. These compositions may also contain other conventional components such as anionic, non-ionic, cationic or amphoteric surfactants, aL~ali metal salts (e.g. sodium carbonate, sodium silicate), neutral salts (e.g. sodium sulphate), zeolites, bleaching agents, bleaching activators and other minor ingredients.
In accordance with one preferred embodiment of the present invention the novel co-builders are used in combination with zeolite-based detergents.
The co-builders used according to the present in~ention are particularly efficacious in the presence of inorganic persalts, such as sodium perborate tetrahydrate or monohydrate.
The amount of the co-builders used in the process can vary from 1 g/washing cycle to 40 g/washing cycle, and preferably from 2 g/washing cycle to 20 g/washing cycle. This amount is achieved by a range of from 0.5 ~ to 20 ~ and preferably by a range of from 1 ~ to 10 %, expressed as 100 % dry substance of co-builder in the detergent or anti-incrustation compositions.
The co-builders used according to the present invention are naturally derived, _ 4 _ 7 1 4 biodegradable compounds. In combination with detergents they reduce the build up of inorganic incrustations on fabrics and on washing machine components. Such activity is more significant at high temperatures e.g. at 90C.
The present invention is disclosed in still further detail in the following Example, which is supplied for purely illustrative and not limiting purposes.
Example The co-builder activities of the following compositions were evaluated on a laboratory scale using the so-called "Harnpshire" test which measures the Ca~ sequestering capacity of the composition. The test was carried out as follows :-1 gram of the substance under test is dissolved in 100 ml of demineralised water, the solutionfiltered and the filtrate made up to 100 ml with demineralised water. 10 ml of a 2 % by weight aqueous solution of sodium carbonate is then added, the pH adjusted to 11 with sodium hydroxide solution (0.1 N or more concentrated for a large pH adjustment) and the temperature regulated at 20C. The solution is then titrated with a calcium acetate solution (39.59 g/l) at a rate of 1 ml/min until a perm?nent turbidity becomes apparent. The quantity of Ca~ in the calcium acetate solution, determined by a preliminary titration with EDTA, is 10.03 mg Ca~/ml.
The results of the determinations in mg Ca~/g of-test substance were as follows: -Substance Solution with borax Solution without borax (2~/50 ml) Maltodextrin (DE = 12) 40.7 9.7 Mannitol 46.9 7.9 Maltitol 47.~ 9.2
Claims (10)
1. A process for decreasing the build up of inorganic incrustations on fabrics and on washing machine components during multiple washing cycles characterized by the addition to the washing cycle of a co-builder based on a carbohydrate or carbohydrate derivative having a DE of 0.5 to 20 inclusive.
2. The process according to Claim 1, characterized in that the carbohydrate or carbohydrate derivative is a maltodextrin.
3. The process according to Claim 2 characterized in that the maltodextrin has a DE of 8 to 17 inclusive.
4. The process according to Claim 1, characterized in that the co-builder as such is added directly to the washing bath.
5. The process according to Claim 4, characterized in that the co-builder is added in amount ranging from 1 g/washing cycle to 40 g/washing cycle, preferably from 2 g/washing cycle to 20 g/washing cycle.
6. The process according to Claim 1, characterized in that the co-builder is incorporated in the detergent composition.
7. Detergent and/or anti-incrustation composition containing a co-builder based on a carbohydrate or carbohydrate derivative having a DE of 0.5 to 20.
8. Detergent and/or anti-incrustation composition according to Claim 7, characterized in that it contains a zeolite.
9. Detergent and/or anti-incrustation composition according to Claim 7, characterized in that it contains the co-builder in an amount ranging from 0.5 % to 20 %, preferably from 1 % to 10%, expressed as 100 % dry substance of the detergent or anti-incrustation composition.
10. Detergent and/or anti-incrustation composition according to Claim 7, characterized in that it contains an inorganic persalt.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9419091A GB9419091D0 (en) | 1994-09-22 | 1994-09-22 | Process for decreasing the build up of inorganic incrustations on textiles and detergent composition used in such process |
| GB9419091.5 | 1994-09-22 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2158714A1 true CA2158714A1 (en) | 1996-03-23 |
Family
ID=10761731
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002158714A Abandoned CA2158714A1 (en) | 1994-09-22 | 1995-09-20 | Process for decreasing the build up of inorganic incrustations on textiles and detergent compositions used in such process |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0703292B1 (en) |
| JP (1) | JPH08176593A (en) |
| AT (1) | ATE200692T1 (en) |
| CA (1) | CA2158714A1 (en) |
| DE (1) | DE69520720T2 (en) |
| ES (1) | ES2155500T3 (en) |
| FI (1) | FI113664B (en) |
| GB (1) | GB9419091D0 (en) |
| MX (1) | MX9504068A (en) |
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| US6610752B1 (en) | 1999-10-09 | 2003-08-26 | Cognis Deutschland Gmbh | Defoamer granules and processes for producing the same |
| US6616705B2 (en) | 2000-09-08 | 2003-09-09 | Cognis Deutschland Gmbh & Co. Kg | Laundry detergent compositions |
| US6620209B2 (en) | 2000-09-08 | 2003-09-16 | Cognis Deutschland Gmbh & Co. Kg | Laundry detergent compositions |
| US6686327B1 (en) | 1999-10-09 | 2004-02-03 | Cognis Deutschland Gmbh & Co. Kg | Shaped bodies with improved solubility in water |
| US6723135B2 (en) | 2000-09-19 | 2004-04-20 | Cognis Deutschland Gmbh & Co. Kg | Laundry detergents and cleaning products based on alkyl and/or alkenyl oligoglycosides and fatty alcohols |
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| EP0874889A1 (en) * | 1995-12-07 | 1998-11-04 | Henkel Kommanditgesellschaft auf Aktien | Washing agent comprising a carbonate-containing builder system and/or percarbonate-containing bleach |
| DE19545723A1 (en) * | 1995-12-07 | 1997-06-12 | Henkel Kgaa | Process for the production of dirt-dissolving granules with dextrin carrier and middle containing them |
| DE19704634A1 (en) | 1997-02-07 | 1998-08-27 | Henkel Kgaa | pH-controlled release of detergent components |
| DE19709411A1 (en) | 1997-03-07 | 1998-09-10 | Henkel Kgaa | Detergent tablets |
| DE19850100A1 (en) | 1998-10-29 | 2000-05-04 | Henkel Kgaa | Polymer granules through fluidized bed granulation |
| DE19936613B4 (en) | 1999-08-04 | 2010-09-02 | Henkel Ag & Co. Kgaa | Process for the preparation of a detergent with a soluble builder system |
| DE19944218A1 (en) | 1999-09-15 | 2001-03-29 | Cognis Deutschland Gmbh | Detergent tablets |
| DE19953792A1 (en) | 1999-11-09 | 2001-05-17 | Cognis Deutschland Gmbh | Detergent tablets |
| DE19956802A1 (en) | 1999-11-25 | 2001-06-13 | Cognis Deutschland Gmbh | Detergent tablets |
| DE19956803A1 (en) | 1999-11-25 | 2001-06-13 | Cognis Deutschland Gmbh | Surfactant granules with an improved dissolution rate |
| DE19962883A1 (en) | 1999-12-24 | 2001-07-12 | Cognis Deutschland Gmbh | Detergent tablets |
| DE10003124A1 (en) | 2000-01-26 | 2001-08-09 | Cognis Deutschland Gmbh | Process for the preparation of surfactant granules |
| DE10012949A1 (en) | 2000-03-16 | 2001-09-27 | Henkel Kgaa | Mixtures of cyclic and linear silicic esters of lower alcohols and fragrance and/or biocide alcohols are used as fragrance and/or biocide in liquid or solid laundry and other detergents and in skin and hair cosmetics |
| DE10019344A1 (en) | 2000-04-18 | 2001-11-08 | Cognis Deutschland Gmbh | Detergents and cleaning agents |
| DE10019405A1 (en) | 2000-04-19 | 2001-10-25 | Cognis Deutschland Gmbh | Dry detergent granulate production comprises reducing fatty alcohol content in technical mixture of alkyl and/or alkenyl-oligoglycosides and mixing resultant melt with detergent additives in mixer or extruder |
| DE10031620A1 (en) | 2000-06-29 | 2002-01-10 | Cognis Deutschland Gmbh | liquid detergent |
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| US3022343A (en) * | 1959-11-17 | 1962-02-20 | Pfanstiehl Lab Inc | Sequestrant derived from corn syrup and process for making the same |
| JPS5259605A (en) * | 1975-11-11 | 1977-05-17 | Kao Corp | Detergent composition |
| IT1249883B (en) * | 1990-08-13 | 1995-03-30 | Ferruzzi Ricerca & Tec | CALCIUM SEQUESTRING AGENTS BASED ON OXIDIZED CARBOHYDRATES AND THEIR USE AS BUILDER FOR DETERGENTS |
| EP0618286A1 (en) * | 1993-03-30 | 1994-10-05 | AUSIMONT S.p.A. | Process for decreasing the build up of inorganic incrustations on textiles and detergent composition used in such process |
-
1994
- 1994-09-22 GB GB9419091A patent/GB9419091D0/en active Pending
-
1995
- 1995-09-20 CA CA002158714A patent/CA2158714A1/en not_active Abandoned
- 1995-09-21 JP JP7243433A patent/JPH08176593A/en active Pending
- 1995-09-21 DE DE69520720T patent/DE69520720T2/en not_active Expired - Fee Related
- 1995-09-21 AT AT95306663T patent/ATE200692T1/en not_active IP Right Cessation
- 1995-09-21 EP EP95306663A patent/EP0703292B1/en not_active Expired - Lifetime
- 1995-09-21 ES ES95306663T patent/ES2155500T3/en not_active Expired - Lifetime
- 1995-09-22 FI FI954506A patent/FI113664B/en active
- 1995-09-22 MX MX9504068A patent/MX9504068A/en unknown
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6610752B1 (en) | 1999-10-09 | 2003-08-26 | Cognis Deutschland Gmbh | Defoamer granules and processes for producing the same |
| US6686327B1 (en) | 1999-10-09 | 2004-02-03 | Cognis Deutschland Gmbh & Co. Kg | Shaped bodies with improved solubility in water |
| US6616705B2 (en) | 2000-09-08 | 2003-09-09 | Cognis Deutschland Gmbh & Co. Kg | Laundry detergent compositions |
| US6620209B2 (en) | 2000-09-08 | 2003-09-16 | Cognis Deutschland Gmbh & Co. Kg | Laundry detergent compositions |
| US6723135B2 (en) | 2000-09-19 | 2004-04-20 | Cognis Deutschland Gmbh & Co. Kg | Laundry detergents and cleaning products based on alkyl and/or alkenyl oligoglycosides and fatty alcohols |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0703292B1 (en) | 2001-04-18 |
| DE69520720T2 (en) | 2001-08-02 |
| FI954506A (en) | 1996-03-23 |
| FI113664B (en) | 2004-05-31 |
| ATE200692T1 (en) | 2001-05-15 |
| GB9419091D0 (en) | 1994-11-09 |
| JPH08176593A (en) | 1996-07-09 |
| DE69520720D1 (en) | 2001-05-23 |
| FI954506A0 (en) | 1995-09-22 |
| EP0703292A1 (en) | 1996-03-27 |
| MX9504068A (en) | 1997-02-28 |
| ES2155500T3 (en) | 2001-05-16 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FZDE | Discontinued |