CN1084415C - Process for preparing hydrolyzable sheet - Google Patents
Process for preparing hydrolyzable sheet Download PDFInfo
- Publication number
- CN1084415C CN1084415C CN96191731A CN96191731A CN1084415C CN 1084415 C CN1084415 C CN 1084415C CN 96191731 A CN96191731 A CN 96191731A CN 96191731 A CN96191731 A CN 96191731A CN 1084415 C CN1084415 C CN 1084415C
- Authority
- CN
- China
- Prior art keywords
- water
- carboxymethyl cellulose
- salt
- paper
- comparative example
- 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 - Fee Related
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Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
- D21H17/24—Polysaccharides
- D21H17/25—Cellulose
- D21H17/26—Ethers thereof
Landscapes
- Paper (AREA)
- Cleaning Implements For Floors, Carpets, Furniture, Walls, And The Like (AREA)
Abstract
The invention relates to a process to improve wet strength and dispersibility to water of a water-disintegrable sheet usable as wet wipes. A mixture of water-swelling or water-insoluble carboxymethyl cellulose and/or salt thereof having a degree of substitution which is equal to 0.30 - 0.60 and a value of pH which is more than or equal to 5.0 and water-dispersible fibers is subjected to a sheet-making step of a process to obtain the water-disintegrable sheet and, before or after the sheet-making step of the process, the mixture is added with a base.
Description
Technical field
The present invention relates to a kind of manufacture method of the water-disintegrable paper wood (sheet) that can in water, disperse or dissolve.
Background technology
In the past, a kind of hygenic towelette (wet wipes) that is used to wipe hand or wiping domestic appliance is well-known.In addition, a kind of can be that the water dispersible or the water-disintegrable paper products of representative also are well-known at the hygenic towelette that washes away with water in case just can disperse or dissolve very soon when dropping in the water such as water closet and with it.Said herein water dispersible is identical with water-disintegrable implication, and for the hygenic towelette with this character, people have high intensity when requiring it to use under moisture state, but just can promptly disperse in dropping into a large amount of water the time.In order to take into account said intensity and dispersed this two aspect, open sodium/sylvite that uses a kind of water-insoluble carboxymethyl cellulose in the flat 1-168999 communique or the sodium salt that uses carboxymethyl cellulose the spy.Disclose a kind of system paper method in the public clear 48-27605 communique of spy, this method is at first to use water-insoluble carboxymethyl cellulose to copy the system l Water Paper, then to this l Water Paper alkali-metal aqueous solution of spraying.Disclosed method is that alkali metal salt with water-insoluble carboxymethyl cellulose mixes with paper stock in the Te Kaiping 3-167400 communique, copies system then.In addition, it is at first the alkali metal salt of carboxymethyl cellulose to be mixed with paper stock and copy and make paper that the spy opens disclosed method in the flat 5-25792 communique, floods with a kind of water-containing organic solvent that contains polyvalent metal ion then and copies the paper of making.
In above-mentioned prior art, the carboxymethyl cellulose and the salt thereof that use as adhesive are gone forward side by side and are become water-soluble to the swelling variation by water-insoluble step by step along with the rising of its degree of exchange (D.S.) and pH value usually.When these carboxymethyl celluloses or its salt are made when being used for copying paper as adhesive, the swelling of adhesive is high more, then be difficult to even more with mixed with fibers, in addition, if adhesive is water miscible, can make that then adhering to the amount of binder of copying on the paper wood of making tails off, and can't see the raising with the paper strength of the use amount certain degree of adhesive.In addition, in copying the operation that again adhesive is attached to by spraying after making paper wood on the paper wood,, be difficult to adhesive is sprayed equably if the swelling height of carboxymethyl cellulose or its salt then this viscosity in aqueous solution increase.
So problem of the present invention is to can be used as in the manufacture method of the hydrolyzable sheet that hygenic towelette etc. uses in manufacturing, with the carboxymethyl cellulose of aequum and/or its salt expeditiously attached on the paper wood.
Disclosure of an invention
In order to solve above-mentioned problem, the purpose of this invention is to provide a kind of manufacture method of the hydrolyzable sheet that constitutes by carboxymethyl cellulose and/or its salt and water-dispersible fiber.
The invention is characterized in, make a kind of by having degree of exchange (D.S.)=0.30～0.60, the mixture that the water-swellable of pH 〉=5.0 or water-insoluble carboxymethyl cellulose and/or its salt and water-dispersible fiber constitute is made above-mentioned hydrolyzable sheet through machine hand's preface, adds alkali before or after above-mentioned machine hand's preface of this manufacturing process in said mixture.
In a preferred embodiment of the invention, above-mentioned alkali is sodium carbonate.In addition, in manufacture method of the present invention, also comprise and use the dipping operation of a kind of hygenic towelette with soup dipping said hydrolyzed paper wood.
The preferred plan that is used to carry out an invention
The raw material that is used for manufacture method of the present invention comprises a kind of water-dispersible fiber that can realize paper woodization with carboxymethyl cellulose and/or its salt.For this fiber, preferably use paper pulp fiber, but be not limited in this respect, also can use natural fabrics such as flax, wool; Regenerated fibers such as rayon fiber; Semisynthetic fibres such as acetate fiber; Synthetic fiber such as nylon, polyester.For these fibers, use a class to have D.S.=0.30～0.60, pH 〉=5.0, water-swellable low or water miscible carboxymethyl cellulose and/or its salt as adhesive.In order to make said adhesive become the high or water miscible adhesive of water-swellable, can be to wherein adding alkali.As said alkali, which type of alkali can use, but preferably uses sodium carbonate.For the mixture of fiber and adhesive is made paper wood, preferably utilize the known paper technology of copying.In addition, also can utilize wet type or dry type nonwoven fabric manufacturing technology, utilize the nonwoven fabric manufacturing technology of high-pressure injection current (water-jet) etc.The operation that adds alkali in adhesive can be carried out in the arbitrary stage before or after copying the system operation.Also can think and be included in stage before or after this and copy system operation itself interior.Explain the present invention according to embodiment below.
Embodiment 1～5
Paper grade (stock) coniferous tree paper pulp (NBKP), carboxymethyl cellulose and/or its salt are mixed in running water, in this dispersion liquid, add the sodium carbonate of dissolving aequum, with this mixture as paper stock.After this paper stock left standstill, copy system with a kind of small-scale test paper machine, use then a kind of turn round the drum type drying machine under 110 ℃ humidity with the warm paper that is obtained dry 90 seconds, obtaining a kind of weight per unit area is 40g/m
2Dry paper wood.The mixed liquor that uses a kind of propylene glycol/calcium chloride/ion exchange water=30/0.5/69.5 (weight ratio) then is as the hygenic towelette soup, according to the amount of liquid medicine that is equivalent to 2.5 times of paper wood weight spray the dipping this paper wood, left standstill 24 hours at 20 ℃ then, promptly obtained hygenic towelette.By the water dispersible and the moistening tensile strength of following condition determination hygenic towelette that evaluation obtains, confirm that with this various conditions in copying the system process are to the influence of above-mentioned characteristic.The results are shown in Table 1 in evaluation.In addition, list the relation of a series of embodiment and comparative example below.
(1) embodiment 1 and comparative example 1
Show influence with respect to the addition (weight %) of the sodium carbonate of the dry weight of carboxymethyl cellulose and/or its salt.
(2) embodiment 2 and comparative example 2
Show the degree of exchange (D.S.) of carboxymethyl cellulose and/or its salt and the influence of pH value generation.
(3) embodiment 3 and comparative example 3
The influence that the total amount (weight %) of paper pulp in the paper stock and carboxymethyl cellulose and/or its salt of showing produces.
(4) embodiment 4 and comparative example 4
Show the influence that the time of repose after adding sodium carbonate produces.
(5) embodiment 5 and comparative example 5
Show the influence of the mixing ratio generation of paper pulp and carboxymethyl cellulose and/or its salt.
The evaluation of water dispersible
One of the hygenic towelette test film input of one 10cm * 10cm is equipped with in the 300ml glass beaker of 300ml ion exchange water, uses magnetic stirring apparatus to stir (rotation number 600rpm), in time through observing the dispersity in the l Water Paper.Observed result is done following evaluation.
A: test film 100 seconds with interior finely divided.
B: test film 200 seconds with interior finely divided.
C: test film 200 seconds with interior do not have finely divided.
The evaluation of moistening tensile strength
With a kind of clamp of hygenic towelette test film of a kind of wide 25mm * long 250mm, be spaced apart 100mm between two chucks, stretch to measure its breaking strength according to the draw speed of 100mm/min.The result shows, just is enough to be used in actual use as long as the breaking strength of hygenic towelette is not less than 300g.
According to the evaluation result of embodiment and comparative example, can be summarized as follows:
(1) carboxymethyl cellulose and/or its salt preferably have degree of exchange D.S=0.30～0.60, pH 〉=5.0 (embodiment 2); (2) amount of sodium carbonate preferably is equivalent to 10～400% (embodiment 1) of the weight of carboxymethyl cellulose and/or its salt; (3) weight ratio of paper pulp and carboxymethyl cellulose and/or its salt is preferably 98: 2～55: 45 scope; (4) paper pulp and carboxymethyl cellulose and/or its salt shared concentration in paper stock is preferably 0.5～5 weight %; And the time of repose behind (5) interpolation sodium carbonate is preferably more than 30 minutes.Table 1
| Test No. | Paper pulp/CMC mixing ratio | CMC | Paper pulp in the paper stock/CMC concentration (%) | Sodium carbonate amount (the weight % of CMC relatively) | The time of repose of paper stock (hour) | Evaluation result | Remarks | ||
| D.S. | pH | Water dispersible | Tensile strength (g/25mm is wide) | ||||||
| 1 of embodiment 1 | 87.5/12.5 | 0.43 | 6.1 | 1 | 80 | 2 | B | 466 | |
| 2 of embodiment 1 | 87.5/12.5 | 0.43 | 6.1 | 1 | 160 | 2 | A | 704 | |
| 3 of embodiment 1 | 87.5/12.5 | 0.43 | 6.1 | 1 | 400 | 2 | B | 737 | |
| 1 of embodiment 1 | 87.5/12.5 | 0.43 | 6.1 | 1 | 2 | 2 | C | 448 | |
| 2 of embodiment 1 | 87.5/12.5 | 0.43 | 6.1 | 1 | 0 | 2 | C | 326 | |
| 1 of embodiment 2 | 87.5/12.5 | 0.58 | 6.0 | 1 | 80 | 2 | A | 517 | |
| 1 of comparative example 2 | 87.5/12.5 | 0.43 | 4.7 | 1 | 80 | 2 | B | 195 | |
| 2 of comparative example 2 | 87.5/12.5 | 0.88 | 6.9 | 1 | 80 | 2 | A | 253 | |
| 1 of embodiment 3 | 87.5/12.5 | 0.43 | 6.1 | 3 | 160 | 2 | A | 589 | |
| 1 of comparative example 3 | 87.5/12.5 | 0.43 | 6.1 | 0.04 | 160 | 2 | A | 271 | |
| 2 of comparative example 3 | 87.5/12.5 | 0.43 | 6.1 | 10 | 160 | 2 | - | - | Can not copy system |
| 1 of embodiment 4 | 87.5/12.5 | 0.43 | 6.1 | 2 | 160 | 1 | B | 466 | |
| 1 of comparative example 4 | 87.5/12.5 | 0.43 | 6.1 | 2 | 160 | 0.15 | C | 428 | |
| 1 of embodiment 5 | 95/5 | 0.43 | 6.1 | 2 | 80 | 2 | A | 320 | |
| 1 of comparative example 5 | 99.5/0.5 | 0.43 | 6.1 | 2 | 80 | 2 | A | 63 | |
| 2 of comparative example 5 | 50/50 | 0.43 | 6.1 | 2 | 80 | 2 | - | - | Can not peel off from drying machine |
(notes) CMS: carboxymethyl cellulose and/or its salt
Embodiment 6 and 7
Paper grade (stock) coniferous tree paper pulp (NBKP) is mixed in running water with carboxymethyl cellulose and/or its salt, disperseing the back liquid that obtains as raw material, copy system with the small-scale test paper machine, use then to contain to be equivalent to the aqueous solution spraying that institute obtains the sodium carbonate of contained carboxymethyl cellulose in the wet paper and/or its salt 2.4～8 weight % and to flood the wet paper that is obtained, the amount of said spray solution is equivalent to 2.5 times of wet paper dry weight.Use revolution drum type drying machine 110 ℃ of following dry 90 seconds then, obtaining a kind of weight per unit area is 40g/m
2Dry paper wood.The mixed liquor that uses a kind of propylene glycol/calcium chloride/ion exchange water=30/0.5/69.5 (weight ratio) then is as the hygenic towelette soup, with the soup that is equivalent to 2.5 times of amounts of paper wood weight spray the dipping this paper wood, under 20 ℃, left standstill 24 hours again, thereby obtained hygenic towelette.By the water dispersible and the moistening tensile strength of said determination hygenic towelette that condition evaluating obtains, the various conditions of affirmation in copying the system process are to the influence of above-mentioned characteristic.The relation of embodiment and comparative example is as described below.
(1) embodiment 6 and comparative example 6
Show influence with respect to the addition (weight %) of the sodium carbonate of the dry weight of carboxymethyl cellulose and/or its salt.
(2) embodiment 7 and comparative example 7
Show the degree of exchange (D.S.) of carboxymethyl cellulose and/or its salt and the influence that the pH value produces.The evaluation result of embodiment and comparative example is as shown in table 2.
Table 2
| Test No. | Paper pulp/CMC mixing ratio | CMC | Sodium carbonate amount (the weight % of CMC relatively) | Evaluation result | ||
| D.S | pH | Water dispersible | Tensile strength (g/25mm is wide) | |||
| 1 of embodiment 6 | 87.5/12.5 | *0.50 | 7.3 | 2.4 | A | 475 |
| 2 of embodiment 6 | 87.5/12.5 | *0.50 | 7.3 | 4.0 | A | 416 |
| 3 of embodiment 6 | 87.5/12.5 | *0.50 | 7.3 | 8.0 | A | 380 |
| 1 of comparative example 6 | 87.5/12.5 | *0.50 | 7.3 | 0.0 | C | 438 |
| 1 of embodiment 7 | 87.5/12.5 | *0.43 | 6.1 | 8.0 | A | 401 |
| 2 of embodiment 7 | 87.5/12.5 | *0.50 | 7.3 | 8.0 | A | 380 |
| 1 of comparative example 7 | 87.5/12.5 | **0.64 | 3.9 | 8.0 | A | 133 |
| 2 of comparative example 7 | 87.5/12.5 | *0.88 | 6.9 | 8.0 | A | 83 |
1.CMC: carboxymethyl cellulose and/or its salt
2.
*: sodium carboxymethylcellulose
3.
*: the acid type carboxymethyl cellulose
The possibility of utilizing on the industry
In the manufacture method of the said hydrolyzable sheet of the present invention, owing to mixing with water-dispersible fiber as the low swelling of adhesive or water-insoluble carboxymethyl cellulose and/or its salt, so so that on the paper wood by this mixture acquisition, adhere to easily the adhesive of more amount. Said adhesive is owing to the interpolation of alkali becomes water-swellable or water-soluble, therefore not only can improve the moistening intensity of hydrolyzable sheet, and the hydrolysis paper after using can dissolve rapidly or swelling in dropping into a large amount of water the time, thereby hydrolyzable sheet is promptly disperseed.
Claims (2)
1. manufacture method of making hydrolyzable sheet by carboxymethyl cellulose and/or its salt and water-dispersible fiber, it is characterized in that, with a kind of by the water-swellable with degree of exchange (D.S.)=0.30～0.60 and pH 〉=5.0 or water-insoluble carboxymethyl cellulose and/or its salt be dispersed in the water after water-dispersible fiber mixes, add 10～400% sodium carbonate then with respect to the weight of carboxymethyl cellulose and/or its salt, carboxymethyl cellulose and/or the concentration range of its salt in dispersed mixture are 0.5-5 weight %, after adding sodium carbonate dispersed mixture was left standstill 30 minutes, then dispersed mixture is made hydrolyzable sheet through machine hand's preface.
2. manufacture method as claimed in claim 1 wherein also comprises and uses the operation of warm paper handkerchief with soup dipping said hydrolyzed paper wood.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP285480/95 | 1995-11-02 | ||
| JP285479/95 | 1995-11-02 | ||
| JP28548095A JP3150587B2 (en) | 1995-11-02 | 1995-11-02 | Water disintegration sheet manufacturing method |
| JP28547995A JP3150586B2 (en) | 1995-11-02 | 1995-11-02 | Water disintegration sheet manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1172515A CN1172515A (en) | 1998-02-04 |
| CN1084415C true CN1084415C (en) | 2002-05-08 |
Family
ID=26555907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96191731A Expired - Fee Related CN1084415C (en) | 1995-11-02 | 1996-11-01 | Process for preparing hydrolyzable sheet |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP0802282A1 (en) |
| KR (1) | KR100235789B1 (en) |
| CN (1) | CN1084415C (en) |
| CA (1) | CA2208759C (en) |
| MY (1) | MY125612A (en) |
| TW (1) | TW306943B (en) |
| WO (1) | WO1997016597A1 (en) |
Families Citing this family (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3205705B2 (en) * | 1996-07-26 | 2001-09-04 | ユニ・チャーム株式会社 | Method for manufacturing wet wipes |
| JP3865506B2 (en) * | 1997-09-08 | 2007-01-10 | ユニ・チャーム株式会社 | Water-decomposable fiber sheet containing fibers with different fiber lengths |
| US6423804B1 (en) | 1998-12-31 | 2002-07-23 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive hard water dispersible polymers and applications therefor |
| US6579570B1 (en) | 2000-05-04 | 2003-06-17 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| US6713414B1 (en) | 2000-05-04 | 2004-03-30 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| SE9903418D0 (en) * | 1999-09-22 | 1999-09-22 | Skogsind Tekn Foskningsinst | Method for modifying cellulose-based fiber materials |
| JP2001098489A (en) | 1999-09-30 | 2001-04-10 | Uni Charm Corp | Water-disintegrable fibrous sheet containing water- insoluble carboxymethyl cellulose |
| JP3703661B2 (en) * | 1999-10-05 | 2005-10-05 | ユニ・チャーム株式会社 | Water-decomposable fiber sheet containing gel compound |
| CO5200821A1 (en) | 1999-11-23 | 2002-09-27 | Kimberly Clark Co | TISU SANITARY PRODUCTS WITH IMPROVED DISPOSAL CAPACITY IN THE TOILET |
| JP3722665B2 (en) * | 2000-03-31 | 2005-11-30 | ユニ・チャーム株式会社 | Multi-structured water-decomposable wiping sheet |
| US6815502B1 (en) | 2000-05-04 | 2004-11-09 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive, water-dispersable polymers, a method of making same and items using same |
| US6835678B2 (en) | 2000-05-04 | 2004-12-28 | Kimberly-Clark Worldwide, Inc. | Ion sensitive, water-dispersible fabrics, a method of making same and items using same |
| US6653406B1 (en) | 2000-05-04 | 2003-11-25 | Kimberly Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| US6683143B1 (en) | 2000-05-04 | 2004-01-27 | Kimberly Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| US6599848B1 (en) | 2000-05-04 | 2003-07-29 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| US6444214B1 (en) | 2000-05-04 | 2002-09-03 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| US6548592B1 (en) | 2000-05-04 | 2003-04-15 | Kimberly-Clark Worldwide, Inc. | Ion-sensitive, water-dispersible polymers, a method of making same and items using same |
| EP1167510A1 (en) * | 2000-06-23 | 2002-01-02 | The Procter & Gamble Company | Flushable hard surface cleaning wet wipe |
| JP2002078733A (en) * | 2000-06-28 | 2002-03-19 | Uni Charm Corp | Absorptive article |
| US6586529B2 (en) | 2001-02-01 | 2003-07-01 | Kimberly-Clark Worldwide, Inc. | Water-dispersible polymers, a method of making same and items using same |
| US6828014B2 (en) | 2001-03-22 | 2004-12-07 | Kimberly-Clark Worldwide, Inc. | Water-dispersible, cationic polymers, a method of making same and items using same |
| MXPA04012890A (en) | 2002-06-19 | 2005-03-31 | Bayer Chemicals Corp | Strong and dispersible paper products. |
| KR102635615B1 (en) | 2023-07-04 | 2024-02-14 | 주식회사 정우세이프티 | Signs outputting safety information and method for providing safety information of signs |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03167400A (en) * | 1989-11-27 | 1991-07-19 | Nichirin Kagaku Kogyo Kk | Hydrolyzable paper |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01168999A (en) * | 1987-12-23 | 1989-07-04 | Kao Corp | Cleaning material easily dispersible in water |
| JP2700825B2 (en) * | 1989-03-25 | 1998-01-21 | ライオン株式会社 | Water-decomposable / absorbable sheet and method for producing the same |
| JPH03180596A (en) * | 1989-12-06 | 1991-08-06 | Nichirin Kagaku Kogyo Kk | Water-soluble paper giving little dissolution residue |
| JP3243066B2 (en) * | 1992-10-29 | 2002-01-07 | ニチリン化学工業株式会社 | Method for producing water-dispersible sheet |
| US5487813A (en) * | 1994-12-02 | 1996-01-30 | The Procter & Gamble Company | Strong and soft creped tissue paper and process for making the same by use of biodegradable crepe facilitating compositions |
-
1996
- 1996-11-01 MY MYPI9604567 patent/MY125612A/en unknown
- 1996-11-01 CN CN96191731A patent/CN1084415C/en not_active Expired - Fee Related
- 1996-11-01 WO PCT/JP1996/003213 patent/WO1997016597A1/en active IP Right Grant
- 1996-11-01 CA CA002208759A patent/CA2208759C/en not_active Expired - Fee Related
- 1996-11-01 KR KR1019970704561A patent/KR100235789B1/en not_active IP Right Cessation
- 1996-11-01 EP EP96935528A patent/EP0802282A1/en not_active Withdrawn
- 1996-11-19 TW TW85114165A patent/TW306943B/zh not_active IP Right Cessation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03167400A (en) * | 1989-11-27 | 1991-07-19 | Nichirin Kagaku Kogyo Kk | Hydrolyzable paper |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0802282A4 (en) | 1997-11-05 |
| TW306943B (en) | 1997-06-01 |
| EP0802282A1 (en) | 1997-10-22 |
| CN1172515A (en) | 1998-02-04 |
| KR987001056A (en) | 1998-04-30 |
| CA2208759C (en) | 2003-03-11 |
| KR100235789B1 (en) | 1999-12-15 |
| CA2208759A1 (en) | 1997-05-09 |
| WO1997016597A1 (en) | 1997-05-09 |
| MY125612A (en) | 2006-08-30 |
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Granted publication date: 20020508 Termination date: 20131101 |