EP0659219B1 - Fibres cellulosiques - Google Patents

Fibres cellulosiques Download PDF

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Publication number
EP0659219B1
EP0659219B1 EP94921517A EP94921517A EP0659219B1 EP 0659219 B1 EP0659219 B1 EP 0659219B1 EP 94921517 A EP94921517 A EP 94921517A EP 94921517 A EP94921517 A EP 94921517A EP 0659219 B1 EP0659219 B1 EP 0659219B1
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EP
European Patent Office
Prior art keywords
air gap
air
spinning
cellulose
pct
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
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EP94921517A
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German (de)
English (en)
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EP0659219A1 (fr
Inventor
Hartmut Rüf
Markus Eibl
Raimund Jurkovic
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Lenzing AG
Original Assignee
Lenzing AG
Chemiefaser Lenzing AG
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Publication of EP0659219A1 publication Critical patent/EP0659219A1/fr
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/30—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising olefins as the major constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D04H3/007—Addition polymers
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/016—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the fineness
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion

Definitions

  • the present invention relates to cellulose fibers and to a process for the production of cellulose fibers, a solution of cellulose in a tertiary amine oxide being extruded through spinning holes in a spinneret and the extruded filaments being passed through an air gap with delay into a precipitation bath.
  • N-methylmorpholine-N-oxide is used as the solvent.
  • NMMO N-methylmorpholine-N-oxide
  • Fibrillation is understood to mean breaking open the fiber in the longitudinal direction under mechanical stress in the wet state, as a result of which the fiber is given a hairy, furry appearance.
  • a fabric made and dyed from these fibers loses its color intensity over the course of a few washes.
  • the cause of the fibrillation is assumed to be that the fiber consists of fibrils arranged in the direction of the fibers, between which there is only a small amount of cross-connection.
  • WO 92/14871 describes a method for producing a fiber with a reduced tendency to fibrillation. This is achieved in that all baths with which the fiber comes into contact before the first drying have a pH of maximum 8.5.
  • WO 92/07124 also describes a method for producing a fiber with a reduced tendency to fibrillation, according to which the undried fiber is treated with a cationic polymer.
  • a polymer with imidazole and azetidine groups is mentioned as such a polymer.
  • treatment with an emulsifiable polymer e.g. Polyethylene or polyvinyl acetate, or crosslinking with glyoxal.
  • the invention is based on the knowledge that the structure of the cellulose fiber can be influenced so favorably by setting the spinning parameters that a less fibrillating fiber is formed.
  • a preferred embodiment of the method according to the invention is that the method is carried out in such a way that the mathematical expression results in a maximum of 5.
  • the overall parameters titer, spinning mass emissions per nozzle hole, air gap width and moisture in the air gap are related in terms of their effect on the fibrillation behavior of the fibers via the above mathematical expression, that is, a change in a parameter which has a negative effect on fibrillation can be achieved by appropriate adaptation one or more other parameters can be compensated.
  • This naturally results Limits due to economic or technical circumstances, for example a spinning mass throughput of 0.01 g / hole / min offers excellent conditions for spinning a low-fibrillation fiber, but is unfavorable for economic reasons. A spinning mass throughput of 0.025 to 0.05 g / hole / min is therefore preferred.
  • the humidity of the air in the air gap the humidity of the normal indoor climate is sufficient for nozzles with a small diameter of the spinning holes or the lowest spinning mass throughput, while for higher throughputs or for the more easily spinnable nozzles an air humidity between 20 and 30 g is sufficient Water / kg air is preferred.
  • the temperature in the air gap is chosen so that on the one hand the dew point is not fallen below, i.e. that no water condenses in the air gap and on the other hand that there are no difficulties in spinning due to the temperature being too high. Values between 10 and 60 ° C can be set, with temperatures between 20 and 40 ° C being preferred.
  • All known cellulosic spinning materials can be processed by the process according to the invention. So these spinning masses can contain between 5 and 25% cellulose. However, cellulose contents between 10 and 18% are preferred. Hard or softwood can be used as the raw material for pulp production, and the degrees of polymerization of the pulp (s) can be in the range of commercially available products. However, it has been shown that the spinning behavior is better with a higher molecular weight of the pulp is. Depending on the degree of polymerization of the pulp or solution concentration, the spinning temperature can be between 75 and 140 ° C. and can be optimized in a simple manner for each pulp or for each concentration.
  • the warping in the air gap depends on the diameter of the nozzle hole and the concentration of cellulose in the solution when the titer of the fibers is fixed. In the range of the preferred cellulose concentration, however, no influence of this on the fibrillation obsolescence could be determined as long as one is in the area of the optimal spinning temperature.
  • the friction of the fibers against one another during washing processes or during finishing processes in the wet state was simulated by the following test: 8 fibers were placed in a 20 ml sample vial with 4 ml water and in a laboratory shaker type RO-10 from Gerhardt for 3 hours, Bonn (FRG) shaken at level 12. The fibrillation behavior of the fibers was then assessed under the microscope by counting the number of fibrils per 0.276 mm fiber length.
  • a melt index device from Davenport used in plastics processing was used as the spinning apparatus. This device consists of a heated, temperature-controlled cylinder into which the spinning mass is poured. The spinning mass is extruded through the spinneret attached to the underside of the cylinder by means of a piston which is loaded with a weight. This process is called dry / wet spinning because the extruded filament is immersed in a spinning bath after passing through an air gap.
  • the table shows the diameter of the spinning hole in ⁇ m, the output in g of spinning mass / hole / min, the titer in dtex, the air gap in mm and the moisture in g H2O / kg of air.
  • the number given under "Fibrils" is an average of several results. Examples 4, 12, 13, 14, 20, 22, 25, 27 and 29 are comparative examples. All other examples are according to the invention and, when the corresponding parameters are inserted in the empirically found mathematical expression, give a number less than 10.
  • the table shows that the cellulose fibers according to the invention have remarkably fewer fibrils than the comparison fibers in the test.
  • Examples 30, 31, 33, 35, 36 and 38 do not meet the mathematical expression used according to the invention and represent comparative examples.
  • the table shows that these fibers have an increased number of fibrils (more than 10 fibrils per 276 ⁇ m fiber length).
  • Table 3 shows characteristic fiber data for the fibers shown in Table 2.
  • Table 3 Example No. Fiber strength cond. cN / tex Fiber elongation cond. % Fiber strength wet cN / tex Fiber stretch wet% 30 (V) 46.1 10.5 33.8 14.2 31 (V) 50 11.3 41.4 14 32 31.9 17.7 27.5 24.5 33 (V) 34.3 15.2 29.1 23.5 34 28.8 16.5 24.5 21.8 35 (V) 34.1 14.8 29.3 19.8 36 (V) 33.3 16.3 30.5 18.8 37 29.4 17.2 23.9 21.3 38 (V) 30.4 11.8 22.5 14.3 39 25.6 15.6 19.5 22.5 40 24.6 14.8 18.2 21.4 41 28.5 15.8 24.2 20.9
  • Table 4 shows a significant reduction in the number of fibrils as soon as an air gap of about 25-30 mm is exceeded.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Materials For Medical Uses (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Claims (6)

  1. Procédé de fabrication de fibres cellulosiques par extrusion d'une solution de cellulose dans un oxyde d'amine tertiaire par les orifices de filage d'une filière et amenée des filaments extrudés par un interstice sous étirage dans un bain de précipitation, pour autant que la largeur de l'interstice prévu soit supérieure à 30 mm, caractérisé en ce que le procédé est mis en oeuvre de façon telle que l'expression mathématique 51,4 + 0,033xD = 1937xM 2 - 7,18xt - 0,094xL - 2,50xF + 0,045xF 2
    Figure imgb0008
     où D est le diamètre des orifices de filage en µm, N le débit de masse de filage par orifice en g/min, T le titre d'un filament individuel en dtex, L la largeur de l'interstice en mm et F l'humidité de l'air dans l'interstice en g d'eau par kg d'air, donne au maximum le chiffre de 10.
  2. Procédé selon la revendication 1, caractérisé en ce que le procédé est mis en oeuvre de telle sorte que l'expression mathématique donne au maximum le chiffre de 5.
  3. Procédé selon une des revendications 1 et 2, caractérisé en ce que le débit de masse de filage par orifice est compris entre 0,025 et 0,05 g/min.
  4. Procédé selon une ou plusieurs des revendications 1 à 3, caractérisé en ce que la largeur de l'interstice prévu est inférieure à 100 mm.
  5. Procédé selon la revendication 1 ou 2, caractérisé en ce que, dans le cas d'une filière ayant des orifices de filage dont le diamètre est compris entre 70 et 130 µm, on règle l'humidité de l'air dans l'interstice à un chiffre compris entre 20 et 30 g d'eau par kg d'air.
  6. Fibre cellulosique du type Lyocell présentant une tendance réduite à la fibrillation, qu'il est possible d'obtenir par un procédé selon les revendications 1 à 5.
EP94921517A 1993-07-08 1994-07-08 Fibres cellulosiques Expired - Lifetime EP0659219B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT0134893A AT401271B (de) 1993-07-08 1993-07-08 Verfahren zur herstellung von cellulosefasern
AT1348/93 1993-07-08
PCT/AT1994/000087 WO1995002082A1 (fr) 1993-07-08 1994-07-08 Fibres cellulosiques

Publications (2)

Publication Number Publication Date
EP0659219A1 EP0659219A1 (fr) 1995-06-28
EP0659219B1 true EP0659219B1 (fr) 1996-01-31

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EP94921517A Expired - Lifetime EP0659219B1 (fr) 1993-07-08 1994-07-08 Fibres cellulosiques

Country Status (34)

Country Link
US (1) US5543101A (fr)
EP (1) EP0659219B1 (fr)
JP (1) JP2768831B2 (fr)
KR (1) KR0173007B1 (fr)
CN (1) CN1090249C (fr)
AT (2) AT401271B (fr)
AU (1) AU668655B2 (fr)
BG (1) BG99431A (fr)
BR (1) BR9405504A (fr)
CA (1) CA2142111A1 (fr)
CZ (1) CZ288757B6 (fr)
DE (2) DE4494808D2 (fr)
DK (1) DK0659219T3 (fr)
ES (1) ES2085187T3 (fr)
FI (1) FI951057A (fr)
GB (1) GB2284383B (fr)
GR (1) GR3019296T3 (fr)
HK (1) HK1000327A1 (fr)
HR (1) HRP940392B1 (fr)
HU (1) HU214034B (fr)
ID (1) ID913B (fr)
NO (1) NO950865D0 (fr)
PE (1) PE696A1 (fr)
PH (1) PH30806A (fr)
PL (1) PL307852A1 (fr)
RO (1) RO113875B1 (fr)
RU (1) RU2120505C1 (fr)
SI (1) SI0659219T1 (fr)
SK (1) SK29095A3 (fr)
TR (1) TR28323A (fr)
UA (1) UA29456C2 (fr)
WO (1) WO1995002082A1 (fr)
YU (1) YU48582B (fr)
ZA (1) ZA944768B (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10043297B4 (de) * 2000-09-02 2005-12-08 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. Verfahren zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen

Families Citing this family (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT399729B (de) * 1993-07-01 1995-07-25 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer fasern sowie vorrichtung zur durchführung des verfahrens und deren verwendung
KR100398294B1 (ko) * 1994-12-02 2003-12-31 네브첼 게엠베하 운트 콤파니 카게 셀룰로즈형성물의제조방법및셀룰로즈필라멘트사
AT402740B (de) * 1995-10-06 1997-08-25 Chemiefaser Lenzing Ag Cellulosefaser
AT404032B (de) * 1996-03-04 1998-07-27 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer fasern
GB9605504D0 (en) * 1996-03-15 1996-05-15 Courtaulds Plc Manufacture of elongate members
GB9607456D0 (en) * 1996-04-10 1996-06-12 Courtaulds Fibres Holdings Ltd Spinning of filaments
US6471727B2 (en) 1996-08-23 2002-10-29 Weyerhaeuser Company Lyocell fibers, and compositions for making the same
US6306334B1 (en) 1996-08-23 2001-10-23 The Weyerhaeuser Company Process for melt blowing continuous lyocell fibers
US6331354B1 (en) 1996-08-23 2001-12-18 Weyerhaeuser Company Alkaline pulp having low average degree of polymerization values and method of producing the same
US6210801B1 (en) 1996-08-23 2001-04-03 Weyerhaeuser Company Lyocell fibers, and compositions for making same
GB2319495A (en) * 1996-11-26 1998-05-27 Courtaulds Fibres Method and apparatus for the manufacture of lyocell fibres
AT405531B (de) 1997-06-17 1999-09-27 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer fasern
US6773648B2 (en) 1998-11-03 2004-08-10 Weyerhaeuser Company Meltblown process with mechanical attenuation
DE10062083B4 (de) * 2000-12-13 2008-04-10 Ostthüringische Materialprüfgesellschaft Für Textil Und Kunststoffe Mbh Verfahren zur Herstellung von Celluloseendlosformkörpern
AT6807U1 (de) * 2004-01-13 2004-04-26 Chemiefaser Lenzing Ag Cellulosische faser der gattung lyocell
KR100575378B1 (ko) * 2004-11-10 2006-05-02 주식회사 효성 셀룰로오스 섬유의 제조방법
TWI667378B (zh) * 2014-01-03 2019-08-01 奧地利商蘭精股份有限公司 纖維素纖維
US20200240043A1 (en) * 2017-10-06 2020-07-30 Lenzing Aktiengesellschaft Flame retardant lyocell filament
EP3536852A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibre cellulosique et de type lyocell a degre de blanc reglable
TWI814782B (zh) 2018-03-06 2023-09-11 奧地利商蘭仁股份有限公司 溶劑紡絲之纖維素纖維
EP3536832A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibre lyocell présentant des propriétés de désintégration améliorées
EP3536831A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibre lyocell comportant une nouvelle section transversale
EP3536833A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibres de lyocell sans mannane
EP3536850A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Pulpe et articles en lyocell avec un taux en cellulose réduit
EP3536851A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibre lyocell présentant une tendance accrue à la fibrillation
EP3536853A1 (fr) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibre lyocell à formation de bouloche réduite

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US4096227A (en) * 1973-07-03 1978-06-20 W. L. Gore & Associates, Inc. Process for producing filled porous PTFE products
US4246221A (en) * 1979-03-02 1981-01-20 Akzona Incorporated Process for shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent
US4416698A (en) * 1977-07-26 1983-11-22 Akzona Incorporated Shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent and a process for making the article
AT391473B (de) * 1989-04-06 1990-10-10 Chemiefaser Lenzing Ag Monoaxial verstreckter formkoerper aus polytetrafluoraethylen und verfahren zu seiner herstellung
GB9022175D0 (en) * 1990-10-12 1990-11-28 Courtaulds Plc Treatment of fibres
AT395863B (de) * 1991-01-09 1993-03-25 Chemiefaser Lenzing Ag Verfahren zur herstellung eines cellulosischen formkoerpers
AT395862B (de) * 1991-01-09 1993-03-25 Chemiefaser Lenzing Ag Verfahren zur herstellung eines cellulosischen formkoerpers
GB9103297D0 (en) * 1991-02-15 1991-04-03 Courtaulds Plc Fibre production method
ATA53792A (de) * 1992-03-17 1995-02-15 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer formkörper, vorrichtung zur durchführung des verfahrens sowie verwendung einer spinnvorrichtung
GB9222059D0 (en) * 1992-10-21 1992-12-02 Courtaulds Plc Fibre treatment
TW257811B (fr) * 1993-04-21 1995-09-21 Chemiefaser Lenzing Ag
GB9313128D0 (en) * 1993-06-24 1993-08-11 Courtaulds Fibres Ltd Fabric treatment
AT399729B (de) * 1993-07-01 1995-07-25 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer fasern sowie vorrichtung zur durchführung des verfahrens und deren verwendung

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10043297B4 (de) * 2000-09-02 2005-12-08 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. Verfahren zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen

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BR9405504A (pt) 1999-09-08
DK0659219T3 (da) 1996-06-17
US5543101A (en) 1996-08-06
HK1000327A1 (en) 1998-02-27
DE4494808D2 (de) 1995-09-21
RO113875B1 (ro) 1998-11-30
ZA944768B (en) 1995-02-16
JP2768831B2 (ja) 1998-06-25
NO950865L (no) 1995-03-06
UA29456C2 (uk) 2000-11-15
KR0173007B1 (ko) 1999-02-18
AU7221394A (en) 1995-02-06
CZ288757B6 (cs) 2001-08-15
GR3019296T3 (en) 1996-06-30
PH30806A (en) 1997-10-17
YU40994A (sh) 1996-10-09
CZ54695A3 (en) 1995-10-18
FI951057A0 (fi) 1995-03-07
GB2284383A (en) 1995-06-07
SI0659219T1 (fr) 1997-10-31
ES2085187T3 (es) 1996-05-16
GB9503084D0 (en) 1995-04-05
HU9500591D0 (en) 1995-04-28
ATA134893A (de) 1995-12-15
EP0659219A1 (fr) 1995-06-28
JPH08501356A (ja) 1996-02-13
CA2142111A1 (fr) 1995-01-19
BG99431A (bg) 1996-01-31
AU668655B2 (en) 1996-05-09
HU214034B (en) 1997-12-29
DE59400105D1 (de) 1996-03-14
ID913B (id) 1996-09-11
RU95110578A (ru) 1997-05-27
RU2120505C1 (ru) 1998-10-20
CN1090249C (zh) 2002-09-04
FI951057A (fi) 1995-03-07
WO1995002082A1 (fr) 1995-01-19
ATE133724T1 (de) 1996-02-15
HRP940392B1 (en) 1998-06-30
CN1112367A (zh) 1995-11-22
SK29095A3 (en) 1995-08-09
HUT72230A (en) 1996-04-29
GB2284383B (en) 1997-04-09
AT401271B (de) 1996-07-25
HRP940392A2 (en) 1996-08-31
TR28323A (tr) 1996-04-17
PE696A1 (es) 1996-02-26
YU48582B (sh) 1998-12-23
PL307852A1 (en) 1995-06-26
NO950865D0 (no) 1995-03-06

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