EP0918894B1 - Verfahren zur herstellung cellulosischer fasern - Google Patents

Verfahren zur herstellung cellulosischer fasern Download PDF

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Publication number
EP0918894B1
EP0918894B1 EP98927999A EP98927999A EP0918894B1 EP 0918894 B1 EP0918894 B1 EP 0918894B1 EP 98927999 A EP98927999 A EP 98927999A EP 98927999 A EP98927999 A EP 98927999A EP 0918894 B1 EP0918894 B1 EP 0918894B1
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EP
European Patent Office
Prior art keywords
spinning
mass
cellulose
solution
molecular weight
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Expired - Lifetime
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EP98927999A
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German (de)
English (en)
French (fr)
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EP0918894A1 (de
Inventor
Eduard Mülleder
Christoph Schrempf
Hartmut Rüf
Wilhelm Feilmair
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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Application filed by Lenzing AG, Chemiefaser Lenzing AG filed Critical Lenzing AG
Priority to SI9830464T priority Critical patent/SI0918894T1/xx
Priority to AT98927999T priority patent/ATE239111T1/de
Publication of EP0918894A1 publication Critical patent/EP0918894A1/de
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—Spinnerettes
    • 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

Definitions

  • the present invention relates to a method for manufacturing cellulosic fibers of the Lyocell genus by processing a spinnable solution of cellulose in an aqueous tertiary amine oxide after the dry / wet spinning process.
  • NMMO N-methylmorpholine-N-oxide
  • Tertiary amine oxides have long been an alternative Known solvents for cellulose. From U.S. Patent 2,179,181 it is known, for example, that tertiary amine oxides are of high quality Chemical pulp can solve without derivatization and that from these solutions by precipitation cellulosic moldings, how fibers can be obtained. In the US PSen 3,447,939, 3,447,956 and 3,508,941 are other methods described for the production of cellulosic solutions, wherein as Solvents preferably cyclic amine oxides are used. In all of these processes, cellulose is made at elevated temperature physically solved.
  • EP-A-0 356 419 by the applicant describes a method described, preferably in a thin film treatment apparatus is carried out in which a suspension of crushed pulp in an aqueous tertiary amine oxide in the form of a thin layer spread over a Heating surface is transported, the surface of this thin layer is exposed to a vacuum. While transporting the suspension over the heating surface, water is evaporated and the cellulose can be brought into solution so that from the Film spuder a spinnable cellulose solution is discharged.
  • a method for spinning cellulose solutions is e.g. known from US-A-4 246 221. According to this procedure the spinning solution through a spinneret to filaments or threads extruded, which passed through an air gap into a precipitation bath in which the cellulose is precipitated. In the air gap the filaments are stretched, making the fiber more favorable physical properties, e.g. higher strength, can be awarded. By precipitating the cellulose in the Precipitation bath these physical properties are fixed, so that no further stretching is necessary. This method is commonly known as dry / wet spinning.
  • the freshly spun can Filaments in the air gap are cooled with air. Further will suggested the surface of the filaments with a precipitant wetting to reduce the risk that the Glue filaments together. Such wetting has however, the disadvantage that the cellulose on the filament surface is felled, which makes it more difficult to stretch adjust the fiber properties.
  • EP-A-0 648 808 describes a molding process a cellulose solution, the cellulosic components the solution a first component made of a cellulose with a Average degree of polymerization (DP) from 500 to 2000 and a second cellulose component with a DP less than 90% of the DP of the first component in the range from 350 to 900 included.
  • the weight ratio of the first for the second component should be 95: 5 to 50:50.
  • Applicant's WO 93/19230 improves the dry / wet spinning process and increases its productivity. This is brought about by a specific blowing with an inert cooling gas, the cooling being provided directly below the spinneret. In this way it is possible to greatly reduce the stickiness of the freshly extruded threads and thus to spin denser thread curtains, ie to use a spinneret with a high hole density, namely up to 1.4 holes / mm 2 , which naturally increases the productivity of the dry / Wet spinning can be increased considerably. Air with a temperature between -6 ° C and + 24 ° C is used to cool the freshly extruded threads.
  • the applicant's WO 95/02082 also describes a dry / wet spinning process. This method uses cooling air that has a temperature between 10 ° C and 60 ° C. The humidity of the cooling air supplied is between 20 g H 2 O and 40 g H 2 O per kilogram.
  • WO 95/01470 and WO 95/04173 by the applicant describe spinning processes in which a spinneret with a hole density of 1.59 holes / mm 2 or a spinneret with a total of 15048 holes is used.
  • the cooling air has a temperature of 21 ° C.
  • WO 94/28218 generally proposes the use of spinnerets with 500 to 100,000 holes.
  • the temperature of the cooling air is between 0 ° C and 50 ° C.
  • the person skilled in the art can see from this literature that the moisture is between 5.5 g H 2 O and 7.5 g H 2 O per kilogram of air. This creates a relatively dry climate in the air gap.
  • WO 96/17118 also deals with the climate in the air gap, it being determined that the climate should be as dry as possible, namely 0.1 g H 2 O to 7 g H 2 O per kilogram of air, with a relative humidity of less than 85%. 6 ° C to 40 ° C is suggested as the temperature for the cooling air.
  • the specialist therefore takes from this literature to keep the climate as dry as possible during spinning.
  • WO 96/20300 by the applicant describes, inter alia, the use of a spinneret with 28392 spinning holes.
  • the air in the air gap has a temperature of 12 ° C and a humidity of 5 g H 2 O per kilogram of air.
  • This literature also shows the tendency, particularly when using a nozzle with a greatly increased number of spinning holes, that is to say when spinning a relatively dense thread curtain, to keep the climate in the air gap rather dry and cool.
  • WO 96/21758 also deals with that to be set climate in the air gap, with a two-stage blowing with different cooling air is proposed and in the upper Area of the air gap with less humid and cooler air is blown.
  • the object of the invention is therefore to overcome these disadvantages eliminate and a process for making cellulosic Fibers of the Lyocell genus by processing a spinnable Solution of cellulose in an aqueous tertiary amine oxide to provide after the dry / wet spinning process, wherein a dense thread curtain can be spun and the blowing air still doesn't have to be dry.
  • a dense thread curtain can be spun and the blowing air still doesn't have to be dry.
  • the process should be carried out with good spinnability can be, the spinnability being so much the better is considered, the smaller the minimum achievable titer (see below).
  • the molecular weight is determined according to the chromatographic method described below.
  • cellulose molecules or other polymer molecules which, according to the chromatographic method described below, provide signals which correspond to a molecular weight of at least 5 ⁇ 10 5 are referred to as long-chain molecules.
  • the invention is based on the knowledge that the presence of long chain cellulose molecules and / or other polymers in the spinning solution in the specified concentration range Spinning behavior improved so that blowing air can be used, which need not be dry. This means that even when blowing very thick thread curtains good spinnability even in those areas of the thread curtain given, seen in the direction of blowing, are further out and therefore only with "used", i.e. to reach significantly warmed and humid blowing air are.
  • cellulose mixtures are preferred used which the specified in the spinning solution Have long-chain molecules content.
  • the tertiary amine oxide is N-methyl-morpholine-N-oxide best proven.
  • the invention further relates to the use of a spinnable solution of cellulose in an aqueous tertiary amine oxide, which solution between 0.05 mass% and 0.70 mass%, in particular between 0.10 and 0.55 mass%, and preferably between 0.15 and 0.45% by mass, based on the mass of the solution, of cellulose having a molecular weight of at least 5x10 5 , for the production of cellulosic fibers with a titer of at most 1 dtex.
  • the invention also relates to a cellulosic fiber of the Lyocell genus, which is characterized in that it is obtainable by the process according to the invention and between 0.25 and 7.0% by mass, in particular between 1.0 and 3.0% by mass, based on the mass of the cellulosic fiber, cellulose having a molecular weight of at least 5x10 5 .
  • the fiber according to the invention is preferred characterized in that they have a Titer of maximum 1 dtex.
  • Lyocell fibers with a titer of 1 dtex or less are described in WO 96/13071, the WO 97/35054 and WO 98/07911 mentioned.
  • Fiber is the staple fiber.
  • linear density is a critical quantity defined by the applicant and indicates the number of fibers per millimeter of thread curtain through which the blowing air flows.
  • the linear density can be calculated by dividing the total number of spinning holes in the nozzle by the so-called inflow area (in mm 2 ) and multiplying by the air gap length (in mm).
  • the "inflow surface” is the surface at right angles to the surface of the spinning bath, which is spanned by the air gap (in mm) and by the filament row first reached by the blowing gas and the associated "row of holes" of the spinneret and the line formed thereby (total length in mm) becomes.
  • Figure 3 shows schematically a rectangular nozzle 1 with spinning holes 2, from which the filaments 3 are extruded. The length the air gap is marked with "l". The filaments 3 occur after passing the air gap into the precipitation bath (not shown) a. In Fig. 3, the filaments are only in Air gap clearly drawn.
  • the inflow surface is the mathematical product of the length of the air gap "l" and the width "b" of the first row of filaments.
  • the molecular weight profile of a pulp can be determined using Gel permeation chromatography (GPC) can be obtained, whereby in the "Differential Weight Fraction" in [%] as a graph Ordinate against molecular weight [g / mol; logarithmic Application] is applied.
  • GPC Gel permeation chromatography
  • the size "differential weight fraction” describes the percentage frequency fraction of the molar mass fraction.
  • the measuring apparatus is implemented by means of measures familiar to the person skilled in the art calibrated.
  • the signals are evaluated according to Zimm, using the Zimm formula if necessary, set in the evaluation software.
  • FIG. 1a For the Viscokraft LV pulp (manufacturer: International Paper) the molecular weight profile in FIG. 1a is exemplary shown.
  • the diagram of Fig. 1a shows that this pulp largely consists of molecules with one There is a molecular weight of about 100,000 and that this Pulp practically no proportions (about 0.2%) with one Has molecular weight greater than 500,000.
  • Fig. 1b shows the molecular weight profile of the pulp Alistaple LD 9.2 (manufacturer: Western Pulp).
  • This pulp has a maximum molar mass frequency at around 200,000, and the graph also shows that this A high proportion (about 25%) of molecules with a pulp Has molecular weight greater than 500,000.
  • a spinning mass, who exclusively use such a pulp to 15 Contains% by mass, has about 4% (based on the mass of Solution; Degradation not taken into account during solution production) Cellulose molecules with a molecular weight of larger than 500,000 and therefore does not correspond to those who is used according to the invention.
  • 1c shows the molecular weight profile of a pulp mixture from 70% Viscokraft LV and 30% Alistaple LD 9.2. at this pulp mixture has a maximum of about 100,000, and the diagram also shows that this pulp mixture a proportion of about 7% of molecules with a molecular weight of more than 500,000.
  • a dope containing 15% of this mixture would - disregarding the degradation of the molecules during the Solution preparation - about 1% (based on the mass of the Solution) cellulose molecules with a molecular weight of greater than 500,000 included.
  • the cellulose molecules are subject to dissolution degradation in the aqueous amine oxide, so that the content of long chain molecules decreases and that a dope that is made from the mixture mentioned, a significant has a lower proportion of these long-chain molecules.
  • FIG. 1d shows the molecular weight profile created by means of GPC of the spinning mass immediately before Represents spun pulp. This spinning mass represents the cellulose solution immediately before spinning, contains only 0.4 mass% long-chain molecules and is thus a cellulose solution used according to the invention.
  • a pulp of the type Solucell 400 (manufacturer: Bacell SA, Brazil) has a molecular weight distribution, which for the production of a cellulose solution according to the invention suitable is.
  • the shredded pulp or a mixture of shredded Pulps are suspended in aqueous, 50% NMMO, into a kneader (Type: IKA laboratory kneader HKD-T; manufacturer: IKA laboratory technology) and impregnate for one hour calmly. Then, by heating the kneader a heating medium heated to 130 ° C and by reduction the pressure water is evaporated until the pulp is completely in Solution has gone.
  • a kneader Type: IKA laboratory kneader HKD-T; manufacturer: IKA laboratory technology
  • a spinning apparatus is used in plastics processing Common melt index device from Davenport used.
  • This device consists of a heatable, temperature-controllable Steel cylinder into which the spinning mass is poured becomes.
  • a piston loaded with a weight is the spinning mass by the at the bottom of the Steel cylinder attached spinneret that has a hole with a Has diameter of 100 microns, extruded.
  • the one placed in the spinning apparatus Spinning mass (cellulose content: 15%) extruded through the spinning hole and over an air gap 3 cm in length led an aqueous precipitation bath, deflected, over a godet deducted, which is provided behind the precipitation bath, and thereby stretched.
  • the spinning mass output through the nozzle is 0.030 g / min.
  • the spinning temperature is 80 ° C to 120 ° C.
  • the minimally spinnable is used to simulate the spinning behavior Titer taken. This is the maximum take-off speed (m / min) determined by the take-off speed so is increased for a long time until the thread breaks. That speed is noted and for the calculation of the titer see below Formula used. The higher this value, the more the spinning behavior or the spinnability is better.
  • the filaments in the air gap were blown through their entire length and at right angles to them.
  • the humidity the air was removed by means of a thermostat set.
  • the Pulp Viscokraft LV (manufacturer: International Paper Corp.), whose molecular weight profile is shown in Fig. 1a is a spinning mass made and at different Moistures are spun in the air gap and the maximum Take-off speed or the minimum spinnable titer determined.
  • the results are shown in Table 1.
  • the Pulp Alistaple LD 9.2 (manufacturer: Western Pulp), whose Molecular weight profile is shown in Fig. 1b, a Spinning mass produced and at different moisture levels in the Spun air gap and the maximum take-off speed or the minimum spinnable titer is determined. It was got a reverse result: the spinnability was at higher humidity in the air gap slightly better than lower Humid. However, the spinnability of such Spinning masses, as can be seen from the minimal titer, overall significantly worse, since the proportion is already too high is contained in high molecular weight components.
  • Fig. 2 shows the spinning behavior of cellulose solutions with varying proportions of long chain molecules, where as Ordinate the minimum titer (dtex) and as the abscissa the Concentration of the respective cellulose solution on cellulose molecules with a molecular weight of at least 500,000 is applied. The concentrations were just before determined by spinning.
  • the proportion of long chain molecules was determined by adding corresponding amounts of Alistaple LD 9.2 to Viscokraft LV set.
  • the cellulose concentration of the solution was in 15 mass% in all cases.
  • the spinning behavior was determined for each cellulose solution both at a humidity in the air gap of 30 g H 2 O (curve “a") and at 0 g H 2 O (dry) (straight line “b").
  • the range according to the invention is (0.05 to 0.70 Mass%).
  • Spinning the concentration range in dense thread curtains in which the humidity is practically none has a negative influence on the spinnability, so that complex air conditioning and conditioning of the blowing air unnecessary.
  • the cellulose solution which is 100% Viscokraft LV as a cellulose Material contained corresponded immediately before Do not spin a cellulose solution used according to the invention.
  • the cellulose solution which is 85% Viscokraft LV and 15% Alistaple LD 9.2 contained, corresponded directly to the Spinning a cellulose solution used according to the invention.
  • the friction of the fibers against each other during washing processes or at Finishing operations in the wet state was carried out by the following test simulated: 8 fibers with a length of 20 mm were with 4 ml Put water in a 20 ml vial and during 9 Hours in a laboratory shaker type RO-10 from Fa. Gehardt, Bonn (FRG) shaken at level 12. The Fibrillation behavior of the fibers was then under the Microscope by counting the number of fibrils per 0.276 mm fiber length assessed.
  • the following table shows the fibrillation determined according to the above regulation: Used pulp Titer (dtex) Blowing air humidity (g H 2 O / kg air) Number of fibrils 100% visco power LV 1.7 10 > 50 15% Alistaple LD 9.2 / 85% Viscokraft LV 1.7 10 24 15% Alistaple LD 9.2 / 85% Viscokraft LV 1.7 20 12
  • the table clearly shows that the tendency to fibrillation from cellulose solutions with the Fibers produced composition according to the invention is lower than with fibers made from cellulose solutions composition not according to the invention. Furthermore, it can be seen from the table that the Fibrillation tendency of from used according to the invention Cellulose solutions produced fibers will drop even further if air with higher humidity is used for blowing.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Inorganic Fibers (AREA)
EP98927999A 1997-06-17 1998-06-17 Verfahren zur herstellung cellulosischer fasern Expired - Lifetime EP0918894B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
SI9830464T SI0918894T1 (en) 1997-06-17 1998-06-17 Method for producing cellulose fibres
AT98927999T ATE239111T1 (de) 1997-06-17 1998-06-17 Verfahren zur herstellung cellulosischer fasern

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
AT0105397A AT405531B (de) 1997-06-17 1997-06-17 Verfahren zur herstellung cellulosischer fasern
AT1053/97 1997-06-17
AT105397 1997-06-17
PCT/AT1998/000151 WO1998058103A1 (de) 1997-06-17 1998-06-17 Verfahren zur herstellung cellulosischer fasern

Publications (2)

Publication Number Publication Date
EP0918894A1 EP0918894A1 (de) 1999-06-02
EP0918894B1 true EP0918894B1 (de) 2003-05-02

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EP98927999A Expired - Lifetime EP0918894B1 (de) 1997-06-17 1998-06-17 Verfahren zur herstellung cellulosischer fasern

Country Status (20)

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US (1) US6241927B1 (ko)
EP (1) EP0918894B1 (ko)
JP (1) JP3849062B2 (ko)
KR (1) KR100517273B1 (ko)
CN (1) CN1111617C (ko)
AT (2) AT405531B (ko)
AU (1) AU740994B2 (ko)
BR (1) BR9806227A (ko)
CA (1) CA2263183C (ko)
DE (1) DE59808154D1 (ko)
ES (1) ES2198717T3 (ko)
HK (1) HK1023152A1 (ko)
ID (1) ID21230A (ko)
MY (1) MY125882A (ko)
NO (1) NO315949B1 (ko)
PT (1) PT918894E (ko)
SI (1) SI0918894T1 (ko)
TW (1) TW544476B (ko)
WO (1) WO1998058103A1 (ko)
ZA (1) ZA985246B (ko)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6221487B1 (en) 1996-08-23 2001-04-24 The Weyerhauser Company Lyocell fibers having enhanced CV properties
US6235392B1 (en) 1996-08-23 2001-05-22 Weyerhaeuser Company Lyocell fibers and process for their preparation
AT408355B (de) * 2000-06-29 2001-11-26 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer fasern
EP1311718B1 (en) * 2000-08-03 2005-02-02 BBA Nonwovens Simpsonville, Inc. Process and system for producing multicomponent spunbonded nonwoven fabrics
WO2005001174A1 (en) * 2003-06-30 2005-01-06 Hyosung Corporation A solution containing cellulose dissolved in n-methylmorpholine-n-oxide and high tenacity lyocell multifilament using the same
CN1973065B (zh) * 2004-06-25 2012-03-28 东丽株式会社 干湿式纺纱用喷丝组件、纤维束制造装置及制造方法
KR100575378B1 (ko) * 2004-11-10 2006-05-02 주식회사 효성 셀룰로오스 섬유의 제조방법
KR100966111B1 (ko) * 2005-03-15 2010-06-28 주식회사 효성 셀룰로오스 멀티 필라멘트의 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
EP3385430A1 (en) * 2017-04-03 2018-10-10 Lenzing Aktiengesellschaft Optically transparent wet nonwoven cellulose fiber fabric
EP3674454A1 (en) 2018-12-28 2020-07-01 Lenzing Aktiengesellschaft Cellulose filament process

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US3447939A (en) 1966-09-02 1969-06-03 Eastman Kodak Co Compounds dissolved in cyclic amine oxides
US3447956A (en) 1966-09-02 1969-06-03 Eastman Kodak Co Process for strengthening swellable fibrous material with an amine oxide and the resulting material
US4144080A (en) 1977-07-26 1979-03-13 Akzona Incorporated Process for making amine oxide solution of cellulose
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SE445563B (sv) * 1984-11-19 1986-06-30 Berol Kemi Ab Sett att forbettra cellulosabaserade spinnlosningars processbarhet genom att en etylenoxidaddukt tillsettes
US5094690A (en) 1988-08-16 1992-03-10 Lenzing Aktiengesellschaft Process and arrangement for preparing a solution of cellulose
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
KR100297308B1 (ko) 1993-02-16 2001-10-24 나가이 야타로 성형용셀룰로오즈용액및이를사용하는성형방법
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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
AT401271B (de) 1993-07-08 1996-07-25 Chemiefaser Lenzing Ag Verfahren zur herstellung von cellulosefasern
AT402738B (de) 1993-07-28 1997-08-25 Chemiefaser Lenzing Ag Spinndüse
GB9421261D0 (en) * 1994-10-21 1994-12-07 Courtaulds Plc Non-woven fabrics
HU220367B (hu) 1994-12-02 2001-12-28 Akzo Nobel N.V. Eljárás cellulóz formatestek előállítására és cellulóz filamentből készült fonal
DE4444140A1 (de) 1994-12-12 1996-06-13 Akzo Nobel Nv Lösungsmittelgesponnene cellulosische Filamente
ATA239194A (de) 1994-12-22 1996-02-15 Chemiefaser Lenzing Ag Vorrichtung zur durchführung eines trocken-/nassspinnverfahrens
GB9500387D0 (en) 1995-01-10 1995-03-01 Courtaulds Fibres Ltd Manufacture of extruded articles
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ATE245214T1 (de) * 1996-11-21 2003-08-15 Toyo Boseki Fasern aus regenerierte zellulose und verfahren zu ihrer herstellung
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Also Published As

Publication number Publication date
SI0918894T1 (en) 2003-10-31
ID21230A (id) 1999-05-06
CN1236403A (zh) 1999-11-24
ATA105397A (de) 1999-01-15
KR20000068155A (ko) 2000-11-25
ZA985246B (en) 1999-01-08
AU740994B2 (en) 2001-11-22
JP3849062B2 (ja) 2006-11-22
WO1998058103A1 (de) 1998-12-23
CA2263183C (en) 2006-10-10
NO315949B1 (no) 2003-11-17
EP0918894A1 (de) 1999-06-02
HK1023152A1 (en) 2000-09-01
JP2000517009A (ja) 2000-12-19
US6241927B1 (en) 2001-06-05
NO990731D0 (no) 1999-02-17
CA2263183A1 (en) 1998-12-23
AU8002598A (en) 1999-01-04
CN1111617C (zh) 2003-06-18
TW544476B (en) 2003-08-01
ATE239111T1 (de) 2003-05-15
BR9806227A (pt) 2000-03-21
MY125882A (en) 2006-08-30
PT918894E (pt) 2003-08-29
ES2198717T3 (es) 2004-02-01
DE59808154D1 (de) 2003-06-05
KR100517273B1 (ko) 2005-09-27
NO990731L (no) 1999-02-17
AT405531B (de) 1999-09-27

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