EP1315856B1 - Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques - Google Patents

Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques Download PDF

Info

Publication number
EP1315856B1
EP1315856B1 EP01967050A EP01967050A EP1315856B1 EP 1315856 B1 EP1315856 B1 EP 1315856B1 EP 01967050 A EP01967050 A EP 01967050A EP 01967050 A EP01967050 A EP 01967050A EP 1315856 B1 EP1315856 B1 EP 1315856B1
Authority
EP
European Patent Office
Prior art keywords
solution
cellulose
spinning
elongation rate
filament
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
Application number
EP01967050A
Other languages
German (de)
English (en)
Other versions
EP1315856A1 (fr
Inventor
Christoph Michels
Birgit Kosan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Original Assignee
Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Thueringisches Institut fuer Textil und Kunststoff Forschung eV filed Critical Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Publication of EP1315856A1 publication Critical patent/EP1315856A1/fr
Application granted granted Critical
Publication of EP1315856B1 publication Critical patent/EP1315856B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • 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
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/12—Stretch-spinning methods

Definitions

  • the invention relates to a process for the production of cellulose fibers or cellulose filament yarns with improved properties of pulp by the dry wet extrusion process with aqueous amine oxides, in particular N-methyl-morpholine-N-oxide, as solvent, in which a) pulp and aqueous amine oxide at elevated Dissolved temperature in a reactor, transferred under dehydration and shear in a homogeneous solution having a zero shear viscosity in the range of 1000 - 8000 Pas and a relaxation time in the range of 0.5 - 80 seconds at 85 ° C, b) the solution at least one spinneret feeds and deformed, c) the solution jet is transported through a non-precipitating medium under further deformation and d) precipitates in a precipitation bath the cellulose filament or strand, separates via a deflecting element from the precipitation bath and washes in a multi-stage aftertreatment, aviviert, dries and optionally cross-linked ,
  • U.S. Patents 4,246,221 and 4,416,698 disclose dissolving cellulose in water-containing amine oxides, forming under low shear strain capillaries, distorting the solution jets in a large air gap, precipitating the cellulose through a aqueous amine oxide-containing spinning bath and stripping the cellulose filaments over a godet.
  • U.S. Patent No. 5,417,909 discloses a process which deforms the solution under medium to high shear in the spin capillaries, draws solution jets in a short air gap, precipitates the cellulose, and senses the yarns across a spinning cone and carries them cocurrently ,
  • EP 0 430 926, EP 0 494 852, EP 0 756 025 and WO 94/28 210 describe certain nozzles with different spin capillary geometry and arrangement.
  • WO 96/20 300 deals with the distance between two spinning capillaries and the path between spinning capillary and deflecting element in the precipitation bath.
  • EP 0 584 318, EP 0 671 492, EP 0 795 052, WO 94/28 218 and WO 96/21 758 describe the differentiated forms of treating the group of threads in the gap between spinneret and precipitation bath with air of different water content.
  • EP 0 659 219 describes the preparation of a cellulose fiber having a lower tendency to fibrillation, in that an empirical formula of spinneret orifice diameter, spinning mass flow, titer, width of the air gap and moisture content of the blowing air should not exceed a value of 10.
  • a lower fibrillation tendency is to be achieved in that the blow-in air contains aliphatic alcohols and in EP 0 853 146 in that the precipitation takes place in two or more stages.
  • the object of the present invention is to provide a method with an improved thread formation process, which records all relevant sizes for the thread formation in a relationship and thus allows a targeted adjustment of fiber / filament properties starting from a solution with defined cellulose concentration, molecular weight and molecular weight distribution.
  • the fibers spun according to the invention are intended to permit subsequent crosslinking without significant embrittlement.
  • ⁇ D is the extensional viscosity in Pas
  • ⁇ is the strain rate in s -1
  • T 10 is the fineness of the fiber to be spun in dtex
  • v a is the take-off speed in m / min
  • ⁇ L is the density of the solution in g / cm 3
  • c Cell . the cellulose concentration of the spinning solution in%
  • D E inlet diameter and D A exit diameter of the spinning capillary in cm 1 length of the spinning capillary in cm, a length of the air gap in cm and SV the spinning distortion in the air gap, ie the ratio of withdrawal and injection speed.
  • the extensional viscosity for a spinning solution is determined by the cellulose concentration, the molecular weight and molecular weight distribution, and changes only with the temperature and strain rate.
  • the zero-shear viscosity of the cellulose solutions at 85 ° C. is preferably 1000-8000 Pas during spinning to filaments and preferably 5000-40000 Pas during spinning into staple fibers.
  • the width of the viscosity range results from the fact that the experimentally accessible zero-shear viscosity of the cellulosic solutions, in addition to the molecular weight and
  • Concentration also depends on their degree of solvation or solution state and only at complete solvation. long release time reaches a minimum final value.
  • Practice-relevant spinning solutions are often solubilized in an unsatisfactorily solvated manner and thus simulate a higher value for the zero-shear viscosity or the molecular weight.
  • fibers are spun at a strain rate in the range between 15 and 40 [1 / s] and the fibers are treated in the last stage before drying with a solution which simultaneously contains a lubricant, a crosslinking agent and a crosslinking catalyst. After drying and crosslinking, a fiber is obtained with significantly increased wet rub resistance with only a small change in the other fiber parameters.
  • filament yarns are spun at a stretching speed in the range of 60-100 [1 / s], the amine oxide is removed by multi-stage washing, dried over a first heated roller pair to a water content> 80%, carried by piston diaphragm pumps driven by compressed air motors and spray nozzles a defined amount of a mixture of avivage and
  • Crosslinking agent on the group of threads dried and crosslinked via a second heated roller duo. This gives a filament yarn with significantly increased wet scrub resistance.
  • the lyocell fibers have a wet scrub resistance in the range of between 10 and 50 rubs. It is also apparent from the cited literature that sufficient wet abrasion resistance is present if the fiber test gives ⁇ 340 rubs.
  • the fiber was washed, refined and dried at 125 ° C (A).
  • the avivage liquor contained 5 g / l glyoxal and 0.5 g / l magnesium chloride (pH 6.7).
  • the application was carried out by spraying the fiber (B) predried to> 80% water and by dipping and pressing with roller duo (C).
  • 300 g of eucalyptus pulp, enzymatically pretreated, pressed to a water content of 45% by weight, are dispersed in 2726 g of NMMO with a water content of 30% by weight and heated, shearing and evaporating 772 g of water in a homogeneous solution (density 1.178 g / cm 3 ) with a zero shear viscosity of 5,081 Pas and a relaxation time of 6.0 s at 85 ° C.
  • the particle analysis showed a filter value of 76.
  • the composition of the solution was 12.0 mass% cellulose (Cuoxam DP 508, 5.67 ununiformity), 76.3 mass% NMMO and 11.7 mass% water.
  • the calculated strain rate was 21.8 s -1 .
  • the fiber was washed, refined and dried at 125 ° C (A).
  • the avivage liquor contained at the same time 7.5 g / l of an adduct of glyoxal and sodium bisulfite (B).
  • the filaments were spooled as yarn of fineness 75 dtex f (58) (A).
  • the application of the lubricant was done by precision pump and "finger".
  • the lubricant contained at the same time 10 g / l of Arkofix (commercial product of procurement AG) and 1 g / l of magnesium sulfate (B).

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)

Claims (9)

  1. Procédé de fabrication de fibres cellulosiques ou de filaments cellulosiques à partir de cellulose après le procédé d'extrusion par voie humide / séchage avec des oxydes d'amine aqueux, en particulier du N-méthylmorpholin-N-oxyde, dans lequel
    a) on disperse la cellulose et l'oxyde d'amine aqueux à haute température dans un réacteur mélangeur / pétrisseur et la transforme, avec élimination d'eau et cisaillement, en une solution homogène avec une durée de relaxation dans la plage de 0,5 à 80 secondes,
    b) on introduit la solution au moins dans une filière, et la déforme dans le ou les capillaires de filage à la vitesse d'extension εD,
    c) on véhicule la solution déformée par l'intermédiaire d'un milieu qui ne précipite pas, simultanément à une déformation supplémentaire à la vitesse d'extension εa,
    d) on réalise la régénération des fils cellulosiques ou de la nappe de fils cellulosiques dans un bain de régénération, les sépare du bain de régénération par transfert à l'aide d'une galette, on lave, le cas échéant blanchit, avive, sèche, le cas échant réticule ces derniers dans un dispositif de post-traitement à plusieurs étages, sous forme de fibres ou de filaments, puis enroule individuellement les filaments sous la forme de fil ou les regroupe pour obtenir un câble et les découpe afin d'obtenir des fibres coupées,

    caractérisé en ce que, à l'étape a), on produit une solution avec un DP (degré de polymérisation) Cuoxam (hydroxyde de cuprammonium) de la cellulose ≥ 450, on déforme cette solution à l'étape b) et c) avec une vitesse d'extension ε ˙ D , a = ε ˙ D ⋅ ε ˙ a ≤ 160 [ s − 1 ]
    Figure imgb0012
    et en ce que le bain d'avivage à l'étape d) contient, le cas échéant, parallèlement, un agent de réticulation.
  2. Procédé selon la revendication 1, caractérisé en ce que la vitesse d'extension dans le canal d'alimentation satisfait à la formule : ε ˙ D = 19 , 1 ⋅ 10 − 5 T 10 ⋅ v a ρ L ⋅ c Cell . ⋅ D E 2 ⋅ l ⋅ e [ ln ( D E D A ) 2 − 1 ]
    Figure imgb0013
    où T10 est le titre de la fibre / filament en dtex, va la vitesse de déroulement en m/min, ρL la masse volumique de la solution de filage en g/cm3, ccell. est la concentration en cellulose de la solution en %, 1 la longueur du canal d'alimentation en cm et DE ou DA le diamètre de l'entrée ou respectivement de la sortie des capillaires de filage.
  3. Procédé selon la revendication 1, caractérisé en ce que la vitesse d'extension entre la sortie des capillaires de filage et l'entrée du bain de régénération satisfait à la formule ε ˙ a = 19 , 1 ⋅ 10 − 5 T 10 ⋅ v a ρ L ⋅ c Cell . ⋅ D A 2 ⋅ a e ln S V − 1
    Figure imgb0014
    où a est la longueur de la trajectoire d'étirage en cm, et Sv l'étirage de filage, à savoir le rapport entre la vitesse de déroulement et la vitesse d'extrusion.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que, lors du filage des fibres, la vitesse d'extension εD,a se trouve de préférence dans la plage de 4 à 40 s-1.
  5. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que, lors du filage des nappes de filaments, la vitesse d'extension εD,a se trouve de préférence dans la plage de 40 à 120 s-1.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que le bain d'avivage contient également un agent de réticulation bifonctionnel ou polyfonctionnel de type dialdéhyde, de préférence du glyoxal et / ou ses dérivés, et la valeur de pH du bain d'avivage est ≤ 9.
  7. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que l'agent de réticulation est un adduit composé de glyoxal et de bisulfite de sodium.
  8. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce qu'on applique le contenu du bain de post-traitement, par l'intermédiaire d'unités de dosage, constituées de filières et de pompes à diaphragme à haute fréquence, sous la forme d'un brouillard finement divisé, sur la nappe de fils et, le cas échéant, on extrait par pression un excédent possible par l'intermédiaire d'un dispositif à cylindres.
  9. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce qu'on applique l'agent de réticulation ou l'avivage contenant l'agent de réticulation par l'intermédiaire d'une unité constituée d'une ou plusieurs pompes de précision et d'une ou plusieurs vis de dosage.
EP01967050A 2000-09-02 2001-08-30 Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques Expired - Lifetime EP1315856B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10043297A DE10043297B4 (de) 2000-09-02 2000-09-02 Verfahren zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen
DE10043297 2000-09-02
PCT/DE2001/003334 WO2002018682A1 (fr) 2000-09-02 2001-08-30 Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques

Publications (2)

Publication Number Publication Date
EP1315856A1 EP1315856A1 (fr) 2003-06-04
EP1315856B1 true EP1315856B1 (fr) 2006-03-01

Family

ID=7654765

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01967050A Expired - Lifetime EP1315856B1 (fr) 2000-09-02 2001-08-30 Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques

Country Status (6)

Country Link
EP (1) EP1315856B1 (fr)
CN (1) CN1211509C (fr)
AT (1) ATE318947T1 (fr)
AU (1) AU2001287542A1 (fr)
DE (2) DE10043297B4 (fr)
WO (1) WO2002018682A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4007826B1 (fr) 2019-08-02 2023-06-07 Lenzing Aktiengesellschaft Procédé de fabrication de fibres discontinues lyocellulaires

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10062083B4 (de) * 2000-12-13 2008-04-10 Ostthüringische Materialprüfgesellschaft Für Textil Und Kunststoffe Mbh Verfahren zur Herstellung von Celluloseendlosformkörpern
KR100611890B1 (ko) * 2002-05-31 2006-08-11 주식회사 효성 고균질 셀룰로오스 용액의 제조방법
WO2009031868A2 (fr) * 2007-09-07 2009-03-12 Kolon Industries, Inc. Fibres filaments de fibres lyocell et câble pour pneu à base de cellulose
ES2402442T3 (es) * 2008-03-27 2013-05-03 Cordenka Gmbh & Co. Kg Cuerpos celulósicos conformados
US20130101843A1 (en) * 2010-06-30 2013-04-25 Kolon Industries, Inc. Dope for spinning lyocell, method for preparing lyocell filament fiber, and method for preparing lyocell staple fiber using the same
EP2565303A1 (fr) * 2011-09-02 2013-03-06 Aurotec GmbH Procédé d'extrusion
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
CN105088415B (zh) * 2015-06-15 2018-01-05 中国科学技术大学 一种湿纺用氧化石墨烯溶液及其制备方法以及一种石墨烯纤维及其制备方法
CN105316780A (zh) * 2015-10-27 2016-02-10 湖州大成纺织有限公司 一种荧光增白扁平丝生产工艺
EP3467162A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Filaments de lyocell ignifuge
US20200240043A1 (en) 2017-10-06 2020-07-30 Lenzing Aktiengesellschaft Flame retardant lyocell filament
EP3467161A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Procédé de production d'un filament de cellulose de type lyocell
EP3467163A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Étoffe de doublure de filaments lyocellulaires
EP3505659A1 (fr) * 2018-08-30 2019-07-03 Aurotec GmbH Procédé et dispositif de filage des filaments à déviation
EP3674454A1 (fr) 2018-12-28 2020-07-01 Lenzing Aktiengesellschaft Procédé de filament de cellulose

Family Cites Families (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE670504C (de) * 1933-06-03 1939-01-19 I G Farbenindustrie Akt Ges Verfahren zum Knitterfestmachen von Textilfasern oder -geweben
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
AT397392B (de) * 1989-11-29 1994-03-25 Chemiefaser Lenzing Ag Spinndüse
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
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
US5417909A (en) * 1992-06-16 1995-05-23 Thuringisches Institut Fur Textil- Und Kunststoff-Forschung E.V. Process for manufacturing molded articles of cellulose
US5652001A (en) * 1993-05-24 1997-07-29 Courtaulds Fibres Limited Spinnerette
MY115308A (en) * 1993-05-24 2003-05-31 Tencel Ltd Spinning cell
AT401271B (de) * 1993-07-08 1996-07-25 Chemiefaser Lenzing Ag Verfahren zur herstellung von cellulosefasern
AT401393B (de) * 1994-09-05 1996-08-26 Chemiefaser Lenzing Ag Verfahren zur herstellung von cellulosefasern
CA2204412A1 (fr) * 1994-11-03 1996-05-17 Frank Meister Corps de moulage en cellulose regeneree et son procede de production
WO1996017118A1 (fr) * 1994-12-02 1996-06-06 Akzo Nobel N.V. Procede de production de corps cellulosiques façonnes et fil realise a partir de filaments cellulosiques
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
AT402642B (de) * 1995-08-18 1997-07-25 Chemiefaser Lenzing Ag Cellulosefaser cellulosefaser
AT402740B (de) * 1995-10-06 1997-08-25 Chemiefaser Lenzing Ag Cellulosefaser
DE19600572B4 (de) * 1996-01-09 2005-03-10 Fraunhofer Ges Forschung Verfahren zur Herstellung von Cellulosefasern und die mit diesem Verfahren hergestellten Fasern
GB9611252D0 (en) * 1996-05-30 1996-07-31 Courtaulds Fibres Holdings Ltd Fibre manufacture
EP0853146A3 (fr) * 1997-01-09 1999-03-24 Akzo Nobel N.V. Procédé de production de fibres cellulosiques et fibres cellulosiques
DE19954152C2 (de) * 1999-11-10 2001-08-09 Thueringisches Inst Textil Verfahren und Vorrichtung zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4007826B1 (fr) 2019-08-02 2023-06-07 Lenzing Aktiengesellschaft Procédé de fabrication de fibres discontinues lyocellulaires

Also Published As

Publication number Publication date
AU2001287542A1 (en) 2002-03-13
WO2002018682A1 (fr) 2002-03-07
EP1315856A1 (fr) 2003-06-04
CN1449460A (zh) 2003-10-15
DE10043297A1 (de) 2002-03-21
DE10043297B4 (de) 2005-12-08
ATE318947T1 (de) 2006-03-15
DE50109092D1 (de) 2006-04-27
CN1211509C (zh) 2005-07-20

Similar Documents

Publication Publication Date Title
EP1315856B1 (fr) Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques
EP1763596B1 (fr) Procede pour produire des corps façonnes en cellulose
DE69913117T2 (de) Zusammensetzung für die herstellung von lyocellfasern
DE69716092T2 (de) Lyocellfasern und verfahren zu ihrer herstellung
EP0659219B1 (fr) Fibres cellulosiques
EP0574870B1 (fr) Procédé de fabrication d'articles moulés en cellulose
DE102005029793A1 (de) Vliesstoffe, Verfahren zu deren Herstellung sowie deren Verwendung
AT401393B (de) Verfahren zur herstellung von cellulosefasern
EP1379713B1 (fr) Procede et dispositif de fabrication de fibres cellulosiques et de filaments continus cellulosiques
EP0797696B2 (fr) Procede de fabrication de fibres cellulosiques
WO2006125484A1 (fr) Procede et dispositif pour couper des fils contenant du nmmo et des fibres coupees de cellulose
DE4219658C2 (de) Verfahren zur Herstellung von Cellulosefasern -filamenten und -folien nach dem Trocken-Naßextrusionsverfahren
WO1997033020A1 (fr) Procede de production de fibres cellulosiques
EP1268888B1 (fr) Procede et dispositif pour produire des fibres de cellulose et des fils continus de cellulose
EP1358371B1 (fr) Procede de fabrication de corps profiles sans fin en cellulose
WO1997004148A1 (fr) Fibres de cellulose
EP0944750B1 (fr) Fibres de polyacrylonitrile hautement resistantes et a module eleve, leur procede de fabrication et leur utilisation
DE2720087A1 (de) Verfahren zum herstellen von viskosefaeden und nach dem verfahren hergestellte faeden
AT405532B (de) Cellulosische mikrofaser
EP0645479A1 (fr) Fibres de polyacrylonitrile ayant une haute tenacité et un haut module, procédé de leur préparation et leur utilisation
EP0178293B1 (fr) Procédé de production de fils et de fibres de cellulose et dispositif pour la mise en oeuvre du procédé

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20030402

AK Designated contracting states

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

AX Request for extension of the european patent

Extension state: AL LT LV RO SI

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.

Effective date: 20060301

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060301

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060301

Ref country code: IE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060301

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: GERMAN

REF Corresponds to:

Ref document number: 50109092

Country of ref document: DE

Date of ref document: 20060427

Kind code of ref document: P

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20060427

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060601

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060601

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060612

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060801

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20060831

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20060831

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20060831

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20060831

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
REG Reference to a national code

Ref country code: IE

Ref legal event code: FD4D

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20061204

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

EN Fr: translation not filed
BERE Be: lapsed

Owner name: THURINGISCHES INSTITUT FUR TEXTIL- UND KUNSTSTOFF

Effective date: 20060831

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070309

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060602

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20060830

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060301

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060301

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060301

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20080814

Year of fee payment: 8

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20080821

Year of fee payment: 8

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20090830

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20090830

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20090830

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20200819

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 50109092

Country of ref document: DE