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WO2002018682A1 - 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

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Publication number
WO2002018682A1
WO2002018682A1 PCT/DE2001/003334 DE0103334W WO0218682A1 WO 2002018682 A1 WO2002018682 A1 WO 2002018682A1 DE 0103334 W DE0103334 W DE 0103334W WO 0218682 A1 WO0218682 A1 WO 0218682A1
Authority
WO
WIPO (PCT)
Prior art keywords
cellulose
solution
spinning
speed
crosslinking agent
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.)
Ceased
Application number
PCT/DE2001/003334
Other languages
German (de)
English (en)
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
Priority to DE50109092T priority Critical patent/DE50109092D1/de
Priority to EP01967050A priority patent/EP1315856B1/fr
Priority to AU2001287542A priority patent/AU2001287542A1/en
Publication of WO2002018682A1 publication Critical patent/WO2002018682A1/fr
Anticipated expiration legal-status Critical
Ceased 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 from cellulose 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 are added dispersed at elevated temperature in a reactor, with removal of water and shear in 0 a homogeneous solution with 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 Spinning nozzle feeds and deforms, c) the solution jet is transported through a non-precipitating medium with further deformation, and d) the cellulose thread or the yarn filament precipitates in a precipitation bath, separates it from the precipitation bath via a deflecting element and washes in a multi-stage aftertreatment , dries and crosslinked if necessary.
  • EP 0 430 926, EP 0 494 852, EP 0 756 025 and WO 94/28 210 describe certain nozzles with different spinning capillary geometry and arrangement.
  • WO 96/20 300 deals with the distance between two spinning capillaries and the path between spinning capillary and deflection 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 different forms of treating the thread family in the gap between the spinneret and the precipitation bath with air having different water contents.
  • EP 0 659 219 describes the production of a cellulose fiber with a lower tendency to fibrillation, in that an empirical formula of spinneret hole diameter, spinning mass flow, titer, width of the air gap and moisture content of the blown air should not exceed a value of 10.
  • a lower tendency to fibrillation is to be achieved by the fact that the blowing air contains aliphatic alcohols and in EP 0 853 146 by the precipitation taking place in two or more stages.
  • the object of the present invention is to create a method with an improved thread-forming process which captures all the relevant variables for thread-forming in a relationship and thus allows a targeted adjustment of fiber / filament properties based on a solution with a defined cellulose concentration, molecular weight and molecular weight distribution.
  • the fibers spun according to the invention are intended to allow subsequent crosslinking without significant embrittlement.
  • ⁇ D is the expansion viscosity in Pas
  • s the expansion speed in s "1 , T 10 the fineness of the material to be spun
  • Fiber in dtex v a the withdrawal speed in m / min, p L the density of the solution in g / cm 3 , c Ce ⁇ . the cellulose concentration of the spinning solution in%, D E inlet diameter and D A outlet 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 spinning in the air gap, ie the ratio of take-off and spraying speed.
  • the expansion viscosity for a spinning solution is determined by the cellulose concentration, the molar mass and molar mass distribution and only changes with the temperature and elongation speed.
  • the rate of expansion of the overall process follows
  • Concentration also depends on its degree of solvation or state of solution and only after complete solvation, i.e. long release time reaches a minimum final value. Practical spinning solutions are often incompletely solvated for spinning and thus simulate a higher value for the zero shear viscosity or the molar mass. [Cf. Michels Ch. U. Meister F. "Das Textil” 51 (1997) 4 pp. 161-165 and Michels Ch. And Kosan B. "Chemical Fibers Intern.” 50 (2000) 12 pp. 556-561].
  • fibers are spun at a stretching speed 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 softening agent, a crosslinking agent and a crosslinking catalyst. After drying and crosslinking, a fiber with a significantly increased wet scrub resistance is obtained with only a slight change in the other fiber parameters.
  • filament yarns are spun at a stretching speed in the range 60-100 [l / s], the amine oxide is removed by washing in several stages, dried to a water content> 80% by means of a first heated roller duo and carried by piston diaphragm pumps driven by compressed air motors and spray nozzles onto the thread sheet a defined amount of a mixture of finishing agent and crosslinking agent, dries and crosslinks via a second heated roller duo.
  • a filament yarn with significantly increased wet scrub resistance is obtained.
  • the method for determining wet scrub resistance has been described in the literature [Mieck KP; Langner H.; Nechwatal A. "Melliand Textile Reports" 74 (1993) p.
  • the measure of wet abrasion resistance is the required number of revolutions of a roller of a certain geometry covered with a cellulose fabric, which leads to the breakage of a moistened fiber under defined tension.
  • the lyocell fibers have in Depending on their molar mass and orientation, a wet scrub resistance in the range between 10 and 50 scrubbing cycles. From the literature mentioned it also appears that there is sufficient wet scrub resistance if the fiber test results in> 340 scrubbing cycles.
  • fibers were produced with the following settings: fiber fineness 1.10 dtex
  • the filament sheet was washed, cut into stacks of 50 mm, finished and dried.
  • the test revealed the following fiber parameters:
  • Cotton-Linters-Zeil-fabric was pretreated enzymatically, pressed to a water content of 50% by mass, dispersed in 2593 g of NMMO with a water content of 25% and with heating, shearing and evaporation of 623 g of water in a homogeneous solution with a zero shear viscosity of 4108 Pas and a relaxation time of 4.9 s transferred at 85 ° C.
  • the particle analysis gave a filter value of 90.
  • the composition of the solution was 10.6 mass% cellulose, 77.8 mass% NMMO and 11.6 mass% water.
  • the cellulose mixture of the solution had a Cuoxam DP of 543 and a non-uniformity of 6.05.
  • the application was carried out once by spraying the fiber (B) predried to> 80% water and on the other hand by dipping and pressing using a roller duo (C).
  • the fiber test gave the following values:
  • 300 g eucalyptus pulp, enzymatically pretreated, pressed to a water content of 45 mass%, are dispersed in 2726 g NMMO with a water content of 30 mass% and with heating, shearing and evaporation of 772 g water in a homogeneous solution (density 1.178 g / cm 3 ) transferred 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, non-uniformity 5.9), 76.3 mass% NMMO and 11.7 mass% water.
  • the calculated elongation rate was 21.8 s "1.
  • the fiber was washed, finished and dried at 125 ° C. (A).
  • A a second series of tests the
  • the solution preparation (10.6% cellulose; density 1.16 g / cm 3 at 85 ° C) is carried out analogously to Example 2, the spinning at 84 ° C
  • the filaments were wound up as yarn with a fineness of 75 dtex f (58) (A).
  • the finish was applied using a precision pump and "fingers".
  • the finish contained 10 g / 1 Arkofix (commercial product from 0. AG) and 1 g / 1 magnesium sulfate (B) at the same time.
  • the test was carried out using the standard methods as filament yarn ( a, b) as well as after cutting into stacks as fiber A, 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)

Abstract

L'invention concerne un procédé de fabrication de fibres cellulosiques et de fils continus cellulosiques ayant des propriétés améliorées, à partir de cellulose, selon le procédé d'extrusion par voie sèche/humide avec des aminoxydes aqueux, en particulier N-méthyl-morpholine-N-oxyde, en tant que solvant. Ledit procédé consiste a) à disperser de la cellulose et de l'aminoxyde aqueux à température élevée dans un réacteur, avec déshydratation et cisaillement dans une solution homogène avec une durée de relaxation de 0,5 à 80 secondes à 85 DEG C, b) à amener cette solution dans au moins une filière et à déformer ladite solution, c) à transporter le filet de solution dans un milieu non précipitant avec déformation ultérieure, et d) à précipiter le fil cellulosique ou l'ensemble de fils cellulosiques dans un bain de précipitation, à séparer le fil d'un bain au moyen d'un organe de déviation, et à laver, aviver, sécher et éventuellement réticuler le fil dans un traitement ultérieur en plusieurs étapes. Au cours de l'étape a) on fabrique une solution avec un DP d'hydroxyde de cuprammonium de la cellulose >/= 450, on déforme cette solution en b) et en c) avec une vitesse d'extension (I), et le bain d'avivage de l'étape d) contient également un agent réticulant.
PCT/DE2001/003334 2000-09-02 2001-08-30 Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques Ceased WO2002018682A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE50109092T DE50109092D1 (de) 2000-09-02 2001-08-30 Verfahren zur herstellung von cellulosefasern und cellulose-filamentgarnen
EP01967050A EP1315856B1 (fr) 2000-09-02 2001-08-30 Procede de fabrication de fibres cellulosiques et de fils continus cellulosiques
AU2001287542A AU2001287542A1 (en) 2000-09-02 2001-08-30 Method for producing cellulose fibers and cellulose filament yarns

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10043297.2 2000-09-02
DE10043297A DE10043297B4 (de) 2000-09-02 2000-09-02 Verfahren zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen

Publications (1)

Publication Number Publication Date
WO2002018682A1 true WO2002018682A1 (fr) 2002-03-07

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE2001/003334 Ceased WO2002018682A1 (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 (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002048435A1 (fr) * 2000-12-13 2002-06-20 Thüringisches Institut für Textil-und Kunststoff-Forschung E.V. Procede de fabrication de corps profiles sans fin en cellulose
GB2389111B (en) * 2002-05-31 2006-08-02 Hyosung Corp Process of producing highly homogeneous cellulose solution
WO2009118262A1 (fr) * 2008-03-27 2009-10-01 Cordenka Gmbh Corps moulés cellulosiques
EP2185754A4 (fr) * 2007-09-07 2010-12-01 Kolon Inc Fibres filaments de fibres lyocell et câble pour pneu à base de cellulose
EP2589689A4 (fr) * 2010-06-30 2014-01-22 Kolon Inc Dope pour le filage de fibre cellulosique à haute ténacité, procédé pour la préparation de fibre de filament cellulosique à haute ténacité utilisant un tel dope, et procédé pour la préparation de fibre courte de fibre cellulosique à haute ténacité
US9751247B2 (en) 2011-09-02 2017-09-05 Aurotec Gmbh Extrusion method
EP3467162A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Filaments de lyocell ignifuge
EP3467163A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Étoffe de doublure de filaments lyocellulaires
EP3467161A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Procédé de production d'un filament de cellulose de type lyocell
WO2019068927A1 (fr) 2017-10-06 2019-04-11 Lenzing Aktiengesellschaft Filament lyocell ignifuge
EP3674454A1 (fr) 2018-12-28 2020-07-01 Lenzing Aktiengesellschaft Procédé de filament de cellulose

Families Citing this family (6)

* Cited by examiner, † Cited by third party
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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
EP3505659A1 (fr) * 2018-08-30 2019-07-03 Aurotec GmbH Procédé et dispositif de filage des filaments à déviation
EP3771755A1 (fr) * 2019-08-02 2021-02-03 Lenzing Aktiengesellschaft Procédé de fabrication de fibres discontinues lyocellulaires
CN120401037A (zh) * 2024-02-01 2025-08-01 中国纺织科学研究院有限公司 一种莱赛尔竹纤维的制备方法及莱赛尔竹纤维

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DE19954152A1 (de) * 1999-11-10 2000-07-20 Thueringisches Inst Textil Verfahren und Vorrichtung zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002048435A1 (fr) * 2000-12-13 2002-06-20 Thüringisches Institut für Textil-und Kunststoff-Forschung E.V. Procede de fabrication de corps profiles sans fin en cellulose
GB2389111B (en) * 2002-05-31 2006-08-02 Hyosung Corp Process of producing highly homogeneous cellulose solution
EP2185754A4 (fr) * 2007-09-07 2010-12-01 Kolon Inc Fibres filaments de fibres lyocell et câble pour pneu à base de cellulose
WO2009118262A1 (fr) * 2008-03-27 2009-10-01 Cordenka Gmbh Corps moulés cellulosiques
KR20100129293A (ko) * 2008-03-27 2010-12-08 코르덴카 게엠베하 셀룰로오스 성형체
KR101580115B1 (ko) 2008-03-27 2016-01-04 코르덴카 게엠베하 운트 코. 카게 셀룰로오스 성형체
EP2589689A4 (fr) * 2010-06-30 2014-01-22 Kolon Inc Dope pour le filage de fibre cellulosique à haute ténacité, procédé pour la préparation de fibre de filament cellulosique à haute ténacité utilisant un tel dope, et procédé pour la préparation de fibre courte de fibre cellulosique à haute ténacité
US9751247B2 (en) 2011-09-02 2017-09-05 Aurotec Gmbh Extrusion method
EP3467162A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Filaments de lyocell ignifuge
EP3467163A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Étoffe de doublure de filaments lyocellulaires
EP3467161A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Procédé de production d'un filament de cellulose de type lyocell
WO2019068927A1 (fr) 2017-10-06 2019-04-11 Lenzing Aktiengesellschaft Filament lyocell ignifuge
WO2019068922A1 (fr) 2017-10-06 2019-04-11 Lenzing Aktiengesellschaft Procédé de production de filament de cellulose de type lyocell
WO2019068468A1 (fr) 2017-10-06 2019-04-11 Lenzing Aktiengesellschaft Tissu de doublure en filaments lyocell
US11414786B2 (en) 2017-10-06 2022-08-16 Lenzing Aktiengesellschaft Cellulose filament process
US11686016B2 (en) 2017-10-06 2023-06-27 Lenzing Aktiengesellschaft Lyocell filament lining fabric
EP3674454A1 (fr) 2018-12-28 2020-07-01 Lenzing Aktiengesellschaft Procédé de filament de cellulose
WO2020136108A1 (fr) 2018-12-28 2020-07-02 Lenzing Aktiengesellschaft Procédé de production de filament de cellulose
US11898272B2 (en) 2018-12-28 2024-02-13 Lenzing Aktiengesellschaft Cellulose filament process

Also Published As

Publication number Publication date
DE10043297B4 (de) 2005-12-08
EP1315856A1 (fr) 2003-06-04
DE50109092D1 (de) 2006-04-27
CN1211509C (zh) 2005-07-20
ATE318947T1 (de) 2006-03-15
EP1315856B1 (fr) 2006-03-01
AU2001287542A1 (en) 2002-03-13
CN1449460A (zh) 2003-10-15
DE10043297A1 (de) 2002-03-21

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