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EP1129241A1 - Procede de production de fibres cellulosiques - Google Patents

Procede de production de fibres cellulosiques

Info

Publication number
EP1129241A1
EP1129241A1 EP99947074A EP99947074A EP1129241A1 EP 1129241 A1 EP1129241 A1 EP 1129241A1 EP 99947074 A EP99947074 A EP 99947074A EP 99947074 A EP99947074 A EP 99947074A EP 1129241 A1 EP1129241 A1 EP 1129241A1
Authority
EP
European Patent Office
Prior art keywords
wash
washing
baths
bath
fibers
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.)
Granted
Application number
EP99947074A
Other languages
German (de)
English (en)
Other versions
EP1129241B1 (fr
Inventor
Wilhelm Feilmair
Heinrich Firgo
Johann Männer
Bruno Mangeng
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.)
Lenzing AG
Original Assignee
Lenzing AG
Chemiefaser Lenzing AG
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 Lenzing AG, Chemiefaser Lenzing AG filed Critical Lenzing AG
Priority to AT99947074T priority Critical patent/ATE258238T1/de
Publication of EP1129241A1 publication Critical patent/EP1129241A1/fr
Application granted granted Critical
Publication of EP1129241B1 publication Critical patent/EP1129241B1/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
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06—Washing or drying
    • 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 invention relates to a method for producing cellulosic fibers from solutions of cellulose in an aqueous tertiary amine oxide.
  • a mixture of a tertiary amine oxide and water is particularly suitable as an organic solvent for the production of Lyocell fibers or other shaped bodies.
  • the amine oxide used is predominantly N-methylnorpholine-N-oxide (NMMO).
  • NMMO N-methylnorpholine-N-oxide
  • Other suitable amine oxides are in the
  • EP-A 0 553 070 Process for producing cellulosic foils from a
  • PCT-WO 92/14871 describes a process for washing fibers produced by the amine oxide process.
  • the continuous fibers, which have not yet been cut, are passed through several washing baths in the form of a fiber cable.
  • the fibers are cut into staple fibers only in a later process stage.
  • PCT-WO 92/14871 emphasizes that the pH of the wash baths must be below 8.5, since otherwise the resulting fibers have an increased tendency to fibrillation.
  • PCT-WO 92/14871 indicates that it is known from the viscose process for the production of cellulosic fibers that one of the washing stages is designed as a bleaching stage in which an alkaline pH prevails. However, it is known in the amine oxide process that all washing liquids for the recovery of
  • NMMO are circulated. In this context it is also from the
  • PCT-WO 92/14871 known that the washing baths are in communication with each other and fresh washing liquid is added in the last washing bath and countercurrent to
  • Amine oxide processes do not implement bleaching calls in the washing liquid circuit. It is only possible to provide a bleaching bath independently of the washing baths connected to one another. So if in the following of
  • Wash baths is meant, it does not mean such an independent bleach bath.
  • Another problem with washing the fibers made by the amine oxide process is that adhering NMMO must be removed entirely from the fiber.
  • the object of the present invention is to provide a method in which the NMMO can be washed out of the fiber with as little effort as possible.
  • This object is achieved by a process for the production of cellulosic fibers from solutions of cellulose in an aqueous tertiary amine oxide, the extruded fibers being passed over a precipitation bath and cut and the cut fibers in the form of a fleece being passed over several washing baths and then dried, which Wash baths are in communication with each other and fresh wash liquid is added to the last wash bath and is carried in countercurrent to the direction of transport of the nonwoven fabric to the first wash bath, and which process is characterized in that the pH value of each of the wash baths is kept higher than 8.5 becomes.
  • alkaline pH a pH of more than 8.5
  • the invention relates to so-called "washing stretches" of several interconnected wash baths.
  • the pH of the wash liquid of each of the interconnected wash baths must be kept higher than 8.5. Baths that are not in contact with the wash baths Connected and are therefore not fed with the same washing liquid, such as separate treatment or bleach baths, are not included in the present invention.
  • An advantageous embodiment of the method according to the invention is characterized in that the pH of the wash baths is kept between 9 and 11.
  • the pH of the wash baths is furthermore preferably kept between 10 and 11. It can be seen that when the NMMO is washed out of the fibers in the first wash baths, the greatest amount of NMMO is removed from the fibers. In the subsequent wash baths, only small amounts of NMMO are present in the fibers, which, however, are more difficult to wash out.
  • An alkaline pH of the washing liquid causes an increase in the rate at which NMMO is washed out, particularly in these subsequent baths.
  • the pH in the wash baths can advantageously be adjusted by adding basic buffering substances.
  • the addition of sodium hydroxide solution is particularly preferred.
  • the required amount of sodium hydroxide solution which is determined by process parameters such as the pH of the nonwoven or the moisture in the nonwoven can be easily determined by the person skilled in the art on the basis of the particular circumstances.
  • the amount added is regulated in a simple manner on the basis of the pH of the wash baths.
  • the sodium hydroxide solution can only be metered into one of the wash baths or at several points in the laundry. It can be seen that the addition of alkali to the wash baths has no negative influence on the subsequent process steps, such as cleaning the wash baths and recovering the solvent.
  • nonwoven fabric is pressed off after leaving a wash bath before entering the following wash bath. This largely prevents carryover of washing water contaminated with NMMO into the following washing stage.
  • the temperature of the wash water is preferably about 20 ° C to 90 ° C.
  • the washing baths can also be designed such that washing liquid is sprayed onto the fleece.
  • the total liquor ratio of the washing liquid to the nonwoven fabric is advantageously 1.5: 1 to 40: 1.
  • 1 schematically denotes a method for washing a nonwoven fabric from freshly spun cut lyocell fibers.
  • the nonwoven (10) is e.g. on a sieve belt (not shown) through the various wash baths (in the figure 1 there are 5 wash baths).
  • various wash baths in the figure 1 there are 5 wash baths.
  • the wash water circulates in the respective baths, and the rate of circulation within a bath may be higher than the rate of supply of the fresh one
  • the direction of transport of the nonwoven fabric is fed to the upstream wash bath.
  • nonwoven fabric is rolled using pairs of rollers, e.g. the pair of rollers (11,
  • Wash bath is further fed to the precipitation bath or the cleaning and recovery of NMMO.
  • the fleece was pressed to a water content of approximately 200%. After the last washing bath, the fleece was pressed to a water content of approximately 100% and then dried.
  • Example 2 The procedure was as in Example 1, but 0.1M NaOH was added in the course of the fourth wash bath in such a way that a pH of approximately 11 resulted in the feed of the third wash bath.
  • the amount of NMMO washed out per wash bath was determined in both experiments. This extent is defined by the discharge factor f, which follows the following
  • ci is the concentration of NMMO on the fiber when entering the wash bath
  • c 2 is the concentration of NMMO on the fiber when leaving the wash bath.
  • a higher value for the discharge factor f means a more complete washing out of the NMMO in the wash bath in question.
  • a comparison of the values shows that the NMMO content of the fibers within a wash bath can be reduced to a greater extent using the process according to the invention. This applies in particular to the last wash baths, in which removal of the low residual NMMO content is particularly difficult. With the method according to the invention, a complete removal of the NMMO is thus possible with significantly fewer wash baths and thus with lower costs.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)
  • Paper (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

L'invention concerne un procédé de production de fibres cellulosiques à partir de solutions de cellulose dans un oxyde d'amine tertiaire aqueux. Les fibres extrudées passent dans un bain de régénération puis sont coupées, avant de passer, sous forme de non tissé, dans plusieurs bains de lavage. Elles sont ensuite séchées. Les bains de lavage communiquent les uns avec les autres, un liquide de lavage frais étant introduit dans le dernier bain de lavage et acheminé dans le sens opposé au sens de transport non tissé, jusqu'au premier bain de lavage. Ce procédé est caractérisé en ce que le pH de chacun des bains de lavage est maintenu à une valeur supérieure à 8,5.
EP99947074A 1998-09-29 1999-09-28 Procede de production de fibres cellulosiques Expired - Lifetime EP1129241B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT99947074T ATE258238T1 (de) 1998-09-29 1999-09-28 Verfahren zur herstellung cellulosischer fasern

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT161498 1998-09-29
AT0161498A AT406588B (de) 1998-09-29 1998-09-29 Verfahren zur herstellung cellulosischer fasern
PCT/AT1999/000229 WO2000018991A1 (fr) 1998-09-29 1999-09-28 Procede de production de fibres cellulosiques

Publications (2)

Publication Number Publication Date
EP1129241A1 true EP1129241A1 (fr) 2001-09-05
EP1129241B1 EP1129241B1 (fr) 2004-01-21

Family

ID=3517237

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99947074A Expired - Lifetime EP1129241B1 (fr) 1998-09-29 1999-09-28 Procede de production de fibres cellulosiques

Country Status (11)

Country Link
US (1) US6645409B2 (fr)
EP (1) EP1129241B1 (fr)
KR (1) KR20010075371A (fr)
CN (1) CN1143011C (fr)
AT (1) AT406588B (fr)
AU (1) AU6066899A (fr)
BR (1) BR9914108A (fr)
DE (1) DE59908380D1 (fr)
ID (1) ID28499A (fr)
TW (1) TW577941B (fr)
WO (1) WO2000018991A1 (fr)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT410319B (de) * 2001-07-25 2003-03-25 Chemiefaser Lenzing Ag Celluloseschwamm und verfahren zu dessen herstellung
WO2004015563A1 (fr) * 2002-08-09 2004-02-19 Intel Corporation Mecanisme de commande a co-processeur multimedia comprenant des instructions d'alignement ou de radiodiffusion
DE102004007617B4 (de) * 2004-02-17 2007-02-08 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung eines Vliesstoffes, Vliesstoff und dessen Verwendung
US7693817B2 (en) * 2005-06-29 2010-04-06 Microsoft Corporation Sensing, storing, indexing, and retrieving data leveraging measures of user activity, attention, and interest
KR100769973B1 (ko) * 2006-12-28 2007-10-25 주식회사 효성 수세 공정 특성을 가진 산업용 셀룰로오스 멀티필라멘트의제조 방법 수세 공정
AT504649B1 (de) * 2007-07-11 2008-07-15 Chemiefaser Lenzing Ag Vorrichtung und verfahren zur behandlung einer fasermasse
AT505904B1 (de) * 2007-09-21 2009-05-15 Chemiefaser Lenzing Ag Cellulosesuspension und verfahren zu deren herstellung
AT507051B1 (de) 2008-06-27 2015-05-15 Chemiefaser Lenzing Ag Cellulosefaser und verfahren zu ihrer herstellung
AT519489B1 (de) * 2016-10-21 2021-11-15 Chemiefaser Lenzing Ag Verfahren und Vorrichtung zum Herstellen von Vliesen auf Cellulosebasis, die direkt aus Lyocell-Spinnlösung gebildet werden
KR101972271B1 (ko) * 2018-09-05 2019-04-24 박한수 인조 모발용 원사를 제조하는 방법 및 장치
EP3828320A1 (fr) 2019-11-26 2021-06-02 Lenzing Aktiengesellschaft Lavage à contre-courant
CN112593305A (zh) * 2020-12-04 2021-04-02 四川辉腾科技股份有限公司 一种芳纶ⅲ纤维纺丝水洗装置及其使用方法
WO2025150879A1 (fr) * 2024-01-09 2025-07-17 코오롱인더스트리 주식회사 Matériau lyocell, filtre pour article à fumer, article à fumer et leurs procédés de fabrication

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
DE3536537A1 (de) 1985-10-12 1987-04-16 Wolff Walsrode Ag Verfahren zur reinigung von produkten aus regenerierter cellulose
GB9103297D0 (en) 1991-02-15 1991-04-03 Courtaulds Plc Fibre production method
AT396930B (de) 1992-01-23 1993-12-27 Chemiefaser Lenzing Ag Aminoxide
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
US5585052A (en) * 1994-08-10 1996-12-17 The Dow Chemical Company Process for the preparation of polybenzazole staple fiber
AT402741B (de) 1995-10-13 1997-08-25 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer fasern
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
GB9614679D0 (en) * 1996-07-12 1996-09-04 Courtaulds Fibres Holdings Ltd Manufacture of fibre
GB9615431D0 (en) * 1996-07-23 1996-09-04 Courtaulds Fibres Holdings Ltd Fibre manufacture

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0018991A1 *

Also Published As

Publication number Publication date
CN1143011C (zh) 2004-03-24
US6645409B2 (en) 2003-11-11
DE59908380D1 (de) 2004-02-26
EP1129241B1 (fr) 2004-01-21
KR20010075371A (ko) 2001-08-09
BR9914108A (pt) 2001-06-12
ATA161498A (de) 1999-11-15
AT406588B (de) 2000-06-26
ID28499A (id) 2001-05-31
CN1320176A (zh) 2001-10-31
AU6066899A (en) 2000-04-17
US20020008331A1 (en) 2002-01-24
TW577941B (en) 2004-03-01
WO2000018991A1 (fr) 2000-04-06

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