EP0811087B1 - Procede et dispositif de production de fibres de cellulose - Google Patents

Procede et dispositif de production de fibres de cellulose Download PDF

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Publication number
EP0811087B1
EP0811087B1 EP96942981A EP96942981A EP0811087B1 EP 0811087 B1 EP0811087 B1 EP 0811087B1 EP 96942981 A EP96942981 A EP 96942981A EP 96942981 A EP96942981 A EP 96942981A EP 0811087 B1 EP0811087 B1 EP 0811087B1
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EP
European Patent Office
Prior art keywords
filaments
precipitating agent
cellulose
process according
air gap
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
EP96942981A
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German (de)
English (en)
Other versions
EP0811087A1 (fr
Inventor
Heinrich Firgo
Hartmut Rüf
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
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Publication date
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Publication of EP0811087A1 publication Critical patent/EP0811087A1/fr
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Publication of EP0811087B1 publication Critical patent/EP0811087B1/fr
Anticipated expiration legal-status Critical
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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
    • 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
    • D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
    • 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 manufacturing cellulosic fibers, in which a solution of cellulose in a tertiary amine oxide in the warm state to filaments is spun, which is guided through an air gap and then brought into contact with a precipitant, to precipitate the cellulose, the filaments being exerted subtracted from a force and stretched in the air gap, which Force is exerted with the precipitant by the Precipitant is allowed to flow in the direction in which the filaments are pulled off and the filaments with the Precipitants are brought into contact.
  • the invention relates also an apparatus for performing the method.
  • tertiary amine oxides Can solve cellulose and that from these solutions through Precipitation cellulosic moldings can be obtained.
  • a A method for producing such solutions is, for example known from EP-A-0 356 419. According to this publication is first a suspension of cellulose in an aqueous prepares tertiary amine oxide. The amine oxide contains up to 40 Mass% water. The aqueous cellulose suspension is heated and water is drawn off under reduced pressure until the cellulose goes into solution. The process can be carried out in one Thin film treatment apparatus are carried out.
  • a spinning process is known from DD-A-271 534, according to which the freshly spun filaments with precipitant in Be brought into contact, which are allowed to flow in the direction into which the filaments are drawn.
  • From DE-C - 195 12 053 is also a method for Manufacture of cellulosic fibers known in which the freshly extruded filaments into one on predetermined Accelerated speed, at least approximately in the direction of extruded filaments introduced laminar flowing precipitation bath become. The filaments are drawn off from a spool.
  • JP-A-7 268 718 describes a method and an apparatus for wet spinning a Cellulose solution in which a precipitation liquid is allowed to flow down in the form of a column is left while the spinning solution comes from a below the outlet for the Precipitation bath solution arranged spinneret at an angle in the direction of the precipitation liquid let flow and is taken down by this.
  • air is not just air such, but any gas or gas mixture which means the Filaments is inert towards and spinning on others Way doesn't bother. Accordingly, another can be in the "air gap” Gas is present as air.
  • the object of the present invention is a method of the type mentioned at the outset so that a high Output can be achieved and highly concentrated, highly viscous Cellulose solutions can be processed.
  • the process according to the invention for the production of cellulosic Fibers in which a solution of cellulose in a tertiary Amine oxide is spun into filaments in the warm state, which passed through an air gap and then with a Precipitating agents are brought into contact with the cellulose fell, the filaments being pulled off by exerting a force and stretched in the air gap, what force with the Precipitant is exercised by the precipitant in the Flow in the direction in which the filaments are drawn and the filaments are in contact with the precipitant brought, is characterized in that the Precipitant at the time when it with the Filaments are brought into contact at a speed that is at least as large as, and is in particular greater than the withdrawal speed of the Filaments.
  • the invention is based on the finding that highly viscous Cellulose solutions with cellulose concentrations of at least 12 % By mass without mechanical stretching device, e.g. a Discharge godet, so only with that of the flowing Precipitant kinetic energy transferred to the filaments can be stretched.
  • the filaments are so-called injector, in which precipitant that the Filaments accelerated, injected with a pressure that is above the ambient pressure.
  • the withdrawal speed is obtained in a known manner from the desired titer of the filaments, the concentration of the Cellulose solution and the ejection of the cellulose solution.
  • the filaments are preferably wetted with precipitant before them with the flowing precipitant, which has the power to Pulling on it exercises be brought into contact.
  • the Precipitant with which the filaments can be wetted be the same precipitant with which on the filaments the stretching force is exerted. But it can also be a be different.
  • the filaments in the air gap by blowing be cooled by a cooling gas, the cooling immediately after spinning is done.
  • the blowing can be damp Air can be made.
  • the invention also relates to a method for producing a Spunbond, which is characterized in that the cellulosic fibers produced according to the invention into one Fleece are laid, which is consolidated.
  • the fleece can be consolidated by treatment with a water jet become. But it can also be solidified advantageously by it with an aqueous solution of a tertiary amine oxide, which Cellulose can dissolve, soaked to the cellulose to dissolve superficially, and by the soaked fleece is then pressed at elevated temperature, after which the Solution of the tertiary amine oxide from the pressed fleece is washed out.
  • a tertiary amine oxide which Cellulose can dissolve, soaked to the cellulose to dissolve superficially, and by the soaked fleece is then pressed at elevated temperature, after which the Solution of the tertiary amine oxide from the pressed fleece is washed out.
  • the invention also relates to a device for carrying out the Method according to the invention, which device comprises: a opening for receiving precipitants and filaments, one Channel that communicates with the opening and in which the Filaments are guided, which device thereby is characterized in that the channel in an acceleration range flows into which the filaments with a precipitant be accelerated by a feeder in the Acceleration range opens, with respect to atmospheric pressure increased pressure is introduced.
  • the invention further relates to a spinning device for Implementation of the amine oxide process after Dry / wet spinning process with a spinneret, a feeder for cooling gas and the above device.
  • 1 is a heatable one (heating not shown) Designated spinneret, which with the line 2 Spinning mass 3, i.e. warm cellulose solution with a temperature from about 100 ° C to 120 ° C.
  • the pump 4 is used for Dosing the spinning mass and setting the for the Extrude required pressure.
  • the from the spinneret 1 over the spin holes 16 are extruded filaments 5 with a Inert gas 6, preferably air, cooled, which over the Gas nozzles 7 onto the filaments 5 leaving the spinneret 1 is directed. This blowing can be done with spinnerets be worked which have a high hole density without that the filaments stick together during the Spinning comes.
  • the filaments 5 are guided into the channel 9 of the injector 17 and finally get into an acceleration range 10 of the Injector 17, in which the filaments with quickly down in The precipitant flowing in the direction of the diffuser 11 come into contact, whereby the cellulose is precipitated.
  • the Filaments accelerated.
  • the one used for acceleration Precipitant is fed into the injector 17 via the feed 14 pressed.
  • the filaments with a higher Speed pulled down as it spins from the spinneret 1 be delivered later. This causes a stretching of the Filaments.
  • the drawn filaments pass through the diffuser 11 from the injector 17 and can, for example, on a Sieve (not shown) are stored.
  • the leadership of the Filaments through the injector 17 is not shown in FIG. 1 shown.
  • the air gap extends from the underside of the spinneret 1 to the end of channel 9, i.e. to the mouth of channel 9 in the acceleration range 10.
  • the length of the channel 9 is not limited and can also be shorter than shown in Figure 1 is.
  • FIG. 2 shows a preferred embodiment of the Device according to the invention shown.
  • Device parts that have already been described in FIG. 1 named with the same reference numbers.
  • the filaments 5 extruded from the spinneret 1 enter a Device which essentially has an injector part 18, on which a kind of spinning funnel 19 is placed.
  • the mechanical connection of the injector part 18 to the spinning funnel 19 can e.g. be made by screwing.
  • the filaments 5 extruded from the spinneret 1 pass over an air gap, which is determined by the distance of the underside of the Spinneret 1 defined by the surface of the precipitant 15 is, in the precipitant 15 of the spinning funnel 19, by channel 9a and finally enter the Acceleration range 10 of the injector 18, in which the Filaments flowing rapidly down towards diffuser 11 Precipitating agents are accelerated.
  • Precipitating agents are accelerated.
  • precipitant used is in the feed 14 in the Injector 18 pressed.
  • the spinning funnel 19 there is a feed 12 for Precipitant pumped into the cone 8 via the channel 13 becomes. Care should be taken to ensure that the amounts of precipitant, which are fed via the feeders 12 and 14 to the spinning funnel 19 or discharged from the injector 18 via the diffuser 11, are coordinated so that the desired in the air gap Stretching is achieved and at the same time a decrease in the Liquid level 15 and thus an increase in Air gap is prevented.
  • a spinnable cellulose solution with a cellulose content of 12% (NMMO: 77%; H 2 O: 11%) was prepared in a heatable and evacuable stirred kettle made from sulfite pulp and aqueous NMMO. This solution was extruded at 130 ° C. from a spinneret with 888 holes (hole diameter: 80 ⁇ m) to form filaments.
  • the air gap was 22 mm.
  • Precipitant was added to feed 14 in an amount of 1008 Injected 1 / hour.
  • the precipitant speed was about 378 in the acceleration area 10 at the exit of the channel 9a m / minute, whereby a stretching or warping of 9.9 is achieved has been.
  • a draw of 9.9 means that the filaments are drawn off at a speed which is 9.9 times the speed at which the filaments leave the spinneret and enter the air gap at which they are drawn.
  • the fibers produced had a titer of 1.30 dtex.
  • Example 1 The process described in Example 1 was carried out, but the precipitant injection and precipitant speed given in the table below were selected and the stretching also given in the table was achieved.
  • Precipitant Stretching Titer (dtex) injection speed Ex. 2 792 l / h 396 m / min 5.3 2.45
  • Ex. 3 828 l / h 414 m / min 6.9 1.87
  • the filament strand produced in Example 2 was run onto a screen belt to form a nonwoven with a basis weight of 40 g / m 2 .
  • the liquid permeability of this fleece was measured with a LISTER device according to EDANA (European Disposables and Nonwovens Association) standard 150.2-93 (methodology: A certain amount (5 ml) of the test liquid (0.9% NaCl solution) is brought onto the fleece at a constant outlet speed (the time for the removal of this liquid through the fleece is measured electronically). The average of 10 measurements was 1.47 sec.

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  • 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)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Nonwoven Fabrics (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Claims (11)

  1. Procédé pour la préparation de fibres de cellulose, dans lequel une solution de cellulose dans un oxyde d'amine tertiaire est filée à chaud en filaments qui sont passés dans un interstice d'air et ensuite mis en contact avec un agent de précipitation pour faire précipiter la cellulose, les filaments étant extraits par l'action d'une force et étirés dans l'interstice d'air, laquelle force est exercée par l'agent de précipitation en faisant s'écouler l'agent de précipitation dans la direction suivant laquelle les filaments sont extraits et les filaments sont mis en contact avec l'agent de précipitation,
       caractérisé en ce qu'au moment auquel l'agent de précipitation est amené en contact avec les filaments, on le fait s'écouler à une vitesse qui est au moins aussi élevée, et qui est en particulier plus élevée, que la vitesse d'extraction des filaments.
  2. Procédé selon la revendication 1, caractérisé en ce que les filaments sont mouillés par l'agent de précipitation avant d'être mis en contact avec l'agent de précipitation en écoulement qui exerce sur eux la force d'extraction.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que les filaments sont refroidis dans l'interstice d'air par soufflage d'un gaz de refroidissement, le refroidissement étant entrepris immédiatement après le filage.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que comme oxyde d'amine tertiaire, on utilise un N-oxyde de N-méthylmorpholine.
  5. Procédé selon la revendication 1, caractérisé en ce que la solution à filer présente une concentration en cellulose d'au moins 12% en poids, et de préférence de 13 à 15% en poids.
  6. Procédé pour la préparation d'un feutre filé, caractérisé en ce que les fibres de cellulose préparées à l'aide du procédé selon l'une ou plusieurs des revendications 1 à 5 sont disposées en un feutre qui est renforcé.
  7. Procédé selon la revendication 6, caractérisé en ce que le feutre est renforcé en l'imprégnant d'une solution aqueuse d'un oxyde d'amine tertiaire apte à solubiliser de la cellulose, pour solubiliser la cellulose superficielle, et en pressant ensuite le feutre imprégné à une température plus élevée, suite à quoi la solution d'amine tertiaire est essorée du feutre pressé.
  8. Dispositif en vue de la mise en oeuvre du procédé selon l'une des revendications de 1 à 7, comportant une ouverture (8) de réception d'agent de précipitation (15) et de filaments (5), un canal (9a) communiquant avec l'ouverture (8) et dans lequel les filaments (5) sont passés, caractérisé en ce que le canal (9a) débouche dans une zone d'accélération (10) dans laquelle les filaments (5) sont accélérés par un agent de précipitation qui est introduit à une pression supérieure à la pression atmosphérique par une amenée (14) qui débouche dans la zone d'accélération (10).
  9. Dispositif de filage en vue de la mise en oeuvre du procédé de filage sec/humide, comportant une filière de filage (1), une amenée (7) de gaz de refroidissement (6) et un dispositif selon la revendication 8.
  10. Utilisation d'un injecteur qui présente:
    un canal (9) dans lequel des filaments de cellulose venant d'être extrudés sont passés,
    une zone d'accélération (10) dans laquelle le canal (9) débouche de telle sorte que les filaments puissent être amenés dans la zone d'accélération, et
    une amenée (14) d'agent de précipitation, laquelle amenée (14) débouche dans la zone d'accélération (10), de telle sorte que de l'agent de précipitation puisse être amené dans la zone d'accélération (10),
       en vue de la mise en oeuvre du procédé selon l'une des revendications 1 à 7.
  11. Feutre filé préparé en disposant en un feutre des fibres de cellulose préparées par le procédé selon l'une ou plusieurs des revendications 1 à 5, et en renforçant le feutre à l'aide d'un jet d'eau.
EP96942981A 1995-12-27 1996-12-20 Procede et dispositif de production de fibres de cellulose Expired - Lifetime EP0811087B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
AT2107/95 1995-12-27
AT2107/99 1995-12-27
AT0210795A AT402947B (de) 1995-12-27 1995-12-27 Verfahren zur herstellung cellulosischer fasern sowie vorrrichtung zur durchführung des verfahrens
PCT/AT1996/000260 WO1997024476A1 (fr) 1995-12-27 1996-12-20 Procede et dispositif de production de fibres de cellulose

Publications (2)

Publication Number Publication Date
EP0811087A1 EP0811087A1 (fr) 1997-12-10
EP0811087B1 true EP0811087B1 (fr) 1999-01-20

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EP96942981A Expired - Lifetime EP0811087B1 (fr) 1995-12-27 1996-12-20 Procede et dispositif de production de fibres de cellulose

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EP (1) EP0811087B1 (fr)
JP (1) JPH11501371A (fr)
CN (1) CN1181788A (fr)
AT (2) AT402947B (fr)
AU (1) AU1185797A (fr)
BR (1) BR9607047A (fr)
CA (1) CA2213221A1 (fr)
DE (1) DE59601184D1 (fr)
ES (1) ES2129992T3 (fr)
NO (1) NO973763D0 (fr)
WO (1) WO1997024476A1 (fr)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6235392B1 (en) 1996-08-23 2001-05-22 Weyerhaeuser Company Lyocell fibers and process for their preparation
US6221487B1 (en) 1996-08-23 2001-04-24 The Weyerhauser Company Lyocell fibers having enhanced CV properties
CN1061106C (zh) * 1997-12-09 2001-01-24 宜宾丝丽雅集团有限公司 溶剂法纤维素纤维制造方法
AT406386B (de) 1998-07-28 2000-04-25 Chemiefaser Lenzing Ag Verfahren und vorrichtung zur herstellung cellulosischer formkörper
DE10025231A1 (de) 2000-05-22 2000-11-02 Lurgi Zimmer Ag Verfahren zum Extrudieren eines Endlosformkörpers
DE10025230A1 (de) * 2000-05-22 2000-11-02 Lurgi Zimmer Ag Verfahren zum Extrudieren eines Endlosformkörpers
DE10060876B4 (de) * 2000-12-07 2006-03-09 Zimmer Ag Ausfällvorrichtung für eine Spinnanlage
JP4593370B2 (ja) * 2005-06-02 2010-12-08 帝人テクノプロダクツ株式会社 乾湿式紡糸装置
AT503625B1 (de) 2006-04-28 2013-10-15 Chemiefaser Lenzing Ag Wasserstrahlverfestigtes produkt enthaltend cellulosische fasern
WO2007124522A1 (fr) * 2006-04-28 2007-11-08 Lenzing Aktiengesellschaft Produit non-tisse obtenu par fusion-soufflage
ES2625035B1 (es) * 2015-12-18 2018-06-21 Universidad De Extremadura Producción de chorros capilares viscoelásticos mediante enfocamiento gaseoso
EP3470557A1 (fr) * 2017-10-12 2019-04-17 Lenzing Aktiengesellschaft Dispositif de filage et procédé destiné à rattacher le fil à un dispositif de filage
CN110424423B (zh) * 2019-08-22 2022-02-08 深圳市如茵生态环境建设有限公司 纤维丝喷丝系统
CN116334778B (zh) * 2023-05-26 2023-07-21 吉林富博纤维研究院有限公司 一种高性能pan基碳纤维原丝的制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT962284B (it) * 1971-08-30 1973-12-20 Asahi Chemical Ind Procedimento per la manifattura di tessuto non tessuto a filamenti continui con il metodo di filatura ad umido sotto tensione
DD271534B5 (de) * 1988-04-26 2002-07-11 Thueringisches Inst Textil Verfahren zur Verspinnung von Polymerloesungen
PL285328A1 (en) * 1989-05-31 1991-01-28 Chemiefaser Lenzing Ag Apparatus for and method of expsing fibre cables to treatment with a liquid
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
JPH07268718A (ja) * 1994-03-29 1995-10-17 Asahi Chem Ind Co Ltd 再生セルロース繊維の湿式紡糸法

Also Published As

Publication number Publication date
DE59601184D1 (de) 1999-03-04
CN1181788A (zh) 1998-05-13
ATE176011T1 (de) 1999-02-15
EP0811087A1 (fr) 1997-12-10
AU1185797A (en) 1997-07-28
ATA210795A (de) 1997-02-15
NO973763L (no) 1997-08-15
NO973763D0 (no) 1997-08-15
AT402947B (de) 1997-09-25
JPH11501371A (ja) 1999-02-02
WO1997024476A1 (fr) 1997-07-10
CA2213221A1 (fr) 1997-07-10
ES2129992T3 (es) 1999-06-16
BR9607047A (pt) 1997-12-30

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