EP0811087B1 - Method for the production of cellulose fibres and device for carrying out the method - Google Patents

Method for the production of cellulose fibres and device for carrying out the method 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
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EP96942981A
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German (de)
French (fr)
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EP0811087A1 (en
Inventor
Heinrich Firgo
Hartmut Rüf
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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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)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Abstract

The invention concerns a method of producing cellulose fibres, the method calling for a warm solution of cellulose in a tertiary-amine oxide to be spun into filaments which are passed across an air gap and then brought into contact with a precipitating agent in order to precipitate the cellulose, the filaments being drawn off by the action of a force which stretches them in the air gap. The force is exerted by the precipitating agent by virtue of the fact that the precipitating agent is allowed to flow in the direction in which the filaments are to be drawn off and brought into contact with the precipitating agent. The method is characterized in that, when the precipitating agent is brought into contact with the filaments, it is allowed to flow at a speed which is at least as great as the speed at which the filaments are drawn off. The invention also concerns a device for carrying out the method.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung cellulosischer Fasern, bei welchem eine Lösung von Cellulose in einem tertiären Aminoxid in warmem Zustand zu Filamenten versponnen wird, welche durch einen Luftspalt geführt und anschließend mit einem Fällungsmittel in Kontakt gebracht werden, um die Cellulose zu fällen, wobei die Filamente durch Ausüben einer Kraft abgezogen und im Luftspalt verstreckt werden, welche Kraft mit dem Fällungsmittel ausgeübt wird, indem das Fällungsmittel in die Richtung strömen gelassen wird, in welche die Filamente abgezogen werden und die Filamente mit dem Fällungsmittel in Kontakt gebracht werden. Die Erfindung betrifft auch eine Vorrichtung zur Durchführung des Verfahrens.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.

Aus der US-PS 2,179,181 ist bekannt, daß tertiäre Aminoxide Cellulose zu lösen vermögen und daß aus diesen Lösungen durch Fällung cellulosische Formkörper gewonnen werden können. Ein Verfahren zur Herstellung derartiger Lösungen ist beispielsweise aus der EP-A - 0 356 419 bekannt. Gemäß dieser Veröffentlichung wird zunächst eine Suspension von Cellulose in einem wässerigen tertiären Aminoxid bereitet. Das Aminoxid enthält bis zu 40 Masse-% Wasser. Die wässerige Cellulose-Suspension wird erhitzt, und unter Druckverminderung wird so lange Wasser abgezogen, bis die Cellulose in Lösung geht. Das Verfahren kann in einem Dünnschichtbehandlungsapparat durchgeführt werden.From US-PS 2,179,181 it is known that 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.

Aus der DE-A - 28 44 163 und der DD-A - 218 121 ist bekannt, daß zur Herstellung von Cellulosefasern oder Cellulosefolien zwischen Spinndüse und Fällungsmittel ein Luftspalt gelegt wird, in welchem die extrudierten Fasern verstreckt werden. Diese Verstreckung ist notwendig, da nach Kontakt der geformten Spinnlösung mit dem wässerigen Fällungsmittel eine Verstreckung der Filamente sehr erschwert ist. Im Fällungsmittel wird die im Luftspalt eingestellte Faserstruktur fixiert. From DE-A - 28 44 163 and DD-A - 218 121 it is known that for the production of cellulose fibers or cellulose films between An air gap is placed in the spinneret and precipitant which the extruded fibers are stretched. This Stretching is necessary because after contact the molded Spinning solution with the aqueous precipitant a stretching the filaments is very difficult. In the precipitant the Air gap adjusted fiber structure fixed.

Im Luftspalt besteht jedoch die Gefahr, daß die noch nicht koagulierten Einzelfilamente aufgrund ihrer extrem hohen Klebrigkeit aneinander haften bzw. miteinander verschmelzen und somit ein Faserspinnen unmöglich machen. Die Verklebungsgefahr ist naturgemäß umso größer, je länger die Strecke zwischen Düsenplatte und Fällungsmitteloberfläche (Luftspalt) ist. Aus der WO 93/19230 ist bekannt, daß mit einem dichten Filamentverband bei langem Luftspalt versponnen werden kann, wenn die warme, geformte Spinnlösung vor dem Einbringen in das Fällungsmittel gekühlt wird, wobei die Kühlung unmittelbar nach dem Formen durch Anblasen mit einem Kühlgas vorgenommen wird.However, there is a risk in the air gap that it is not yet coagulated single filaments due to their extremely high Stickiness or stick together and making fiber spinning impossible. The risk of sticking is naturally the greater the longer the distance between Nozzle plate and precipitant surface (air gap). From the WO 93/19230 is known to have a dense filament dressing can be spun with a long air gap if the warm, shaped spinning solution before introduction into the precipitant is cooled, with cooling immediately after molding Blowing with a cooling gas is made.

Aus der DD-A - 271 534 ist ein Spinnverfahren bekannt, gemäß welchem die frisch gesponnenen Filamente mit Fällungsmittel in Kontakt gebracht werden, welches in die Richtung strömen gelassen wird, in welche die Filamente abgezogen werden.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.

Aus der DE-C - 195 12 053 ist ein ebenfalls ein Verfahren zum Herstellen von cellulosischen Fasern bekannt, bei welchem die frisch extrudierten Filamente in ein auf vorbestimmte Geschwindigkeit beschleunigtes, zumindest in etwa in Richtung der extrudierten Filamente laminar fließendes Fällbad eingeführt werden. Die Filamente werden von einer Spule abgezogen.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.

Die JP-A - 7 268 718 beschreibt ein Verfahren und eine Vorrichtung zum Naßspinnen einer Celluloselösung, bei dem eine Fällflüssigkeit in Form einer Säule nach unten fließen gelassen gelassen wird, während die Spinnlösung aus einer unterhalb des Auslasses für die Fällbadlösung angeordneten Spinndüse in einem Winkel in Richtung der Fällflüssigkeit fließen gelassen und von dieser nach unten mitgenommen wird.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.

Für die Zwecke der vorliegenden Beschreibung und der vorliegenden Patentansprüche soll der Ausdruck "Luft" nicht nur Luft als solche, sondern jedes Gas oder Gasgemisch bedeuten, welches den Filamenten gegenüber inert ist und das Verspinnen auch auf andere Weise nicht stört. Demgemäß kann im "Luftspalt" auch ein anderes Gas vorhanden sein als Luft.For the purposes of this description and the present Claims, the term "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.

Ein Verfahren der eingangs beschriebenen Art ist aus der EP-A - 0 574 870 bekannt. Dieses Verfahren wird mit einem sogenannten Spinntrichter durchgeführt, in welchem mit Hilfe eines flüssigen, strömenden Fällungsmittels ein Verzug der frisch extrudierten Filamente erreicht wird. Die Strömung des Fällungsmittels wird dabei durch die Schwerkraft hervorgerufen. Nachteilig ist bei diesem Verfahren, daß nur relativ niedrigviskose Celluloselösungen, die noch dazu eine relativ geringe Cellulosekonzentration von nur 7,8 Masse-%, 6,1 Masse-% bzw. 10,5 Masse-% aufweisen, versponnen werden können. Aus wirtschaftlicher Sicht sind derartig geringe Cellulosekonzentrationen unbefriedigend, da diese eine geringe Kapazität der Lösungsherstellung und hohe Eindampfkosten bei der Aufarbeitung des gebrauchten Fällungsmittels bedingen.A method of the type described in the opening paragraph is known from EP-A - 0 574,870. This procedure is called a Spinning funnel carried out in which with the help of a liquid, flowing precipitant a delay of the freshly extruded Filaments is reached. The flow of the precipitant will thereby caused by gravity. The disadvantage is this process that only relatively low viscosity Cellulose solutions that are also relatively small Cellulose concentration of only 7.8% by mass, 6.1% by mass and 10.5, respectively Have mass%, can be spun. For more economical Visible are such low cellulose concentrations unsatisfactory as this has a low capacity of Solution preparation and high evaporation costs during processing of the used precipitant.

Eine wirtschaftliche Faserherstellung mit hohen Produktionsraten erfordert jedoch das Verarbeiten von Spinnmassen, die eine höhere Cellulosekonzentration aufweisen. Außerdem soll der Spinnmasseausstoß möglichst hoch sein. Ein derartiges Verfahren kann aber mit dem bekannten Spinntrichter nicht durchgeführt werden, da dieser dazu in unzweckmäßiger Größe gebaut werden müßte.An economical fiber production with high production rates however, requires the processing of spinning masses which are higher Have cellulose concentration. In addition, the Spinning mass emissions should be as high as possible. Such a process but can not be carried out with the known spinning funnel because these are built to an inappropriate size ought to.

Die vorliegende Erfindung stellt sich die Aufgabe, ein Verfahren der eingangs erwähnten Art so weiterzuentwickeln, daß ein hoher Ausstoß erzielt werden kann und hochkonzentrierte, hochviskose Celluloselösungen verarbeitet werden können.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.

Das erfindungsgemäße Verfahren zur Herstellung cellulosischer Fasern, bei welchem eine Lösung von Cellulose in einem tertiären Aminoxid in warmem Zustand zu Filamenten versponnen wird, welche durch einen Luftspalt geführt und anschließend mit einem Fällungsmittel in Kontakt gebracht werden, um die Cellulose zu fällen, wobei die Filamente durch Ausüben einer Kraft abgezogen und im Luftspalt verstreckt werden, welche Kraft mit dem Fällungsmittel ausgeübt wird, indem das Fällungsmittel in die Richtung strömen gelassen wird, in welche die Filamente abgezogen werden und die Filamente mit dem Fällungsmittel in Kontakt gebracht werden, ist dadurch gekennzeichnet, daß das Fällungsmittels in dem Zeitpunkt, in welchem es mit den Filamenten in Kontakt gebracht wird, mit einer Geschwindigkeit strömen gelassen wird, die mindestens so groß ist wie, und insbesondere größer ist als die Abzugsgeschwindigkeit der Filamente.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.

Mit dem erfindungsgemäßen Verfahren können vorteilhaft Celluloselösungen versponnen werden, die eine Cellulosekonzentration von mindestens 12 Masse-%, vorzugsweise 13-15 Masse-%, aufweisen.With the method according to the invention can be advantageous Cellulose solutions are spun, one Cellulose concentration of at least 12% by mass, preferably 13-15% by mass.

Die Erfindung beruht auf der Erkenntnis, daß hochviskose Celluloselösungen mit Cellulosekonzentrationen von mindestens 12 Masse-% ohne mechanische Verstreckungsvorrichtung, wie z.B. eine Abzugsgalette, also lediglich mit der vom strömenden Fällungsmittel auf die Filamente übertragenen kinetischen Energie verstreckt werden können. Dazu werden die Filamente durch einen sogenannten Injektor geführt, in welchen Fällungsmittel, das die Filamente beschleunigt, mit einem Druck eingespritzt wird, der über dem Umgebungsdruck liegt.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. For this purpose, the filaments are so-called injector, in which precipitant that the Filaments accelerated, injected with a pressure that is above the ambient pressure.

Die Abzugsgeschwindigkeit ergibt sich dabei in bekannter Weise aus dem gewünschten Titer der Filamente, der Konzentration der Celluloselösung und dem Ausstoß der Celluloselösung.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.

Die Filamente werden bevorzugt mit Fällungsmittel benetzt, bevor sie mit dem strömenden Fällungsmittel, welches die Kraft zum Abziehen auf sie ausübt, in Kontakt gebracht werden. Das Fällungsmittel, mit welchem die Filamente benetzt werden, kann das gleiche Fällungsmittel sein, mit welchem auf die Filamente die Kraft zum Verstrecken ausgeübt wird. Es kann aber auch ein anderes sein.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.

Um ein Verspinnen im dichten Filamentverband zu ermöglichen, ist es zweckmäßig, daß die Filamente im Luftspalt durch Anblasen mit einem Kühlgas gekühlt werden, wobei die Kühlung unmittelbar nach dem Verspinnen vorgenommen wird. Die Beblasung kann mit feuchter Luft vorgenommen werden. To enable spinning in the dense filament structure, is it is appropriate that 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.

Im erfindungsgemäßen Verfahren wird als tertiäres Aminoxid vorteilhaft N-Methylmorpholin-N-oxid eingesetzt.In the process according to the invention is used as the tertiary amine oxide advantageously used N-methylmorpholine-N-oxide.

Die Erfindung betrifft auch ein Verfahren zur Herstellung eines Spinnvlieses, welches dadurch gekennzeichnet ist, daß die erfindungsgemäß hergestellten cellulosischen Fasern zu einem Vlies gelegt werden, welches verfestigt wird.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.

Das Vlies kann durch Behandlung mit einem Wasserstrahl verfestigt werden. Es kann aber auch vorteilhaft verfestigt werden, indem es mit einer wäßrigen Lösung eines tertiären Aminoxids, welche Cellulose lösen kann, getränkt wird, um die Cellulose oberflächlich anzulösen, und indem das getränkte Vlies anschließend bei erhöhter Temperatur verpreßt wird, wonach die Lösung des tertiären Aminoxids aus dem verpreßten Vlies ausgewaschen wird.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.

Die Erfindung betrifft auch eine Vorrichtung zur Durchführung des erfindungsgemäßen Verfahrens, welche Vorrichtung aufweist: eine öffnung zur Aufnahme von Fällungsmittel und Filamenten, einen Kanal, der mit der öffnung in Verbindung steht und in welchem die Filamente geführt werden, welche Vorrichtung dadurch gekennzeichnet ist, daß der Kanal in einen Beschleunigungsbereich mündet, in welchem die Filamente mit einem Fällungsmittel beschleunigt werden, das über eine Zuführung, die in den Beschleunigungsbereich mündet, mit gegenüber Atmosphärendruck erhöhtem Druck eingebracht wird.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.

Die Erfindung betrifft ferner eine Spinnvorrichtung zur Durchführung des Aminoxidverfahrens nach dem Trocken/Naß-Spinnverfahren mit einer Spinndüse, einer Zuführung für Kühlgas und der oben genannten Vorrichtung.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.

Die Erfindung betrifft auch die Verwendung eines Injektors, welcher aufweist:

  • einen Kanal, in welchem frisch extrudierte cellulosische Filamente geführt werden,
  • einen Beschleunigungsbereich, in welchen der Kanal mündet, sodaß die Filamente dem Beschleunigungsbereich zugeführt werden können, und
  • eine Zuführung für Fällungsmittel, welche Zuführung in den Beschleunigungsbereich mündet, sodaß Fällungsmittel dem Beschleunigungsbereich zugeführt werden kann,
bei der Herstellung cellulosischer Filamente nach dem Trocken/Naßspinnverfahren, bei welchem eine Lösung von Cellulose in einem wäßrigen tertiären Aminoxid zu Filamenten geformt wird, welche in einem Luftspalt verstreckt und anschließend mit Fällungsmittel in Kontakt gebracht werden.The invention also relates to the use of an injector which has:
  • a channel in which freshly extruded cellulosic filaments are guided,
  • an acceleration area into which the channel opens so that the filaments can be fed to the acceleration area, and
  • a feed for precipitant, which feed opens into the acceleration area so that precipitant can be fed to the acceleration area,
in the production of cellulosic filaments by the dry / wet spinning process, in which a solution of cellulose in an aqueous tertiary amine oxide is formed into filaments, which are drawn in an air gap and then brought into contact with precipitant.

Die Erfindung wird an Hand der Zeichnung näher erläutert, welche in der Figur 1 die erfindungsgemäße Verwendung eines Injektors zum Trocken/Naßspinnen von Lösungen von Cellulose in einem tertiären Aminoxid zeigt. Figur 2 zeigt eine bevorzugte Ausgestaltung der erfindungsgemäßen Vorrichtung.The invention is explained in more detail with reference to the drawing, which in Figure 1, the use of an injector according to the invention for dry / wet spinning of cellulose solutions in one shows tertiary amine oxide. Figure 2 shows a preferred Design of the device according to the invention.

In der Figur 1 ist mit 1 eine beheizbare (Beheizung nicht dargestellt) Spinndüse bezeichnet, welche über die Zuleitung 2 mit Spinnmasse 3, d.h. warmer Celluloselösung mit einer Temperatur von etwa 100°C bis 120°C, beschickt wird. Die Pumpe 4 dient zum Dosieren der Spinnmasse und zum Einstellen des für das Extrudieren erforderlichen Druckes. Die aus der Spinndüse 1 über die Spinnlöcher 16 extrudierten Filamente 5 werden mit einem inerten Gas 6, vorzugsweise Luft, gekühlt, welche über die Gasdüsen 7 auf die die Spinndüse 1 verlassenden Filamente 5 gerichtet ist. Durch dieses Anblasen kann mit Spinndüsen gearbeitet werden, welche eine hohe Lochdichte aufweisen, ohne daß es zu einem Verkleben der Filamente während des Spinnvorganges kommt.In FIG. 1, 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.

Die Filamente 5 werden in den Kanal 9 des Injektors 17 geführt und gelangen schließlich in einen Beschleunigungsbereich 10 des Injektors 17, in welchem die Filamente mit schnell nach unten in Richtung Diffusor 11 fließendem Fällungsmittel in Kontakt kommen, wodurch die Cellulose gefällt wird. Gleichzeitig werden die Filamente beschleunigt. Das zur Beschleunigung eingesetzte Fällungsmittel wird über die Zuführung 14 in den Injektor 17 gepreßt. Durch die Beschleunigung der Filamente in Richtung Diffusor 11 werden die Filamente mit einer höheren Geschwindigkeit nach unten gezogen, als sie von der Spinndüse 1 nachgeliefert werden. Dies bewirkt eine Verstreckung der Filamente. Die verstreckten Filamente treten durch den Diffusor 11 aus dem Injektor 17 aus und können beispielsweise auf einem Sieb (nicht dargestellt) abgelegt werden. Die Führung der Filamente durch den Injektor 17 ist in der Figur 1 nicht dargestellt.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. At the same time, the Filaments accelerated. The one used for acceleration Precipitant is fed into the injector 17 via the feed 14 pressed. By accelerating the filaments in the direction Diffuser 11, 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.

In der in Figur 1 dargestellten Ausführungsform der Erfindung erstreckt sich der Luftspalt von der Unterseite der Spinndüse 1 bis zum Ende des Kanals 9, d.h. bis zur Mündung des Kanals 9 in den Beschleunigungsbereich 10. Die Länge des Kanals 9 ist nicht beschränkt und kann auch kürzer sein, als in der Figur 1 gezeigt ist.In the embodiment of the invention shown in Figure 1 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.

In der Figur 2 ist eine bevorzugte Ausführungsform der erfindungsgemäßen Vorrichtung dargestellt. In dieser Figur sind Vorrichtungsteile, die bereits in der Figur 1 beschrieben wurden, mit gleichen Bezugsziffern benannt.FIG. 2 shows a preferred embodiment of the Device according to the invention shown. In this figure are Device parts that have already been described in FIG. 1 named with the same reference numbers.

Die aus der Spinndüse 1 extrudierten Filamente 5 gelangen in eine Vorrichtung, die im wesentlichen einen Injektorteil 18 aufweist, auf welchen eine Art Spinntrichter 19 aufgesetzt ist. Die mechanische Verbindung des Injektorteils 18 mit dem Spinntrichter 19 kann z.B. mittels Verschraubung hergestellt sein.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.

Die aus der Spinndüse 1 extrudierten Filamente 5 gelangen über eine Luftstrecke, welche durch den Abstand der Unterseite der Spinndüse 1 von der Oberfläche des Fällungsmittels 15 definiert ist, in das Fällungsmittel 15 des Spinntrichters 19, werden durch den Kanal 9a geführt und gelangen schließlich in den Beschleunigungsbereich 10 des Injektors 18, in welchem die Filamente von schnell nach unten Richtung Diffusor 11 fließendem Fällungsmittel beschleunigt werden. Das zur Beschleunigung eingesetzte Fällungsmittel wird über die Zuführung 14 in den Injektor 18 gepreßt. Durch die Beschleunigung der Filamente in Richtung Diffusor 11 werden die Filamente mit einer höheren Geschwindigkeit nach unten gezogen, als sie von der Spinndüse 1 nachgeliefert werden. Dies bewirkt eine Verstreckung der Filamente im Luftspalt.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. For acceleration precipitant used is in the feed 14 in the Injector 18 pressed. By accelerating the filaments in The filaments with a higher direction towards the diffuser 11 Speed pulled down as it spins from the spinneret 1 be delivered later. This causes a stretching of the Filaments in the air gap.

Im Spinntrichter 19 befindet sich eine Zuführung 12 für Fällungsmittel, das über den Kanal 13 in den Konus 8 gepumpt wird. Es ist darauf zu achten, daß die Mengen an Fällungsmittel, die über die Zuführungen 12 und 14 dem Spinntrichter 19 zugeführt bzw. über den Diffusor 11 aus dem Injektor 18 abgeführt werden, so aufeinander abgestimmt sind, daß im Luftspalt die gewünschte Verstreckung erreicht wird und gleichzeitig ein Absinken des Flüssigkeitsspiegels 15 und damit eine Vergrößerung des Luftspaltes verhindert wird.In 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.

In der Figur 2 ist die Oberfläche des Fällungsmittels 15 so eingezeichnet, daß sie mit der Oberkante des Spinntrichters 19 abschließt. Es ist dem Fachmann klar, daß diese Oberfläche auch etwas tiefer vorgesehen werden kann, wobei sich dann naturgemäß der Luftspalt entsprechend vergrößert.In Figure 2, the surface of the precipitant 15 is like this marked that it with the upper edge of the spinning funnel 19th completes. It is clear to the person skilled in the art that this surface too can be provided a little deeper, but then naturally the air gap is increased accordingly.

Mit den nachfolgenden Ausführungsbeispielen wird die Erfindung noch näher beschrieben, wobei für die Beispiele 1 - 4 die in der Zeichnung dargestellte Vorrichtung verwendet wurde.With the following embodiments, the invention described in more detail, wherein for Examples 1-4 the in Drawing shown device was used.

Beispiel 1example 1

In der für den Fachmann bekannten Weise wurde in einem beheizbaren und evakuierbaren Rührkessel aus Sulfitzellstoff und wäßrigem NMMO eine spinnbare Celluloselösung mit einem Cellulosegehalt von 12% hergestellt (NMMO: 77%; H2O: 11%). Diese Lösung wurde bei 130°C aus einer Spinndüse mit 888 Loch (Lochdurchmesser: 80 µm) zu Filamenten extrudiert. In the manner known to those skilled in the art, 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 μm) to form filaments.

Der Luftspalt betrug 22 mm.The air gap was 22 mm.

In die Zuführung 14 wurde Fällungsmittel in einer Menge von 1008 1/Stunde eingespritzt. Die Fällungsmittelgeschwindigkeit betrug im Beschleunigungsbereich 10 am Ausgang des Kanals 9a etwa 378 m/Minute, wodurch eine Verstreckung bzw. Verzug von 9,9 erzielt wurde.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.

Eine Verstreckung von 9,9 bedeutet, daß die Filamente mit einer Geschwindigkeit abgezogen werden, die das 9,9fache jener Geschwindigkeit ist, mit der die Filamente die Spinndüse verlassen und in den Luftspalt eintreten, in welchem sie verstreckt werden. Die Verstreckung ist daher gegeben durch: Verstreckung = Geschwindigkeit EndabzugGeschwindigkeit am Düsenaustritt 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 stretching is therefore given by: Stretching = Final withdrawal speed Speed at the nozzle outlet

Die hergestellten Fasern wiesen einen Titer von 1,30 dtex auf.The fibers produced had a titer of 1.30 dtex.

Beispiele 2 - 4Examples 2-4

Es wurde das im Beispiel 1 beschriebene Verfahren durchgeführt, wobei jedoch die in der nachfolgenden Tabelle angegebene Fällungsmitteleinspritzung und Fällungsmittelgeschwindigkeit gewählt wurden und die ebenfalls in der Tabelle angegebene Verstreckung erzielt wurde. Fällungsmittel- Verstreckung Titer (dtex) einspritzung geschwindigkeit Bsp. 2 792 l/h 396 m/min 5,3 2,45 Bsp. 3 828 l/h 414 m/min 6,9 1,87 Bsp. 4 720 l/h 360 m/min 9,3 1,39 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 Ex. 4 720 l / h 360 m / min 9.3 1.39

Beispiel 5Example 5

Der in Beispiel 2 hergestellte Filamentstrang wurde auf ein Siebband zu einem Vlies mit einem Flächengewicht von 40 g/m2 auflaufen gelassen. Die Flüssigkeitsdurchlässigkeit dieses Vlieses wurde mit einem LISTER-Gerät nach der EDANA-(European Disposables and Nonwovens Association)-Norm 150.2-93 gemessen (Methodik: Eine bestimmte Menge (5 ml) der Testflüssigkeit (0,9%ige NaCl-Lösung) wird dabei mit konstanter Auslaufgeschwindigkeit auf das Vlies gebracht. Die Zeit für den Abtransport dieser Flüssigkeit durch das Vlies wird elektronisch gemessen). Der Mittelwert aus 10 Messungen betrug 1,47 sec.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.

Claims (11)

  1. Process for producing cellulosic fibres, in which a solution of cellulose in a tertiary amine oxide in the hot state is spun into filaments which are passed through an air gap and then brought into contact with a precipitating agent in order to precipitate the cellulose, the filaments being drawn off by applying a force and stretched in the air gap, which force is applied by the precipitating agent by allowing the precipitating agent to flow in the direction in which the filaments are drawn off and by bringing the filaments into contact with the precipitating agent, characterized in that, at the instant at which it is brought into contact with the filaments, the precipitating agent is caused to flow with a velocity which is at least as great as, and in particular is greater than, the drawing-off velocity of the filaments.
  2. Process according to claim 1, characterized in that the filaments are wetted with the precipitating agent before they are brought into contact with the flowing precipitating agent which applies the force to them for drawing-off.
  3. Process according to one of Claims 1 or 2, characterized in that the filaments are cooled in the air gap by blasting with a cooling gas, the cooling being carried out immediately after the spinning.
  4. Process according to one of claims 1 to 3, characterized in that N-methylmorpholine N-oxide is used as tertiary amine oxide.
  5. Process according to Claim 4, characterized in that the solution to be spun has a cellulose concentration of at least 12% by mass, preferably 13-15% by mass.
  6. Process for producing a spunbonded material, characterized in that the cellulosic fibres produced by the process according to one or more of Claims 1 to 5 are laid to form a nonwoven fabric which is bonded.
  7. Process according to claim 6, characterized in that the nonwoven fabric is bonded by being impregnated with an aqueous solution of a tertiary amine oxide capable of dissolving cellulose in order to dissolve the cellulose superficially and by then pressing the impregnated nonwoven fabric at elevated temperature, after which the solution of the tertiary amine oxide is washed out of the pressed nonwoven fabric.
  8. Device for carrying out the process according to one of Claims 1 to 7, having an opening (8) for receiving precipitating agent (15) and filaments (5), and a duct (9a) which is connected to the opening (8) and in which the filaments (5) are guided, characterized in that the duct (9a) debouches into an accelerating region (10) in which the filaments (5) are accelerated by a precipitating agent which is introduced at a pressure higher than atmospheric pressure via an inlet (14) which debouches into the accelerating region (10).
  9. Spinning device for carrying out the method according to the dry/wet spinning process having a spinneret (1), an inlet (7) for cooling gas (6) and a device according to Claim 8.
  10. Use of an injector which has
    a duct (9) in which freshly extruded cellulosic filaments are guided,
    an accelerating region (10) into which the duct (9) debouches so that the filaments can be fed to the accelerating region, and
    an inlet (14) for precipitating agent, which inlet (14) debouches into the accelerating region (10) so that precipitating agent can be fed to the accelerating region (10),
    to carry out the process according to one of Claims 1 to 7.
  11. Spunbonded material produced by laying cellulosic fibres produced by the process according to one or more of Claims 1 to 5 to form a nonwoven fabric and bonding the fabric with a water jet.
EP96942981A 1995-12-27 1996-12-20 Method for the production of cellulose fibres and device for carrying out the method Expired - Lifetime EP0811087B1 (en)

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AT2107/99 1995-12-27
AT0210795A AT402947B (en) 1995-12-27 1995-12-27 METHOD FOR PRODUCING CELLULOSIC FIBERS AND DEVICE FOR IMPLEMENTING THE METHOD
PCT/AT1996/000260 WO1997024476A1 (en) 1995-12-27 1996-12-20 Method for the production of cellulose fibres and device for carrying out the method

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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
CN1061106C (en) * 1997-12-09 2001-01-24 宜宾丝丽雅集团有限公司 Method for producing cellulose fiber by dissolvant method
AT406386B (en) 1998-07-28 2000-04-25 Chemiefaser Lenzing Ag METHOD AND DEVICE FOR PRODUCING CELLULOSIC MOLDED BODIES
DE10025231A1 (en) * 2000-05-22 2000-11-02 Lurgi Zimmer Ag Extrusion of continuous filaments or film from a solution of water with cellulose and a tertiary amine oxide has a structured air drawing action in the air gap after the extrusion channel to increase the material strength
DE10025230A1 (en) * 2000-05-22 2000-11-02 Lurgi Zimmer Ag Extrusion of continuous filaments or film from a solution of water with cellulose and a tertiary amine oxide has a structured air drawing action in the air gap after the extrusion channel to increase the material strength
DE10060876B4 (en) * 2000-12-07 2006-03-09 Zimmer Ag Precipitation device for a spinning plant
JP4593370B2 (en) * 2005-06-02 2010-12-08 帝人テクノプロダクツ株式会社 Dry and wet spinning equipment
US20090312731A1 (en) * 2006-04-28 2009-12-17 Lenzing Aktiengesellschaft Nonwoven Melt-Blown Product
AT503625B1 (en) 2006-04-28 2013-10-15 Chemiefaser Lenzing Ag WATER-IRRADIZED PRODUCT CONTAINING CELLULASIC FIBERS
ES2625035B1 (en) * 2015-12-18 2018-06-21 Universidad De Extremadura PRODUCTION OF VISCOELASTIC CAPILLARY JETS BY GASEOUS FOCUS
EP3470557A1 (en) * 2017-10-12 2019-04-17 Lenzing Aktiengesellschaft Spinning device and method for stringing up in a spinning device
CN110424423B (en) * 2019-08-22 2022-02-08 深圳市如茵生态环境建设有限公司 Fiber spinning system
CN116334778B (en) * 2023-05-26 2023-07-21 吉林富博纤维研究院有限公司 Preparation method of high-performance PAN-based carbon fiber precursor

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PL285328A1 (en) * 1989-05-31 1991-01-28 Chemiefaser Lenzing Ag Apparatus for and method of expsing fibre cables to treatment with a liquid
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DE59601184D1 (en) 1999-03-04
AU1185797A (en) 1997-07-28
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CA2213221A1 (en) 1997-07-10
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WO1997024476A1 (en) 1997-07-10
ATA210795A (en) 1997-02-15

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