EP0811087A1 - 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

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Publication number
EP0811087A1
EP0811087A1 EP96942981A EP96942981A EP0811087A1 EP 0811087 A1 EP0811087 A1 EP 0811087A1 EP 96942981 A EP96942981 A EP 96942981A EP 96942981 A EP96942981 A EP 96942981A EP 0811087 A1 EP0811087 A1 EP 0811087A1
Authority
EP
European Patent Office
Prior art keywords
filaments
precipitant
cellulose
air gap
brought
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
EP96942981A
Other languages
German (de)
French (fr)
Other versions
EP0811087B1 (en
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 of EP0811087A1 publication Critical patent/EP0811087A1/en
Application granted granted Critical
Publication of EP0811087B1 publication Critical patent/EP0811087B1/en
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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
    • 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 process for the production of cellulosic fibers, in which a solution of cellulose in a tertiary amine oxide is spun in a warm state into filaments which are passed through an air gap and are subsequently brought into contact with a precipitant in order to precipitate the cellulose, whereby the filaments are withdrawn by exerting a force and stretched in the air gap, which force is exerted on the precipitant by flowing the precipitant in the direction in which the filaments are withdrawn and bringing the filaments into contact with the precipitant.
  • the invention also relates to an apparatus for performing the method.
  • tertiary amine oxides are able to dissolve cellulose and that cellulosic moldings can be obtained from these solutions by precipitation.
  • a method for producing such solutions is known for example from EP-A - 0 356 419.
  • a suspension of cellulose in an aqueous tertiary amine oxide is first prepared.
  • the amine oxide contains up to 40% by mass of water.
  • the aqueous cellulose suspension is heated and water is drawn off under reduced pressure until the cellulose dissolves.
  • the process can be carried out in a thin film treatment apparatus.
  • a spinning process is known, according to which the freshly spun filaments are brought into contact with a precipitant which is allowed to flow in the direction in which the filaments are drawn off.
  • DE-C - 195 12 053 also discloses a process for the production of cellulosic fibers, in which the freshly extruded filaments are introduced into a precipitation bath which is accelerated to a predetermined speed and at least approximately laminar in the direction of the extruded filaments. The filaments are drawn off from a spool.
  • air should not only mean air as such, but also any gas or gas mixture which is inert to the filaments and does not interfere with spinning in any other way. Accordingly, a gas other than air can also be present in the "air gap".
  • a method of the type described at the outset is known from EP-A-0 574 870.
  • This process is carried out with a so-called spinning funnel, in which the freshly extruded filaments are warped with the aid of a liquid, flowing precipitant. The flow of the precipitant is caused by gravity.
  • the disadvantage is this method that only relatively low-viscosity cellulose solutions, which moreover have a relatively low cellulose concentration of only 7.8% by mass, 6.1% by mass and 10.5% by mass, can be spun. From an economic point of view, such low cellulose concentrations are unsatisfactory, since they require low solution production capacity and high evaporation costs when working up the used precipitant.
  • the object of the present invention is to further develop a method of the type mentioned at the outset in such a way 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 in the warm state is spun into filaments, which are passed through an air gap and then brought into contact with a precipitant in order to precipitate the cellulose, the filaments drawn off by exerting a force and stretched in the air gap, which force is exerted with the precipitant, by allowing the precipitant to flow in the direction in which the filaments are drawn off and the filaments are brought into contact with the precipitant, is characterized in that that the precipitant is allowed to flow at a rate at least as large as, and when it is brought into contact with the filaments is in particular greater than the speed at which the filaments are drawn off.
  • the invention is based on the knowledge that highly viscous cellulose solutions with cellulose concentrations of at least 12% by mass without a mechanical stretching device, such as e.g. a take-off godet, that is to say only with the kinetic energy transferred from the flowing precipitant to the filaments.
  • a mechanical stretching device such as e.g. a take-off godet
  • the filaments are passed through a so-called injector, into which precipitant which accelerates the filaments is injected at a pressure which is above the ambient pressure.
  • the removal speed is obtained in a known manner from the desired titer of the filaments, the concentration of the cellulose solution and the output of the cellulose solution.
  • the filaments are preferably wetted with precipitant before they are brought into contact with the flowing precipitant, which exerts the pulling force on them.
  • the precipitant with which the filaments are wetted can be the same precipitant with which the force for stretching is exerted on the filaments. But it can also be different.
  • the filaments In order to enable spinning in the dense filament structure, it is expedient for the filaments to be cooled in the air gap by blowing with a cooling gas, the cooling being carried out immediately after spinning.
  • the blowing can be done with moist air.
  • N-methylmorpholine-N-oxide is advantageously used as the tertiary amine oxide in the process according to the invention.
  • the invention also relates to a method for producing a spunbonded nonwoven, which is characterized in that the cellulosic fibers produced according to the invention are laid to form a nonwoven which is consolidated.
  • the fleece can be consolidated by treatment with a water jet. However, it can also advantageously be solidified by soaking it with an aqueous solution of a tertiary amine oxide which can dissolve cellulose in order to dissolve the cellulose on the surface, and then pressing the soaked fleece at an elevated temperature, after which the solution of the tertiary amine oxide is washed out of the pressed fleece.
  • a tertiary amine oxide which can dissolve cellulose in order to dissolve the cellulose on the surface
  • the invention also relates to a device for carrying out the method according to the invention, which device comprises: an opening for receiving precipitant and filaments, a channel which is connected to the opening and in which the filaments are guided, which device is characterized in that the channel opens into an acceleration area in which the filaments are accelerated with a precipitant which is introduced via a feed which opens into the acceleration area at a pressure which is higher than atmospheric pressure.
  • the invention further relates to a spinning device for carrying out the amine oxide process according to the
  • 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 feeds 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.
  • FIG. 1 shows in FIG. 1 the use according to the invention of an injector for dry / wet spinning of solutions of cellulose in a tertiary amine oxide.
  • Figure 2 shows a preferred embodiment of the device according to the invention.
  • 1 is 1 with a heatable (heating not darge sets) designated spinneret which C, is fed via the feed line 2 with spinning material 3, that hot cellulose solution at a temperature of about 100 ° C to 120 *.
  • the pump 4 serves to meter the spinning mass and to set the pressure required for the extrusion.
  • the filaments 5 extruded from the spinneret 1 via the spinning holes 16 are cooled with an inert gas 6, preferably air, which is directed via the gas nozzles 7 onto the filaments 5 leaving the spinneret 1.
  • the filaments 5 are guided into the channel 9 of the injector 17 and finally reach an acceleration area 10 of the injector 17, in which the filaments come into contact with precipitant flowing rapidly downwards in the direction of the diffuser 11, as a result of which the cellulose is precipitated.
  • the Filaments accelerated.
  • the precipitant used for acceleration is pressed into the injector 17 via the feed 14. Due to the acceleration of the filaments in the direction of the diffuser 11, the filaments are drawn downward at a higher speed than they are supplied by the spinneret 1. This causes the filaments to stretch.
  • the drawn filaments emerge from the injector 17 through the diffuser 11 and can be deposited, for example, on a sieve (not shown). The guidance of the filaments through the injector 17 is not shown in FIG. 1.
  • the air gap extends from the bottom of the spinneret 1 to the end of the channel 9, i.e. to the mouth of the channel 9 in the acceleration range 10.
  • the length of the channel 9 is not limited and can also be shorter than shown in FIG. 1.
  • FIG. 2 shows a preferred embodiment of the device according to the invention.
  • parts of the device which have already been described in FIG. 1 are given 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 type 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 reach the precipitant 15 of the spinning funnel 19 via an air gap, which is defined by the distance of the underside of the spinneret 1 from the surface of the precipitating agent 15, are guided through the channel 9a and finally reach the Acceleration range 10 of the injector 18, in which the filaments flow from the fast downward direction towards the diffuser 11 Precipitating agents are accelerated.
  • the precipitant used for acceleration is pressed into the injector 18 via the feed 14. Due to the acceleration of the filaments in the direction of the diffuser 11, the filaments are drawn downward at a higher speed than they are supplied by the spinneret 1. This causes the filaments to stretch in the air gap.
  • the spinning funnel 19 there is a feed 12 for precipitant which is pumped into the cone 8 via the channel 13. Care must be taken that the amounts of precipitant which are fed to the spinning funnel 19 via the feeds 12 and 14 or discharged from the injector 18 via the diffuser 11 are matched to one another in such a way that the desired stretching is achieved in the air gap and at the same time a decrease in the liquid level 15 and thus an enlargement of the air gap is prevented.
  • a spinnable cellulose solution with a cellulose content of 12% (NMMO: 77%; H 2 0: 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 / im) into filaments. The air gap was 22 mm.
  • Precipitant was injected into feed 14 in an amount of 1008 l / hour.
  • the precipitant speed in the acceleration area 10 at the exit of the channel 9a was approximately 378 m / minute, whereby a stretching or warping of 9.9 was achieved.
  • 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:
  • 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.
  • 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 the 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 mean of 10 measurements was 1.47 see.

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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)
  • 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

Verfahren zur Herstellung cellulosischer Fasern sowie Vorrichtung zur Durchführung des Verfahrens Process for producing cellulosic fibers and device for carrying out the process
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 v/erden 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 process for the production of cellulosic fibers, in which a solution of cellulose in a tertiary amine oxide is spun in a warm state into filaments which are passed through an air gap and are subsequently brought into contact with a precipitant in order to precipitate the cellulose, whereby the filaments are withdrawn by exerting a force and stretched in the air gap, which force is exerted on the precipitant by flowing the precipitant in the direction in which the filaments are withdrawn and bringing the filaments into contact with the precipitant. The invention also relates to 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 zunächεt eine Suspension von Cellulose in einem wässerigen tertiären Aminoxid bereitet. Das Aminoxid enthält bis zu 40 Maεse-% 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 Pat. No. 2,179,181 it is known that tertiary amine oxides are able to dissolve cellulose and that cellulosic moldings can be obtained from these solutions by precipitation. A method for producing such solutions is known for example from EP-A - 0 356 419. According to this publication, a suspension of cellulose in an aqueous tertiary amine oxide is first prepared. The amine oxide contains up to 40% by mass of water. The aqueous cellulose suspension is heated and water is drawn off under reduced pressure until the cellulose dissolves. The process can be carried out in a thin film treatment apparatus.
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. 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.From DE-A - 28 44 163 and DD-A - 218 121 it is known that for the production of cellulose fibers or cellulose films an air gap is placed between the spinneret and the precipitant, in which the extruded fibers are stretched. This stretching is necessary because, after the formed spinning solution comes into contact with the aqueous precipitant, it is very difficult to stretch the filaments. The fiber structure set in the air gap is fixed in the precipitant. In the air gap, however, there is a risk that the individual filaments which have not yet coagulated will adhere to one another or merge with one another due to their extremely high stickiness and thus make fiber spinning impossible. Naturally, the longer the distance between the nozzle plate and the surface of the precipitant (air gap), the greater the risk of sticking. From WO 93/19230 it is known that a dense filament bandage can be spun with a long air gap if the warm, shaped spinning solution is cooled before being introduced into the precipitant, the cooling being carried out immediately after molding by blowing with a cooling gas .
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 v/erden.From DD-A-271 534 a spinning process is known, according to which the freshly spun filaments are brought into contact with a precipitant which is allowed to flow in the direction in which the filaments are drawn off.
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.DE-C - 195 12 053 also discloses a process for the production of cellulosic fibers, in which the freshly extruded filaments are introduced into a precipitation bath which is accelerated to a predetermined speed and at least approximately laminar in the direction of the extruded filaments. The filaments are drawn off from a spool.
Für die Zwecke der vorliegenden Beschreibung und der vorliegenden Patentansprüche soll der Ausdruck "Luft" nicht nur Luft alε 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 the present description and the present patent claims, the term “air” should not only mean air as such, but also any gas or gas mixture which is inert to the filaments and does not interfere with spinning in any other way. Accordingly, a gas other than air can also be present in the "air gap".
Ein Verfahren der eingangs beschriebenen Art iεt 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 Maεse-% bzw. 10,5 Masse-% aufweisen, versponnen werden können. Aus wirtschaftlicher Sicht sind derartig geringe Cellulosekonzentrationen unbefriedigend, da dieεe eine geringe Kapazität der Lösungsherstellung und hohe Eindampfkosten bei der Aufarbeitung des gebrauchten Fällungsmittels bedingen.A method of the type described at the outset is known from EP-A-0 574 870. This process is carried out with a so-called spinning funnel, in which the freshly extruded filaments are warped with the aid of a liquid, flowing precipitant. The flow of the precipitant is caused by gravity. The disadvantage is this method that only relatively low-viscosity cellulose solutions, which moreover have a relatively low cellulose concentration of only 7.8% by mass, 6.1% by mass and 10.5% by mass, can be spun. From an economic point of view, such low cellulose concentrations are unsatisfactory, since they require low solution production capacity and high evaporation costs when working up 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.However, an economical fiber production with high production rates requires the processing of spinning masses which have a higher cellulose concentration. In addition, the spinning mass output should be as high as possible. However, such a method cannot be carried out with the known spinning funnel, since this would have to be built in an unsuitable size.
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 to further develop a method of the type mentioned at the outset in such a way 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 verεtreckt 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 εo 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 in the warm state is spun into filaments, which are passed through an air gap and then brought into contact with a precipitant in order to precipitate the cellulose, the filaments drawn off by exerting a force and stretched in the air gap, which force is exerted with the precipitant, by allowing the precipitant to flow in the direction in which the filaments are drawn off and the filaments are brought into contact with the precipitant, is characterized in that that the precipitant is allowed to flow at a rate at least as large as, and when it is brought into contact with the filaments is in particular greater than the speed at which the filaments are drawn off.
Mit dem erfindungsgemäßen Verfahren können vorteilhaft Celluloselösungen versponnen werden, die eineWith the method according to the invention, cellulose solutions can advantageously be spun, the one
Cellulosekonzentration von mindestens 12 Masse-%, vorzugsweise 13-15 Masse-%, aufweisen.Have 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 knowledge that highly viscous cellulose solutions with cellulose concentrations of at least 12% by mass without a mechanical stretching device, such as e.g. a take-off godet, that is to say only with the kinetic energy transferred from the flowing precipitant to the filaments. For this purpose, the filaments are passed through a so-called injector, into which precipitant which accelerates the filaments is injected at a pressure which 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 removal speed is obtained in a known manner from the desired titer of the filaments, the concentration of the cellulose solution and the output 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 they are brought into contact with the flowing precipitant, which exerts the pulling force on them. The precipitant with which the filaments are wetted can be the same precipitant with which the force for stretching is exerted on the filaments. But it can also 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. Im erfindungsgemäßen Verfahren wird als tertiäres Aminoxid vorteilhaft N-Methylmorpholin-N-oxid eingesetzt.In order to enable spinning in the dense filament structure, it is expedient for the filaments to be cooled in the air gap by blowing with a cooling gas, the cooling being carried out immediately after spinning. The blowing can be done with moist air. N-methylmorpholine-N-oxide is advantageously used as the tertiary amine oxide in the process according to the invention.
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 spunbonded nonwoven, which is characterized in that the cellulosic fibers produced according to the invention are laid to form a nonwoven 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. However, it can also advantageously be solidified by soaking it with an aqueous solution of a tertiary amine oxide which can dissolve cellulose in order to dissolve the cellulose on the surface, and then pressing the soaked fleece at an elevated temperature, after which the solution of the tertiary amine oxide is washed out of the pressed fleece.
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: an opening for receiving precipitant and filaments, a channel which is connected to the opening and in which the filaments are guided, which device is characterized in that the channel opens into an acceleration area in which the filaments are accelerated with a precipitant which is introduced via a feed which opens into the acceleration area at a pressure which is higher than atmospheric pressure.
Die Erfindung betrifft ferner eine Spinnvorrichtung zur Durchführung des Aminoxidverfahrens nach demThe invention further relates to a spinning device for carrying out the amine oxide process according to the
Trocken/Naß-Spinnverfahren mit einer Spinndüse, einer Zuführung für Kühlgas und der oben genannten Vorrichtung.Dry / wet spinning process with a spinneret, a supply for cooling gas and the above-mentioned device.
Die Erfindung betrifft auch die Verwendung eines Injektors, welcher aufweist: einen Kanal, in welchem frisch extrudierte cellulosischeThe invention also relates to the use of an injector which has: a channel in which freshly extruded cellulosic
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.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 feeds 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 shows in FIG. 1 the use according to the invention of an injector for dry / wet spinning of solutions of cellulose in a tertiary amine oxide. Figure 2 shows a preferred embodiment of the device according to the invention.
In der Figur 1 ist mit 1 eine beheizbare (Beheizung nicht darge¬ stellt) 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 l 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 the figure, 1 is 1 with a heatable (heating not darge sets) designated spinneret which C, is fed via the feed line 2 with spinning material 3, that hot cellulose solution at a temperature of about 100 ° C to 120 *. The pump 4 serves to meter the spinning mass and to set the pressure required for the extrusion. The filaments 5 extruded from the spinneret 1 via the spinning holes 16 are cooled with an inert gas 6, preferably air, which is directed via the gas nozzles 7 onto the filaments 5 leaving the spinneret 1. By this blowing, it is possible to work with spinnerets which have a high hole density without the filaments sticking together during the spinning process.
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 reach an acceleration area 10 of the injector 17, in which the filaments come into contact with precipitant flowing rapidly downwards in the direction of the diffuser 11, as a result of which the cellulose is precipitated. At the same time, the Filaments accelerated. The precipitant used for acceleration is pressed into the injector 17 via the feed 14. Due to the acceleration of the filaments in the direction of the diffuser 11, the filaments are drawn downward at a higher speed than they are supplied by the spinneret 1. This causes the filaments to stretch. The drawn filaments emerge from the injector 17 through the diffuser 11 and can be deposited, for example, on a sieve (not shown). The guidance of the filaments through the injector 17 is not shown in FIG. 1.
In der in Figur 1 dargestellten Ausführungsform der Erfindung erstreckt sich der Luftspalt von der Unterseite der Spinndüse l 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 bottom of the spinneret 1 to the end of the channel 9, i.e. to the mouth of the channel 9 in the acceleration range 10. The length of the channel 9 is not limited and can also be shorter than shown in FIG. 1.
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. In this figure, parts of the device which have already been described in FIG. 1 are given 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 type 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 l 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 reach the precipitant 15 of the spinning funnel 19 via an air gap, which is defined by the distance of the underside of the spinneret 1 from the surface of the precipitating agent 15, are guided through the channel 9a and finally reach the Acceleration range 10 of the injector 18, in which the filaments flow from the fast downward direction towards the diffuser 11 Precipitating agents are accelerated. The precipitant used for acceleration is pressed into the injector 18 via the feed 14. Due to the acceleration of the filaments in the direction of the diffuser 11, the filaments are drawn downward at a higher speed than they are supplied by the spinneret 1. This causes the filaments to stretch 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 which is pumped into the cone 8 via the channel 13. Care must be taken that the amounts of precipitant which are fed to the spinning funnel 19 via the feeds 12 and 14 or discharged from the injector 18 via the diffuser 11 are matched to one another in such a way that the desired stretching is achieved in the air gap and at the same time a decrease in the liquid level 15 and thus an enlargement of the 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 drawn in such a way that it ends with the upper edge of the spinning funnel 19. It is clear to the person skilled in the art that this surface can also be provided somewhat deeper, in which case the air gap naturally increases 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.The invention is described in more detail with the following exemplary embodiments, the device shown in the drawing being used for Examples 1-4.
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%; H20: 11%). Diese Lösung wurde bei 130°C aus einer Spinndüse mit 888 Loch (Lochdurchmesser: 80 /im) zu Filamenten extrudiert. Der Luftspalt betrug 22 mm.In the manner known to the person skilled in the art, a spinnable cellulose solution with a cellulose content of 12% (NMMO: 77%; H 2 0: 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 / im) into filaments. 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 injected into feed 14 in an amount of 1008 l / hour. The precipitant speed in the acceleration area 10 at the exit of the channel 9a was approximately 378 m / minute, whereby a stretching or warping of 9.9 was achieved.
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: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:
Geschwindigkeit Endabzug Verstreckung =Speed of final draw stretching
Geschwindigkeit am DüsenaustrittSpeed 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 l 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.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.
Tabelletable
Fällungsmittel- Verstreckung Titer einspritzung geschwindigkeit (dtex)Precipitant stretching Titer injection speed (dtex)
Bsp. 2 792 1/h 396 m/min 5,3 2,45Ex. 2 792 1 / h 396 m / min 5.3 2.45
Bsp. 3 828 1/h 414 m/min 6,9 1,87Ex. 3 828 1 / h 414 m / min 6.9 1.87
Bsp. 4 720 1/h 360 m/min 9,3 1,39 Beispiel 5Ex. 4 720 1 / h 360 m / min 9.3 1.39 Example 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 see. 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 the 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 mean of 10 measurements was 1.47 see.

Claims

Patentansprüche: Claims:
1. 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,1. A process for producing cellulosic fibers, in which a solution of cellulose in a tertiary amine oxide is spun in a warm state into filaments which are passed through an air gap and are subsequently brought into contact with a precipitant to precipitate the cellulose, the filaments withdrawn by exerting a force and stretching in the air gap, which force is exerted on the precipitant by flowing the precipitant in the direction in which the filaments are withdrawn and the filaments are brought into contact with the precipitant,
dadurch gekennzeichnet,characterized,
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.that when the precipitant is brought into contact with the filaments, it is allowed to flow at a rate which is at least as great as, and in particular greater than the rate at which the filaments are withdrawn.
Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Filamente mit Fällungsmittel benetzt werden, bevor sie mit dem strömenden Fällungsmittel, welches die Kraft zum Abziehen auf sie ausübt, in Kontakt gebracht werden.A method according to claim 1, characterized in that the filaments are wetted with precipitant before they are brought into contact with the flowing precipitant which exerts the pulling force on them.
Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß die Filamente im Luftspalt durch Anblasen mit einem Kühlgas gekühlt werden, wobei die Kühlung unmittelbar nach dem Verspinnen vorgenommen wird. Method according to one of claims 1 or 2, characterized in that the filaments are cooled in the air gap by blowing with a cooling gas, the cooling being carried out immediately after spinning.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß als tertiäres Aminoxid N-Methylmorpholin-N-oxid eingesetzt wird.4. The method according to any one of claims 1 to 3, characterized in that N-methylmorpholine-N-oxide is used as the tertiary amine oxide.
5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die zu verspinnende Lösung eine Cellulosekonzentration von mindestens 12 Masse-%, vorzugsweise 13-15 Masse-%, aufweist.5. The method 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.
Verfahren zur Herstellung eines Spinnvlieses, dadurch gekennzeichnet, daß die gemäß dem Verfahren nach einem oder mehreren der Ansprüche 1 bis 5 hergestellten cellulosischen Fasern zu einem Vlies gelegt werden, welches verfestigt wird.A process for producing a spunbonded nonwoven, characterized in that the cellulosic fibers produced according to the process according to one or more of claims 1 to 5 are laid to form a nonwoven which is consolidated.
Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß das Vlies verfestigt wird, 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.A method according to claim 6, characterized in that the nonwoven is consolidated by soaking it with an aqueous solution of a tertiary amine oxide which can dissolve cellulose in order to dissolve the cellulose superficially, and then pressing the impregnated nonwoven at an elevated temperature, after which the solution of the tertiary amine oxide is washed out of the pressed fleece.
8. Vorrichtung zur Durchführung des Verfahrens gemäß einem der Ansprüche 1 bis 7, mit einer Öffnung (8) zur Aufnahme von Fällungsmittel (15) und Filamenten (5), einem Kanal (9a), der mit der Öffnung (8) in Verbindung steht und in welchem die Filamente (5) geführt werden, dadurch gekennzeichnet, daß der Kanal (9a) in einen Beschleunigungsbereich (10) mündet, in welchem die Filamente (5) mit einem Fällungsmittel beschleunigt werden, das über eine Zuführung (14), die in den Beschleunigungsbereich (10) mündet, mit gegenüber Atmosphärendruck erhöhtem Druck eingebracht wird. 8. Device for performing the method according to one of claims 1 to 7, with an opening (8) for receiving precipitant (15) and filaments (5), a channel (9a) which is in communication with the opening (8) and in which the filaments (5) are guided, characterized in that the channel (9a) opens into an acceleration region (10) in which the filaments (5) are accelerated with a precipitant which is supplied via a feed (14) opens into the acceleration area (10), is introduced with increased pressure compared to atmospheric pressure.
Spinnvorrichtung zur Durchführung des Verfahrens nach dem Trocken/Naß-Spinnverfahren mit einer Spinndüse (1), einer Zuführung (7) für Kühlgas (6) und einer Vorrichtung gemäß Anspruch 8. Spinning device for carrying out the method according to the dry / wet spinning method with a spinneret (1), a feed (7) for cooling gas (6) and a device according to claim 8.
10. Verwendung eines Injektors, welcher aufweist: einen Kanal (9) , in welchem frisch extrudierte cellulosische Filamente geführt werden, einen Beschleunigungsbereich (10), in welchen der Kanal10. Use of an injector which has: a channel (9) in which freshly extruded cellulosic filaments are guided, an acceleration area (10) in which the channel
(9) mündet, sodaß die Filamente dem Beschleunigungsbereich zugeführt werden können, und eine Zuführung (14) für Fällungsmittel, welche Zuführung (14) in den Beschleunigungsbereich (10) mündet, sodaß Fällungsmittel dem Beschleunigungsbereich(9) opens so that the filaments can be fed to the acceleration area, and a feed (14) for precipitant, which feed (14) opens into the acceleration area (10), so that precipitant enters the acceleration area
(10) 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. (10) can be supplied in the manufacture 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.
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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DE59601184D1 (en) 1999-03-04
BR9607047A (en) 1997-12-30
ATE176011T1 (en) 1999-02-15
CN1181788A (en) 1998-05-13
AU1185797A (en) 1997-07-28
NO973763L (en) 1997-08-15
JPH11501371A (en) 1999-02-02
CA2213221A1 (en) 1997-07-10
AT402947B (en) 1997-09-25
WO1997024476A1 (en) 1997-07-10
ES2129992T3 (en) 1999-06-16
NO973763D0 (en) 1997-08-15
ATA210795A (en) 1997-02-15
EP0811087B1 (en) 1999-01-20

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