EP0581145B2 - Process and apparatus for the production of fibres, which give off gases and/or vapours during their spinning - Google Patents

Process and apparatus for the production of fibres, which give off gases and/or vapours during their spinning Download PDF

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Publication number
EP0581145B2
EP0581145B2 EP93111453A EP93111453A EP0581145B2 EP 0581145 B2 EP0581145 B2 EP 0581145B2 EP 93111453 A EP93111453 A EP 93111453A EP 93111453 A EP93111453 A EP 93111453A EP 0581145 B2 EP0581145 B2 EP 0581145B2
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EP
European Patent Office
Prior art keywords
spinning
spinning shaft
gas
shaft
gases
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EP93111453A
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German (de)
French (fr)
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EP0581145B1 (en
EP0581145A2 (en
EP0581145A3 (en
Inventor
Herbert Dr. Wellenhofer
Gerhard Dr. Leumer
Andreas Fischer
Diethelm Dr. Rabe
Jürgen Hans Profé
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INVISTA TECHNOLOGIES Sarl
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Arteva Technologies SARL
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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
    • D01D5/08—Melt spinning methods
    • D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
    • D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
    • D01F6/765—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products from polyarylene sulfides

Definitions

  • thermoplastic polymers in which encapsulated spinning shafts are used are known per se.
  • EP-A-147, 173 describes a melt spinning process of thermoplastic polymers, in which the polymer is extruded into a pressurized spinning shaft and is cooled within this shaft. Furthermore, an adapted device for carrying out the method is described, which has a specially designed outlet opening for the solidified filaments drawn off at high speed and with which a good sealing of the spinning shaft can be achieved. The device and the method are primarily aimed at producing a highly oriented multifilament yarn.
  • EP-A-205,694 describes a melt spinning process of thermoplastic polymers, in which the polymer is extruded into a spinning shaft which is under a vacuum of less than 0.7 atm and is cooled within this shaft.
  • the device for carrying out this method essentially relates to the device known from EP-A-147, 173 , to whose outlet side a vacuum pump is connected for the gas located in the spinning shaft.
  • monomers and oligomers evaporating from the spun threads are removed from the spinning shaft by the gas flow, so that problems with residues deposited in the spinning shaft can be avoided.
  • the device and the method are also aimed at producing a highly oriented multifilament yarn.
  • melt spinning polymers are common interfering gases and / or vapors free.
  • spinning polymers containing sulfur-containing Ingredients become strong smelling and possibly even harmful gases or vapors released. This problem is particularly pronounced when spinning multifilaments, as these result from the high surface of the molten capillaries release large quantities of such harmful gases.
  • the present invention is based on the object occurring when spinning polymers to keep disturbing gases away from the environment remove.
  • Fibers made of polymers that during disruptive gases and / or vapors from spinning such fibers are within the scope of this invention to understand those during melt spinning Gases and / or vapors released in the spinning shaft be escaping into the ambient air is not desired.
  • gases and / or vapors released in the spinning shaft be escaping into the ambient air are not desired.
  • gases and / or vaporous components include, for example, the so-called “spinning smoke” and especially gas and / or vaporous components, the sulfur-containing or halogen-containing, in particular chlorine-containing, or contain components containing sulfur and halogen.
  • the polymers that make the latter gas and / or releasing vaporous constituents include sulphurous ones Polymers, such as polyarylene sulfides or polymers, the before or during spinning with halogen and / or sulfur-containing additives are.
  • the process according to the invention is preferably used in the spinning of polyarylene sulfides or in the spinning of mixtures comprising polyarylene sulfides and other thermoplastic polymers.
  • All filament-forming polymers which mainly have the recurring structural unit of the formula I can be used as polyarylene sulfides for use in the process according to the invention -Ar-S- in which Ar represents a divalent mono- or polynuclear aromatic radical, the free valences of which are in the p-position or in the m-position or in a parallel or angled position comparable to these positions.
  • the polymers can also be partially crosslinked structures as long as they can be spun under the spinning conditions defined above.
  • thermoplastics mixed with polyarylene sulfides can be used are polyester, such as polyethylene terephthalate; Poly- ⁇ -olefins, such as Polyethylene or polypropylene; partially or perfluorinated Polymers such as polytetrafluoroethylene; or to the Melting characteristics of the polyarylene sulfide customized polyether ketone.
  • Polyarylene sulfides especially polyphenylene sulfides to polymers in which Ar is a p-phenylene radical represents.
  • Preferred polyphenylene sulfides have a melt viscosity, measured at a shear rate of 1000 sec -1 ( ⁇ 1000 ), of 60 to 150 Pa * s at 320 ° C. and a melt viscosity, measured at a shear rate of 3000 sec -1 ( ⁇ 3000 ), of more than 50 Pa * s , the difference between ⁇ 1000 and ⁇ 3000 being more than 20 Pa * s .
  • the polyarylene sulfide is usually subjected to a drying process before spinning.
  • the polymer is generally dried in a finely divided form, such as powder or granule form, and in particular in the form of chips, preferably under vacuum. Usual drying times are between six and ten hours.
  • the drying temperature is usually 120 to 160 ° C , preferably 120 to 140 ° C.
  • the drying can also be carried out under inert gas.
  • a polyarylene sulfide is particularly preferably used, whose water content is at most 0.01%, measured according to the Karl Fischer method. Using this raw material can be particularly set stable spinning conditions.
  • thread-forming Polymers melt-spun, the melted Polymers using an extruder and a Spinning pump through a spinneret into a closed Spinning shaft is spun.
  • the minimum delivery rate of polymer through the spinneret is preferably 0.5 g / (min * hole). Particularly preferred delivery rates are in the range of 0.7 to 1.3 g / (min * hole).
  • the temperatures in the spinneret are usually 280 to 320 ° C., preferably 295 to 315 ° C.
  • Typical number of holes in a spinneret are in the range from 50 to 500, in particular from 100 to 500.
  • the shape of the nozzle holes can also be chosen as desired, for example triangular or rectangular, multilobal, oval or in particular round.
  • Typical diameters of the nozzle holes are in the range from 0.25 to 0.65 mm.
  • the nozzle holes are preferably in an annular nozzle arranged in the form of concentric circles.
  • the spinning takes place in a closed Spinning shaft in a gas, especially in air, or also in an inert gas such as nitrogen.
  • closed spinning shaft is to be understood in the context of this invention, a spinning shaft in which the supply and discharge of the blowing gas mainly, for example, more than 90 %, takes place via the supply and discharge lines for the blowing gas, and in which only a small part of the blowing gas leaves the spinning shaft through the outlet opening for the filaments formed.
  • This outlet opening must therefore be designed in this way be that in addition to the high penetration speed the filaments formed also a good finish to prevent the contaminated blowing air from escaping allowed inside the spinning shaft.
  • the freshly spun one Pass the thread out through a labyrinth seal or through perforated end plates, under or between which an additional auxiliary suction sucked off entrained blowing gas.
  • the spinning shaft can be operated with negative pressure, external pressure or positive pressure.
  • a slight negative pressure is maintained in the spinning shaft, preferably a negative pressure between 20 and 150 Pa, against the environment. In the event of leaks or pressure fluctuations, this variant prevents the contaminated blowing air from escaping immediately into the environment.
  • the filaments created are after extrusion through the spinneret of a forced cooling in Subjected to spinning shaft by blowing with a gas. All the usual methods of Blowing are used. In addition to the possible Cross-blowing comes especially the central blowing in question. The blowing is particularly important preferred from the inside out.
  • a gas can Inert gas, such as nitrogen. Is preferred Air.
  • the spinning take-off speed of the filaments when leaving the spinning shaft can be more than 500 m / min, preferably between 800 and 5000 m / min, and in particular 1000 to 2000 m / min.
  • Suitable adsorbents are silica gel or in particular activated carbon.
  • the adsorbents are preferably in barrel form with supply and discharge and preferably, the required Fan-provided vessels used.
  • Such Gas cleaning systems are commercially available in modular construction available.
  • the spun ones are prepared Filaments aftertreated in a manner known per se. For this purpose they become, for example, an avivation, Drawing, which may also be multi-stage can and if necessary subjected to a fixation.
  • the aftertreatment can be continued immediately after take off from the spinning machine or after an intermediate storage of the freshly spun Filaments.
  • the obtained filaments either wound or in cut into staple fibers in a known manner.
  • the invention also relates to a specially designed device according to claim 13 for carrying out the method according to the invention.
  • Preferred embodiments of the device according to the invention are defined in claims 14 to 17 .
  • thermoplastic polymer to be spun is melted via an extruder ( 1 ) and transported to a spinning pump ( 2 ).
  • the extruder is fed with polymer chips, for example.
  • the spinning pump ( 2 ) feeds the spin pack ( 3 ), which contains filters ( 4 ) and spinnerets ( 5 ).
  • the spinnerets ( 5 ) open directly into a closed spinning shaft ( 6 ) which has at least one feed line ( 7 ) and one discharge line ( 8 ) for the blowing gas.
  • 1 shows two discharge lines ( 8 ) for the blowing gas at the upper and lower ends of the spinning shaft.
  • an auxiliary suction line ( 12 ) for the blowing gas is provided in this figure 1 , which is attached to the lower end of the spinning shaft next to the outlet opening for the filaments.
  • all discharge lines for the blowing gas are equipped with a gas cleaning system ( 9 ). However, it is entirely possible to have all discharge lines lead to a gas cleaning system. The cleaned blowing air is drawn off from the gas cleaning system by pumps ( 18 ).
  • FIG. 1 a central blowing device ( 11 ) is shown in FIG. 1 , from which the blowing gas ( 10 ) flows radially from the inside out through the filaments formed.
  • blowing devices can be formed from pipes, the jacket of which has bores or other openings, such as slots or sieves, or which preferably consists of sintered metal.
  • the central blowing from the inside out is particularly advantageous because with this embodiment a particularly stable running of the filaments enables becomes.
  • the filaments ( 14 ) are prepared by means of application rollers ( 15 ), passed over a deflecting godet ( 16 ) and wound onto a spool ( 17 ). The spun filaments can then be sent for further processing.
  • the blowing gas is expediently blown into the closed spinning shaft ( 6 ) via a fan through the feed line ( 7 ).
  • At least one of the discharge lines ( 8 ) is equipped with a second fan, for example the suction line at the lower end of the spinning shaft in FIG. 1 .
  • the pressure inside the spinning shaft can be regulated via the different performance of the fans in the supply and discharge lines.
  • the spinning shaft must be used to operate the spinning system be opened during operation of the system.
  • the spinning shaft preferably has its purpose below the spinneret has a device that opens of the spinning shaft when operating the system.
  • a second powerful Suction in the area of the shaft opening under the nozzle, preferably on both sides under the Nozzle is attached when opening the shaft doors is turned on and the leakage of contaminated Blowing gas into the room in front of the shaft when open Door prevented.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)

Abstract

A process is described for producing fibres from polymers which give off troublesome gases and/or vapours during spinning, comprising the steps of: a) extruding the molten polymer through a spinneret (dies) into a closed spinning shaft (chimney, cell), b) quenching the resulting filaments in the spinning shaft with a gas, c) withdrawing the resulting filaments from the spinning shaft, d) conducting the quench gas away from the spinning shaft and introducing it into a gas purification system and e) purifying the used quench gas by contact with an adsorbent for said troublesome gases and/or vapours. It is possible by the present invention to keep hazardous gases occurring during the spinning of polymers away from the surroundings and to dispose of them. Suitable polymers are in particular polyphenylene sulphides. The invention further relates to an adapted apparatus for carrying out the process according to the invention. The apparatus comprises an extruder (1), a spinning pump (2) and a spin pack (3) which contains a filter (4) and spinnerets (5). The spinnerets (5) open out directly into a closed spinning shaft (6) which is provided with at least one feedline (7) and one discharge line (8) for the quench gas. In the representation of Figure 1, two discharge lines (8) for the quench gas are depicted at the top and bottom end of the spinning shaft. In addition, in this Figure 1, an auxiliary extraction line (12) is furnished for the quench gas which is mounted at the bottom end of the spinning shaft next to the outlet orifice for the filaments. In the representation of Figure 1, all discharge lines for the quench gas are equipped with a gas purification system (9). <IMAGE>

Description

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Fasern aus Polymeren, die während des Verspinnens störende Gase und/oder Dämpfe abgeben, umfassend die Schritte:

  • a) Extrudieren des geschmolzenen Polymeren durch eine Spinndüse in einen Spinnschacht,
  • b) Anblasen der erhaltenen Filamente im Spinnschacht mit einem Gas,
  • c) Abziehen der gebildeten Filamente aus dem Spinnschacht,
  • d) Ableitung des Anblasgases aus dem Spinnschacht, sowie eine dafür angepaßte Vorrichtung.
    • The present invention relates to a method for producing fibers from polymers which emit disruptive gases and / or vapors during spinning, comprising the steps:
  • a) extruding the molten polymer through a spinneret into a spinning shaft,
  • b) blowing the filaments obtained in the spinning shaft with a gas,
  • c) pulling off the formed filaments from the spinning shaft,
  • d) deriving the blowing gas from the spinning shaft, and a device adapted for this.

    • Schmelzspinnverfah ren von thermoplastischen Polymeren, bei denen gekapselte Spinnschächte verwendet werden, sind an sich bekannt.Melt spinning process of thermoplastic polymers, in which encapsulated spinning shafts are used are known per se.

    So wird in der EP-A-147, 173 ein Schmelzspinnverfahren von thermoplastischen Polymeren beschrieben, bei dem das Polymere in einen unter Überdruck stehenden Spinnschacht extrudiert wird und innerhalb dieses Schachtes abgekühlt wird. Ferner wird eine angepaßte Vorrichtung zur Durchführung des Verfahrens beschrieben, die eine besonders ausgestaltete Austrittsöffnung für die verfestigten, mit hoher Geschwindigkeit abgezogene Filamente aufweist und mit der eine gute Abdichtung des Spinnschachtes erreicht werden kann. Die Vorrichtung und das Verfahren zielen vor allem auf die Herstellung eines hoch orientierten Multifilamentgarnes ab.For example, EP-A-147, 173 describes a melt spinning process of thermoplastic polymers, in which the polymer is extruded into a pressurized spinning shaft and is cooled within this shaft. Furthermore, an adapted device for carrying out the method is described, which has a specially designed outlet opening for the solidified filaments drawn off at high speed and with which a good sealing of the spinning shaft can be achieved. The device and the method are primarily aimed at producing a highly oriented multifilament yarn.

    In der EP-A-205,694 wird ein Schmelzspinnverfahren von thermoplastischen Polymeren beschrieben, bei dem das Polymere in einen unter Unterdruck von weniger als 0,7 atm stehenden Spinnschacht extrudiert wird und innerhalb dieses Schachtes abgekühlt wird. Die Vorrichtung zur Durchführung dieses Verfahrens betrifft im wesentlichen die aus der EP-A-147, 173 bekannte Vorrichtung, an deren Austrittsseite für das sich im Spinnschacht befindliche Gas eine Vakuumpumpe angeschlossen ist. In der Beschreibung ist erwähnt, daß von den ersponnenen Fäden abdampfende Monomere und Oligomere durch die Gasführung aus dem Spinnschacht entfernt werden, so daß Probleme mit sich im Spinnschacht ablagernden Rückständen vermieden werden können. Die Vorrichtung und das Verfahren zielen ebenfalls auf die Herstellung eines hoch orientierten Multifilamentgarnes ab. EP-A-205,694 describes a melt spinning process of thermoplastic polymers, in which the polymer is extruded into a spinning shaft which is under a vacuum of less than 0.7 atm and is cooled within this shaft. The device for carrying out this method essentially relates to the device known from EP-A-147, 173 , to whose outlet side a vacuum pump is connected for the gas located in the spinning shaft. In the description it is mentioned that monomers and oligomers evaporating from the spun threads are removed from the spinning shaft by the gas flow, so that problems with residues deposited in the spinning shaft can be avoided. The device and the method are also aimed at producing a highly oriented multifilament yarn.

    Beim Schmelzspinnen von Polymeren werden häufig störende Gase und/oder Dämpfe frei. Insbesondere beim Verspinnen von Polymeren enthaltend schwefelhaltige Bestandteile werden stark riechende und eventuell sogar gesundheitsschädliche Gase oder Dämpfe freigesetzt. Dieses Problem tritt besonders ausgeprägt beim Verspinnen von Multifilamenten auf, da diese infolge der hohen Oberfläche der schmelzflüssigen Kapillaren große Mengen solcher schädlichen Gase freisetzen.When melt spinning polymers are common interfering gases and / or vapors free. In particular when spinning polymers containing sulfur-containing Ingredients become strong smelling and possibly even harmful gases or vapors released. This problem is particularly pronounced when spinning multifilaments, as these result from the high surface of the molten capillaries release large quantities of such harmful gases.

    Der vorliegenden Erfindung liegt die Aufgabe zugrunde, beim Verspinnen von Polymeren auftretende störende Gase von der Umgebung fernzuhalten und zu beseitigen.The present invention is based on the object occurring when spinning polymers to keep disturbing gases away from the environment remove.

    Gelöst wird diese Aufgabe dadurch, dass Polymere versponnen werden, die während des Verspinnens schwefel- und/oder halogenhaltige Gase und/oder Dämpfe abgeben, daß die Extrusion des geschmolzenen Polymeren durch eine Spinndüse in einen geschlossenen Spinnschacht erfolgt, daß das Anblasgas und diese Gase und/oder Dämpfe gemäß Schritt d) aus dem geschlossenen Spinnschacht abgeleitet in ein Gasreinigungssystem eingeleitet und durch Kontakt mit einem Adsorptionsmittel von den Gasen und/oder Dämpfen gereinigt wird.This task is solved by the fact that Polymers are spun that during the spinning sulfur and / or halogen-containing gases and / or emit vapors, that the extrusion of the melted Polymers through a spinneret into one closed spinning shaft takes place that the blowing gas and these gases and / or vapors according Step d) derived from the closed spinning shaft in a gas cleaning system initiated and by contact with an adsorbent of the gases and / or vapors is cleaned.

    Unter dem Begriff "Fasern aus Polymeren, die während des Verspinnens störende Gase und/oder Dämpfe abgeben" sind im Rahmen dieser Erfindung solche Fasern zu verstehen, bei denen während des Schmelzspinnens im Spinnschacht Gase und/oder Dämpfe freigesetzt werden, deren Entweichen in die Umgebungsluft nicht erwünscht ist. Dazu zählen beispielsweise der sogenannte "Spinnrauch" und insbesondere gas- und/ oder dampfförmige Bestandteile, die schwefelhaltige oder halogenhaltige, insbesondere chlorhaltige, oder schwefel- und halogenhaltige Komponenten enthalten. Zu den Polymeren, die diese letzteren gas- und/oder dampfförmigen Bestandteile abgeben, zählen schwefelhaltige Polymere, wie Polyarylensulfide oder Polymere, die vor oder während des Verspinnens mit halogen-und/oder schwefelhaltigen Zusätzen versehen worden sind.Under the term "fibers made of polymers that during disruptive gases and / or vapors from spinning such fibers are within the scope of this invention to understand those during melt spinning Gases and / or vapors released in the spinning shaft be escaping into the ambient air is not desired. These include, for example, the so-called "spinning smoke" and especially gas and / or vaporous components, the sulfur-containing or halogen-containing, in particular chlorine-containing, or contain components containing sulfur and halogen. The polymers that make the latter gas and / or releasing vaporous constituents include sulphurous ones Polymers, such as polyarylene sulfides or polymers, the before or during spinning with halogen and / or sulfur-containing additives are.

    Bevorzugt setzt man das erfindungsgemäße Verfahren beim Verspinnen von Polyarylensulfiden oder beim Verspinnen von Mischungen enthaltend Polyarylensulfide und andere thermoplastische Polymere ein. Als Polyarylensulfide für den Einsatz im erfindungsgemäßen Verfahren lassen sich alle fadenbildenden Polymeren einsetzen, die hauptsächlich die wiederkehrende Struktureinheit der Formel I aufweisen -Ar-S- worin Ar einen zweiwertigen ein- oder mehrkernigen aromatischen Rest darstellt, dessen freie Valenzen sich in p-Stellung oder in m-Stellung oder in einer zu diesen Stellungen vergleichbaren parallelen oder gewinkelten Stellung zueinander befinden. Bei den Polymeren kann es sich auch um teilweise vernetzte Strukturen handeln, solange diese unter den oben definierten Spinnbedingungen verspinnbar sind.The process according to the invention is preferably used in the spinning of polyarylene sulfides or in the spinning of mixtures comprising polyarylene sulfides and other thermoplastic polymers. All filament-forming polymers which mainly have the recurring structural unit of the formula I can be used as polyarylene sulfides for use in the process according to the invention -Ar-S- in which Ar represents a divalent mono- or polynuclear aromatic radical, the free valences of which are in the p-position or in the m-position or in a parallel or angled position comparable to these positions. The polymers can also be partially crosslinked structures as long as they can be spun under the spinning conditions defined above.

    Es können auch Mischungen von Polyarylensulfidpolymeren eingesetzt werden, oder Polyarylensulfidpolymere, die in einem Molekül unterschiedliche wiederkehrende Struktureinheiten der Formel I aufweisen. Beispiele für Mischungen von Polyarylensulfiden sind in der EP-A-407,887 aufgeführt, deren Inhalt auch Gegenstand der vorliegenden Beschreibung ist.Mixtures of polyarylene sulfide polymers or polyarylene sulfide polymers which have different recurring structural units of the formula I in one molecule can also be used. Examples of mixtures of polyarylene sulfides are listed in EP-A-407,887 , the content of which is also the subject of the present description.

    Beispiele für Thermoplaste, die im Gemisch mit Polyarylensulfiden eingesetzt werden können, sind Polyester, wie Polyethylenterephthalat; Poly-α-olefine, wie Polyethylen oder Polypropylen; teil- oder perfluorierte Polymere, wie Polytetrafluorethylen; oder an die Schmelzcharakteristik des Polyarylensulfids angepaßtes Polyetherketon.Examples of thermoplastics mixed with polyarylene sulfides can be used are polyester, such as polyethylene terephthalate; Poly-α-olefins, such as Polyethylene or polypropylene; partially or perfluorinated Polymers such as polytetrafluoroethylene; or to the Melting characteristics of the polyarylene sulfide customized polyether ketone.

    Vorzugsweise handelt es sich bei den eingesetzten Polyarylensulfiden um Polyphenylensulfide, insbesondere um Polymere, bei denen Ar einen p-Phenylenrest darstellt.It is preferably the ones used Polyarylene sulfides, especially polyphenylene sulfides to polymers in which Ar is a p-phenylene radical represents.

    Bevorzugte Polyphenylensufide weisen bei 320°C eine Schmelzviskosität, gemessen mit einer Schergeschwindigkeit von 1000 sec-1 (η1000), von 60 bis 150 Pa*s auf und eine Schmelzviskosität, gemessen mit einer Schergeschwindigkeit von 3000 sec-1 (η3000), von mehr als 50 Pa*s auf, wobei die Differenz von η1000 und η3000 mehr als 20 Pa*s beträgt.Preferred polyphenylene sulfides have a melt viscosity, measured at a shear rate of 1000 sec -1 (η 1000 ), of 60 to 150 Pa * s at 320 ° C. and a melt viscosity, measured at a shear rate of 3000 sec -1 (η 3000 ), of more than 50 Pa * s , the difference between η 1000 and η 3000 being more than 20 Pa * s .

    Das Polyarylensulfid wird vor dem Verspinnen üblicherweise einem Trocknungsprozess unterzogen. Dazu wird das Polymere im allgemeinen in feinverteilter Form, wie Pulver- oder Granulatform und insbesondere in Form von Schnitzeln bevorzugt unter Vakuum getrocknet. Übliche Trocknungszeiten liegen zwischen sechs bis zehn Stunden. Die Trocknungstemperatur beträgt üblicherweise 120 bis 160°C, vorzugsweise 120 bis 140°C. Die Trocknung kann aber auch unter Inertgas vorgenommen werden.The polyarylene sulfide is usually subjected to a drying process before spinning. For this purpose, the polymer is generally dried in a finely divided form, such as powder or granule form, and in particular in the form of chips, preferably under vacuum. Usual drying times are between six and ten hours. The drying temperature is usually 120 to 160 ° C , preferably 120 to 140 ° C. The drying can also be carried out under inert gas.

    Besonders bevorzugt wird ein Polyarylensulfid eingesetzt, dessen Wassergehalt höchstens 0,01 %, gemessen nach der Methode nach Karl-Fischer, beträgt. Unter Einsatz dieses Rohmaterials lassen sich besonders stabile Spinnbedingungen einstellen.A polyarylene sulfide is particularly preferably used, whose water content is at most 0.01%, measured according to the Karl Fischer method. Using this raw material can be particularly set stable spinning conditions.

    Im erfindungsgemäßen Verfahren werden fadenbildende Polymere schmelzgesponnen, wobei das geschmolzene Polymere mittels eines Extruders und einer Spinnpumpe durch eine Spinndüse in einen geschlossenen Spinnschacht versponnen wird.In the method according to the invention, thread-forming Polymers melt-spun, the melted Polymers using an extruder and a Spinning pump through a spinneret into a closed Spinning shaft is spun.

    Vorzugsweise beträgt die Mindestförderleistung an Polymer durch die Spinndüse 0,5 g/(min*Loch). Besonders bevorzugte Förderleistungen liegen im Bereich von 0,7 bis 1,3 g/(min*Loch).The minimum delivery rate of polymer through the spinneret is preferably 0.5 g / (min * hole). Particularly preferred delivery rates are in the range of 0.7 to 1.3 g / (min * hole).

    Im Falle des bevorzugten Polyphenylensulfids betragen die Temperaturen in der Spinndüse üblicherweise 280 bis 320°C, vorzugsweise 295 bis 315°C.In the case of the preferred polyphenylene sulfide, the temperatures in the spinneret are usually 280 to 320 ° C., preferably 295 to 315 ° C.

    Es können beliebige Spinndüsen eingesetzt werden. Typische Lochzahlen einer Spinndüse liegen im Bereich von 50 bis 500, insbesondere von 100 bis 500. Die Form der Düsenlöcher kann ebenfalls beliebig gewählt werden, beispielsweise drei- oder rechteckig, multilobal, oval oder insbesondere rund. Typische Durchmesser der Düsenlöcher liegen im Bereich von 0,25 bis 0,65 mm.Any spinnerets can be used. Typical number of holes in a spinneret are in the range from 50 to 500, in particular from 100 to 500. The shape of the nozzle holes can also be chosen as desired, for example triangular or rectangular, multilobal, oval or in particular round. Typical diameters of the nozzle holes are in the range from 0.25 to 0.65 mm.

    Vorzugsweise sind die Düsenlöcher in einer Ringdüse in Form von konzentrischen Kreisen angeordnet.The nozzle holes are preferably in an annular nozzle arranged in the form of concentric circles.

    Das Verspinnen erfolgt in einen geschlossenen Spinnschacht in ein Gas, insbesondere in Luft, oder auch in ein Inertgas, wie Stickstoff.The spinning takes place in a closed Spinning shaft in a gas, especially in air, or also in an inert gas such as nitrogen.

    Unter dem Begriff "geschlossener Spinnschacht" ist im Rahmen dieser Erfindung ein Spinnschacht zu verstehen, bei dem die Zu- und Ableitung des Anblasgases hauptsächlich, beispielsweise zu mehr als 90 %, über die Zuführ- und die Abführleitungen für das Anblasgas erfolgt, und bei dem nur ein geringer Teil des Anblasgases durch die Austrittsöffnung für die gebildeten Filamente den Spinnschacht verläßt.The term "closed spinning shaft" is to be understood in the context of this invention, a spinning shaft in which the supply and discharge of the blowing gas mainly, for example, more than 90 %, takes place via the supply and discharge lines for the blowing gas, and in which only a small part of the blowing gas leaves the spinning shaft through the outlet opening for the filaments formed.

    Diese Austrittsöffnung muß daher so ausgestaltet sein, daß sie neben der hohen Durchtrittsgeschwindigkeit der gebildeten Filamente auch einen guten Abschluß gegen einen Austritt der verunreinigten Anblasluft im Inneren des Spinnschachtes gestattet.This outlet opening must therefore be designed in this way be that in addition to the high penetration speed the filaments formed also a good finish to prevent the contaminated blowing air from escaping allowed inside the spinning shaft.

    So läßt sich beispielsweise der frisch ersponnene Faden durch eine Labyrinthdichtung nach außen führen oder durch durchlochte Abschlußplatten, unter oder zwischen denen eine zusätzliche Hilfsabsaugung das mitgerissene Anblasgas absaugt.For example, the freshly spun one Pass the thread out through a labyrinth seal or through perforated end plates, under or between which an additional auxiliary suction sucked off entrained blowing gas.

    Der Spinnschacht kann mit Unterdruck, Außendruck oder Überdruck betrieben werden. Vorteilhafterweise wird im Spinnschacht ein geringer Unterdruck aufrechterhalten, vorzugsweise ein Unterdruck zwischen 20 und 150 Pa, gegen die Umgebung. Diese Variante verhindert bei Undichtigkeiten bzw. bei Druckschwankungen ein sofortiges Ausströmen der verunreinigten Anblasluft in die Umgebung.The spinning shaft can be operated with negative pressure, external pressure or positive pressure. Advantageously, a slight negative pressure is maintained in the spinning shaft, preferably a negative pressure between 20 and 150 Pa, against the environment. In the event of leaks or pressure fluctuations, this variant prevents the contaminated blowing air from escaping immediately into the environment.

    Die erzeugten Filamente werden nach dem Extrudieren durch die Spinndüse einer Zwangsabkühlung im Spinnschacht durch Anblasen mit einem Gas unterworfen. Dabei können alle an sich üblichen Verfahren des Anblasens zum Einsatz kommen. Neben der möglichen Queranblasung kommt insbesondere die zentrale Anblasung in Frage. Davon ist insbesondere die Anblasung von innen nach außen bevorzugt. Als Gas kann Inertgas, wie Stickstoff eingesetzt werden. Bevorzugt ist Luft.The filaments created are after extrusion through the spinneret of a forced cooling in Subjected to spinning shaft by blowing with a gas. All the usual methods of Blowing are used. In addition to the possible Cross-blowing comes especially the central blowing in question. The blowing is particularly important preferred from the inside out. As a gas can Inert gas, such as nitrogen. Is preferred Air.

    Die Spinnabzugsgeschwindigkeit der Filamente beim Verlassen des Spinnschachts kann mehr als 500 m/min betragen, vorzugsweise zwischen 800 und 5000 m/min, und insbesondere 1000 bis 2000 m/min.The spinning take-off speed of the filaments when leaving the spinning shaft can be more than 500 m / min, preferably between 800 and 5000 m / min, and in particular 1000 to 2000 m / min.

    Zweckmäßigerweise bringt man auf die Filamente beim Verlassen des Spinnschachtes eine übliche Verstreckpräparation auf. Dies kann kurz vor, während oder kurz nach dem Verlassen des Spinnschachtes erfolgen. Die Präparation kann aber auch anderen Stellen der Produktionsanlage aufgebracht werden. Das Aufbringen der Präparation kann mit allen dafür bekannten Mitteln erfolgen, beispielsweise durch Aufsprühen oder durch Aufbringen mit einer Präparationsrolle.Expediently you bring on the filaments a usual stretching preparation when leaving the spinning shaft on. This can happen just before, during or shortly after leaving the spinning shaft. The preparation can also be used in other areas of the body Production plant are applied. The application the preparation can be done with all known means take place, for example by spraying or by applying with a preparation roller.

    Das mit schwefelhaltigen Gasen und/oder Dämpfen beladene Anblasgas wird aus dem Spinnschacht über eine oder mehrere Abführleitungen einem Gasreinigungssystem zugeführt. Es hat sich gezeigt, daß die verbrauchte Anblasluft durch Kontakt mit einem Adsorptionsmittel für besagte störende Gase und/oder Dämpfe gereinigt werden muß.That with gases and / or vapors containing sulfur loaded blowing gas is over from the spinning shaft one or more discharge lines to a gas cleaning system fed. It has been shown that the used blowing air through contact with an adsorbent for said disruptive gases and / or vapors must be cleaned.

    Beispiele für geeignete Adsorptionsmittel sind Silicagel oder insbesondere Aktivkohle. Die Adsorptionsmittel werden bevorzugt in faßförmigen mit Zu- und Ableitung und vorzugsweise, dem erforderlichen Ventilator versehenen Gefäßen eingesetzt. Solche Gasreinigungssysteme sind im Handel in Modulbauweise erhältlich.Examples of suitable adsorbents are silica gel or in particular activated carbon. The adsorbents are preferably in barrel form with supply and discharge and preferably, the required Fan-provided vessels used. Such Gas cleaning systems are commercially available in modular construction available.

    Nach dem Verlassen des Spinnschachtes und gegebenenfalls dem Präparieren werden die ersponnenen Filamente in an sich bekannter Weise nachbehandelt. Dazu werden sie beispielsweise einer Avivierung, einer Verstreckung, die gegebenenfalls auch mehrstufig sein kann und gegebenenfalls einer Fixierung unterworfen. Die Nachbehandlung kann kontinuierlich direkt nach dem Abziehen aus der Spinnmaschine erfolgen oder nach einer Zwischenlagerung der frisch ersponnenen Filamente.After leaving the spinning shaft and if necessary the spun ones are prepared Filaments aftertreated in a manner known per se. For this purpose they become, for example, an avivation, Drawing, which may also be multi-stage can and if necessary subjected to a fixation. The aftertreatment can be continued immediately after take off from the spinning machine or after an intermediate storage of the freshly spun Filaments.

    Am Ende der Nachbehandlungsstufe werden die erhaltenen Filamente entweder aufgespult oder in an sich bekannter Weise zu Stapelfasern zerschnitten.At the end of the post-treatment stage, the obtained filaments either wound or in cut into staple fibers in a known manner.

    Die Erfindung betrifft auch eine besonders ausgestaltete Vorrichtung gemäß Anspruch 13 zur Durchführung des erfindungsgemäßen Verfahrens. Bevorzugte Ausführungsformen der erfindungsgemäßen Vorrichtung sind in den Ansprüchen 14 bis 17 definiert.The invention also relates to a specially designed device according to claim 13 for carrying out the method according to the invention. Preferred embodiments of the device according to the invention are defined in claims 14 to 17 .

    In Figur 1 ist ein Beispiel einer erfindungsgemäßen Vorrichtung dargestellt. Das zu verspinnende thermoplastische Polymere wird über einen Extruder (1) aufgeschmolzen und zu einer Spinnpumpe (2) transportiert. Der Extruder wird beispielsweise mit Polymerschnitzeln beschickt. Die Spinnpumpe (2) speist das Spinnpack (3), welches Filter (4) und Spinndüsen (5) enthält. Die Spinndüsen (5) münden direkt in einen geschlossenen Spinnschacht (6), welcher zumindest eine Zuführleitung (7) und eine Abführleitung (8) für das Anblasgas aufweist. In der Darstellung der Figur 1 sind zwei Abführleitungen (8) für das Anblasgas am oberen und am unteren Ende des Spinnschachtes dargestellt. Zusätzlich ist in dieser Figur 1 noch eine Hilfsabsaugleitung (12) für das Anblasgas vorgesehen, die am unteren Ende des Spinnschachtes neben der Austrittsöffnung für die Filamente angebracht ist. In der Darstellung der Figur 1 sind sämtliche Abführleitungen für das Anblasgas mit einem Gasreinigungssystem (9) ausgestattet. Es ist aber durchaus möglich, alle Abführleitungen in ein Gasreinigungssystem münden zu lassen. Aus dem Gasreinigungssystem wird die gereinigte Anblasluft über Pumpen (18) abgezogen.An example of a device according to the invention is shown in FIG. The thermoplastic polymer to be spun is melted via an extruder ( 1 ) and transported to a spinning pump ( 2 ). The extruder is fed with polymer chips, for example. The spinning pump ( 2 ) feeds the spin pack ( 3 ), which contains filters ( 4 ) and spinnerets ( 5 ). The spinnerets ( 5 ) open directly into a closed spinning shaft ( 6 ) which has at least one feed line ( 7 ) and one discharge line ( 8 ) for the blowing gas. 1 shows two discharge lines ( 8 ) for the blowing gas at the upper and lower ends of the spinning shaft. In addition, an auxiliary suction line ( 12 ) for the blowing gas is provided in this figure 1 , which is attached to the lower end of the spinning shaft next to the outlet opening for the filaments. In the illustration in FIG. 1 , all discharge lines for the blowing gas are equipped with a gas cleaning system ( 9 ). However, it is entirely possible to have all discharge lines lead to a gas cleaning system. The cleaned blowing air is drawn off from the gas cleaning system by pumps ( 18 ).

    Ferner ist in Figur 1 eine zentrale Anblasvorrichtung (11) dargestellt, von welcher das Anblasgas (10) radial von innen nach außen durch die gebildeten Filamente strömt. Solche Anblasvorrichtungen können aus Rohren gebildet werden, deren Mantel Bohrungen oder andere Öffnungen, wie Schlitze oder Siebe aufweisen oder der vorzugsweise aus Sintermetall besteht.Furthermore, a central blowing device ( 11 ) is shown in FIG. 1 , from which the blowing gas ( 10 ) flows radially from the inside out through the filaments formed. Such blowing devices can be formed from pipes, the jacket of which has bores or other openings, such as slots or sieves, or which preferably consists of sintered metal.

    Die zentrale Anblasung von innen nach außen ist besonders vorteilhaft, da mit dieser Ausführungsform ein besonders stabiler Lauf der Filamente ermöglicht wird.The central blowing from the inside out is particularly advantageous because with this embodiment a particularly stable running of the filaments enables becomes.

    Nach dem Verlassen des Spinnschachtes durch die Austrittsöffnung (13) werden die Filamente (14) mittels Auftragsrollen (15) präpariert, über eine Umlenkgalette (16) geführt und auf eine Spule (17) aufgespult. Die ersponnenen Filamente können anschließend einer Weiterverarbeitung zugeführt werden.After leaving the spinning shaft through the outlet opening ( 13 ), the filaments ( 14 ) are prepared by means of application rollers ( 15 ), passed over a deflecting godet ( 16 ) and wound onto a spool ( 17 ). The spun filaments can then be sent for further processing.

    Zur Steuerung des Druckes innerhalb des Spinnschachtes wird das Anblasgas zweckmäßigerweise über einen Ventilator durch die Zuführleitung (7) in den geschlossenen Spinnschacht (6) eingeblasen. Mindestens eine der Abführleitungen (8) ist mit einem zweiten Ventilator ausgestattet, beispielsweise die Absaugleitung am unteren Ende des Spinnschachtes in der Figur 1. Im Normalbetrieb läßt sich der Druck im Innern des Spinnschachtes über die unterschiedliche Leistung der Ventilatoren in der Zu- und Abführleitung regulieren.In order to control the pressure inside the spinning shaft, the blowing gas is expediently blown into the closed spinning shaft ( 6 ) via a fan through the feed line ( 7 ). At least one of the discharge lines ( 8 ) is equipped with a second fan, for example the suction line at the lower end of the spinning shaft in FIG. 1 . In normal operation, the pressure inside the spinning shaft can be regulated via the different performance of the fans in the supply and discharge lines.

    Zum Bedienen der Spinnanlage muß der Spinnschacht im Betrieb der Anlage geöffnet werden. Zu diesem Zweck weist der Spinnschacht vorzugsweise unterhalb der Spinndüse eine Vorrichtung auf, die ein Öffnen des Spinnschachtes beim Betrieb der Anlage gestattet. Um einen Austritt von verunreinigtem Anblasgas zu verhindern, ist es zweckmäßig, wenn eine zweite leistungsstarke Absaugung im Bereich der Schachtöffnung unter der Düse, vorzugsweise beidseitig unter der Düse angebracht wird, die beim Öffnen der Schachttüren eingeschaltet wird und den Austritt von verunreinigtem Anblasgas in den Raum vor dem Schacht bei offener Türe verhindert.The spinning shaft must be used to operate the spinning system be opened during operation of the system. To this The spinning shaft preferably has its purpose below the spinneret has a device that opens of the spinning shaft when operating the system. To prevent contaminated blowing gas from escaping To prevent it is useful if a second powerful Suction in the area of the shaft opening under the nozzle, preferably on both sides under the Nozzle is attached when opening the shaft doors is turned on and the leakage of contaminated Blowing gas into the room in front of the shaft when open Door prevented.

    Claims (17)

    1. A process for producing fibers from polymers which give off troublesome gases and/or vapors during spinning, comprising the steps of:
      a) extruding the molten polymer through a spinneret into a spinning shaft,
      b) quenching the resulting filaments in the spinning shaft with a gas,
      c) taking off the resulting filaments from the spinning shaft,
      d) conducting the quench gas away from the spinning shaft,
      which comprises the polymers which give off sulfur-and/or halogen-containing gases and/or vapors during spinning being spun, the extrusion of the molten polymer being performed through a spinneret into a closed spinning shaft and the quench gas and said gases and/or vapors being conducted away from the closed spinning shaft according to step d), being introduced into a gas purification system and being purified by contact with an adsorbent from said gases and/or vapors.
    2. The process as claimed in claim 1, wherein the polymer is a polyarylene sulfide or a mixture of polyarylene sulfides or a mixture of polyarylene sulfide and other thermoplastic polymers.
    3. The process as claimed in claim 2, wherein the polyarylene sulfide is p-polyphenylene sulfide or a mixture of p-polyphenylene sulfides.
    4. The process as claimed in claim 2, wherein polyphenylene sulfides are used which have, at 320°C, a melt viscosity, measured at a shear rate of 1000 sec-1 (η1000), of 60 to 150 Pa*s and a melt viscosity, measured at a shear rate of 3000 sec-1 (η3000), of more than 50 Pa*s, the difference between η1000 and η3000 being more than 20 Pa*s.
    5. The process as claimed in claim 2, wherein the polyarylene sulfide is dried in a finely divided form prior to spinning.
    6. The process as claimed in claim 5, wherein the drying is performed under vacuum and the drying is carried out until a water content of the polymer of at most 0.01%, measured by the Karl-Fischer method, is achieved.
    7. The process as claimed in claim 1, wherein the spinnerets have more than 100 spinneret holes, which are preferably arranged in concentric circles.
    8. The process as claimed in claim 1, wherein a reduced pressure is maintained in the spinning shaft, in particular a pressure reduced by between 20 and 150 Pa, with respect to the surroundings.
    9. The process as claimed in claim 1, wherein a transport rate of the polymer through the spinneret of at least 0.5 g/(min*hole) is selected.
    10. The process as claimed in claim 1, wherein the spun filaments are taken off from the spinning shaft at a velocity of more than 500 m/min, in particular from 800 to 3000 m/min.
    11. The process as claimed in claim 1, wherein the quench gas flows radially onto the spun filaments, the quench being performed in particular from the inside to the outside.
    12. The process as claimed in claim 1, wherein the adsorbent for said troublesome gases and/or vapors is activated charcoal.
    13. An apparatus for carrying out the process as claimed in claims 1 to 12 for producing melt-spun filaments, in particular multifilaments composed of polymers which give off troublesome gases and/or vapors during spinning, comprising extruder (1), spinning pump (2) and spin pack (3) composed of filter (4) and spinnerets (5) which open out into a closed spinning shaft (6), which is provided with at least one feedline (7) and one discharge line (8) for the quench gas, in which at least one said discharge line (8) opens out into a gas purification system (9), in which the quench gas (10) is purified from said gases and/or vapors.
    14. The apparatus as claimed in claim 13, wherein the feedline (7) opens out into a central quench apparatus (11), from which the quench gas (10) flows radially from the inside to the outside through the filaments formed.
    15. The apparatus as claimed in claim 13, wherein extraction lines (8) for the quench gas are each provided at the top and bottom ends of the spinning shaft (6), which open out into a gas purification system (9) or each of which opens out into a gas purification system (9).
    16. The apparatus as claimed in claim 13, wherein next to the outlet orifice for the filaments at the bottom end of the spinning shaft is provided an additional auxiliary extraction line (12) for the quench gas, which opens out into a gas purification system (9).
    17. The apparatus as claimed in claim 15, wherein the spinning shaft, beneath the spinneret, has an apparatus which permits the spinning shaft to be opened during operation of the plant and the extraction lines (8), situated at the top end of the spinning shaft (6), for the quench gas are furnished with a powerful extractor which is turned on when the shaft doors are opened and prevents the exit of contaminated quench gas into the space in front of the shaft when the doors are open.
    EP93111453A 1992-07-25 1993-07-16 Process and apparatus for the production of fibres, which give off gases and/or vapours during their spinning Expired - Lifetime EP0581145B2 (en)

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    DE4224707 1992-07-25
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    US5935512A (en) * 1996-12-30 1999-08-10 Kimberly-Clark Worldwide, Inc. Nonwoven process and apparatus
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    KR100391706B1 (en) * 2001-01-29 2003-07-12 덕산공조기계주식회사 Ventilation system for fiber ejector
    KR100468086B1 (en) * 2002-12-04 2005-01-26 난야 플라스틱스 코오퍼레이션 Method for manufacturing fine denier polyester hollow pre-oriented yarn and the yarn manufactured from the same
    KR20040049722A (en) * 2002-12-07 2004-06-12 난야 플라스틱스 코오퍼레이션 Method for manufacturing polyester fine dinier multifilaments and the multifilaments manufactured from the same
    US6926854B2 (en) * 2003-06-25 2005-08-09 Nan Ya Plastics Corporation Process of making polyester fine denier multifilament
    BRPI0608521A2 (en) * 2005-03-18 2017-07-25 Diolen Ind Fibers Bv PROCESS FOR PRODUCING A POLYPHENYLENE SULPHIDE MULTIFILAMENT YARN, POLYPHENYLENE SULPHIDE MULTIFILAMENT YARN, AND USE THEREOF

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    EP0581145B1 (en) 1997-10-08
    DK0581145T3 (en) 1998-05-18
    EP0581145A2 (en) 1994-02-02
    US5370833A (en) 1994-12-06
    EP0581145A3 (en) 1994-08-10
    ATE159057T1 (en) 1997-10-15
    ES2110033T5 (en) 2001-09-01
    DE59307483D1 (en) 1997-11-13
    DK0581145T4 (en) 2001-11-12
    JPH06158414A (en) 1994-06-07
    GR3025234T3 (en) 1998-02-27

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