EP0817873B1 - Method of producing cellulose fibres - Google Patents
Method of producing cellulose fibres Download PDFInfo
- Publication number
- EP0817873B1 EP0817873B1 EP96908070A EP96908070A EP0817873B1 EP 0817873 B1 EP0817873 B1 EP 0817873B1 EP 96908070 A EP96908070 A EP 96908070A EP 96908070 A EP96908070 A EP 96908070A EP 0817873 B1 EP0817873 B1 EP 0817873B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- coagulation
- spinning solution
- process according
- zone
- cellulose fibers
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Revoked
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 15
- 230000015271 coagulation Effects 0.000 claims abstract description 71
- 238000005345 coagulation Methods 0.000 claims abstract description 71
- 238000009987 spinning Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 238000007654 immersion Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000004804 winding Methods 0.000 claims abstract description 11
- 229920002678 cellulose Polymers 0.000 claims abstract description 7
- 239000001913 cellulose Substances 0.000 claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims abstract 2
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 150000001204 N-oxides Chemical class 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- 239000000835 fiber Substances 0.000 description 10
- 239000012530 fluid Substances 0.000 description 7
- 230000001133 acceleration Effects 0.000 description 5
- 238000003860 storage Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 241000157282 Aesculus Species 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 235000010181 horse chestnut Nutrition 0.000 description 1
Images
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
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
Definitions
- the invention relates to a method for producing cellulosic fibers by extruding a dissolved cellulose containing spinning solution in a gaseous medium a predetermined gas route, then immersed in and passing through a coagulation bath over a predetermined one Coagulation section, drawing of the cellulose fibers obtained and winding up.
- Such a method is for example from DE-A-4409609 known.
- the spinning solution is made after passing through the gas section immersed in a standing coagulation bath, which then accelerated together with the spinning solution.
- the acceleration of the coagulation bath takes place via a Bottom tapered spinning funnel.
- Such a Spinning funnel has the disadvantage that the piecing of the Spinning solution causes big problems.
- the achievable winding speed is maximum according to the examples 150 m / min, so that this known method is not particularly is economical.
- the object of the present invention is another Spinning process for the production of cellulosic fibers for To make available which works more economically.
- it should at least address the disadvantages described above reduce.
- cellulosic fibers are provided, which also at winding speeds above 1000 m / min sensitive cellulosic spinning solutions, such as it for solutions of cellulose in a water containing N-oxide of a tertiary amine, especially N-methylmorpholine -N-oxide (NMMO), the case is a stable Process supplies.
- NMMO N-methylmorpholine -N-oxide
- This task is achieved in the method mentioned at the outset solved that the extruded spinning solution after the gas line accelerated to a predetermined speed, at least approximately in the direction of the extruded spinning solution laminar flowing coagulation bath is introduced, with the coagulation liquid laterally in the path of the Spinning solution is supplied and the direction of flow of the spinning solution and the coagulation liquid over the entire coagulation distance is kept at least approximately in parallel, and that the cellulose fibers obtained on leaving the The coagulation path is laterally deflected and then wound up become.
- the lateral laminar supply of the coagulation liquid can be achieved in a simple manner in that the one Side of a storage container for the coagulation liquid is designed as an overflow, the overflow being such is formed that the coagulation liquid on the one hand flows along the formation and on the other hand the Coagulation liquid from the horizontal in the flow direction redirects the spinning solution.
- This shape can be done in simple Fall in the form of a quarter circle or parabola have, but it must be ensured that from Run out until the transition to the direction of flow of the spinning solution a constant curve is formed to ensure that turbulence largely avoided, so that the spinning solution Immerse in a laminar coagulation fluid stream can.
- the lower edge of the Overflow can be used to the resulting redirect cellulosic thread by a sideways offset take-up of the resulting thread over the lower edge of the overflow is drawn.
- the method according to the invention is suitable for production of fibers, the term fibers being monofilaments, Multifilament threads, but also hollow threads can be understood.
- the process is also equally suitable for the production of porous ones Fibers suitable.
- the fibers can have a round cross-section, but also have a profiled cross section.
- the production of cellulosic fibers according to the invention succeeds excellent if the coagulation fluid is one-sided of the spinning solution in a constant layer thickness in the range from 1.0 to 5 mm is supplied.
- the layer thickness is about 1 to 3 times as thick is set as the largest diameter of the extruded Spinning solution.
- the speed of the coagulation liquid at the immersion point of the spinning solution to a value between 30 and 200 m / min, preferably between 50 and 80 m / min is, the production of the cellulosic fibers then works particularly well when the coagulation path is on a Length of 0.5 to 8 cm, preferably to a length of 1 to 4 cm.
- the speed at the immersion point can be seen at the above procedure described in more detail by the height difference between the liquid level in the reservoir and the Immersion point of the spinning solution, the point at which the overflow in the flow direction of the spinning solution, determine.
- the speed prevailing at the immersion point is determined then from the root of the product of two times gravitational acceleration times height difference (which multiplied by itself So speed corresponds to the product twice the acceleration of gravity multiplied by the difference in altitude). If such an overflow is used, the coagulation path becomes in a simple way over the route of the Overflow determined between the immersion point and the lower edge of the overflow.
- the cellulose fibers obtained after the coagulation route so suddenly from the direction of flow of the coagulation liquid are deflected that they are in the deflection area a radius of 0.2 to 2 mm, preferably a radius between 0.3 and 1 mm. This can be done with the above Overflow can be achieved in that the lower edge the overflow is provided with a corresponding radius.
- the invention is based on a figure and the following Examples explained in more detail.
- 1 represents a spinneret, from which a spinning solution 2 into a gas, for example Ambient air is spun, which is then in a downward flowing coagulation liquid is immersed in this remains until the deflection point 4, after which the meantime coagulated thread 5 suddenly in the direction of the winding 6 is deflected and then via the winding device 6, for example, on a not shown separately the reel located, is wound up.
- a spinning solution 2 into a gas for example Ambient air is spun
- a downward flowing coagulation liquid is immersed in this remains until the deflection point 4, after which the meantime coagulated thread 5 suddenly in the direction of the winding 6 is deflected and then via the winding device 6, for example, on a not shown separately the reel located, is wound up.
- the Sudden deflection at the deflection point 4 flows far predominant part of the coagulation fluid down continue (see stream 10 with arrow), so that at least thread 5 most of the coagulation fluid is removed. It has turned out here that it is favorable if the
- a reservoir 8 is provided for the coagulation liquid 7 provided a constant in the means not shown Amount of coagulation liquid supplied as free of turbulence as possible becomes.
- the coagulation liquid 7/3 at the immersion point is the Storage container 8 of the coagulation liquid 7 to the direction of flow the spinning solution 2 is limited by an overflow 9, being by the constant and constant addition of Coagulation liquid 7 in the reservoir 8 itself certain thickness of the flowing to the spinning solution 2, at least predominantly laminar coagulation fluid flow.
- Determining the speed at which the coagulating fluid at the immersion point of the spinning solution 2 results from the height difference h between the liquid level the coagulation liquid 7 in the reservoir 8 and the transition of the curve of the overflow 9 to the vertical Arrangement.
- the speed is calculated the coagulation liquid at the immersion point about the root of the product of two times gravitational acceleration times height difference h.
- the spinning solution used contains 15% cellulose, 10% water and 75% NMMMO, which was obtained from pulp V65, to be obtained from Buckeye, in the manner known for the production of NMMO spinning solutions.
- the spinning solution kept at a temperature of 120 ° C was spun in air.
- the nozzle hole diameter of the spinneret used was 200 ⁇ m, the mass flow m given in the table being extruded through the spinneret.
- V sp is therefore the maximum possible winding speed at which no breakage occurred during the manufacture of the threads.
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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)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung von cellulosischen Fasern durch Extrudieren einer gelöste Cellulose enthaltenden Spinnlösung in ein gasförmiges Medium über eine vorbestimmte Gasstrecke, anschließendem Eintauchen in und Führen durch ein Koagulationsbad über eine vorbestimmte Koagulationsstrecke, Verstrecken der erhaltenen Cellulosefasern und Aufwickeln.The invention relates to a method for producing cellulosic fibers by extruding a dissolved cellulose containing spinning solution in a gaseous medium a predetermined gas route, then immersed in and passing through a coagulation bath over a predetermined one Coagulation section, drawing of the cellulose fibers obtained and winding up.
Ein derartiges Verfahren ist beispielsweise aus DE-A-4409609 bekannt. Die Spinnlösung wird nach dem Durchlaufen der GasStrecke in ein stehendes Koagulationsbad eingetaucht, welches dann zusammen mit der Spinnlösung beschleunigt wird. Die Beschleunigung des Koagulationsbades erfolgt über einen nach unten konisch sich verjüngenden Spinntrichter. Ein solcher Spinntrichter hat den Nachteil, daß das Anspinnen der Spinnlösung große Probleme bereitet. Die erreichbare Wickelgeschwindigkeit liegt gemäß der Beispiele bei maximal 150 m/min, sodaß dieses bekannte Verfahren nicht besonders wirtschaftlich ist.Such a method is for example from DE-A-4409609 known. The spinning solution is made after passing through the gas section immersed in a standing coagulation bath, which then accelerated together with the spinning solution. The acceleration of the coagulation bath takes place via a Bottom tapered spinning funnel. Such a Spinning funnel has the disadvantage that the piecing of the Spinning solution causes big problems. The achievable winding speed is maximum according to the examples 150 m / min, so that this known method is not particularly is economical.
Ein weiteres derartiges Verfahren ist aus JP-A-61-19805 bekannt, bei dem wiederum die Spinnlösung in einen Spinntrichter extrudiert wird, wobei aufgrund der Abkapselung der Gasstrecke die Gasathmosphäre, in die die Spinnlösung extrudiert wird, stark mit der Koagulationsflüssigkeit angereichert ist, wodurch in der Gasstrecke eine Vorkoagulation eintritt, was nicht immer wünschenswert ist. Bei diesem bekannten Verfahren soll die Koagulationsflüssigkeit über die Wand des Spinntrichters in einer Schicht geführt werden, wodurch sich gerade am Auftreffpunkt der Spinnlösung auf die Koagulationsflüssigkeit eine Turbulenz ergibt. Diese Turbulenz hat häufige Spinnbrüche zur Folge, sodaß dieses Verfahren nur bei sehr wenig cellulosischen Spinnlösungen zu einem stabilen Spinnprozeß führt. In den Beispielen werden zwar Wickelgeschwindigkeiten von bis zu 1500 m/min genannt. Dies wird aber durch aufwendige Anordnung mehrerer Beschleunigungstrichter erreicht, wodurch zum einen das Anspinnen und zum anderen ein stabiler Spinnprozeß erheblich erschwert wird.Another such method is known from JP-A-61-19805, in which in turn the spinning solution in a spinning funnel is extruded, due to the encapsulation of the gas route the gas atmosphere into which the spinning solution extrudes is heavily enriched with the coagulation liquid, whereby precoagulation occurs in the gas route, which is not always desirable. In this known method should the coagulation liquid over the wall of the spinning funnel be performed in one shift, which makes it straight at the point of impact of the spinning solution on the coagulation liquid results in turbulence. This turbulence has been common Spin breaks result, so that this method only very little cellulosic spinning solutions to a stable Spinning process leads. In the examples there are winding speeds of up to 1500 m / min. But this will due to the complex arrangement of several acceleration funnels achieved, which on the one hand the piecing and on the other one stable spinning process is made considerably more difficult.
Aufgabe der vorliegenden Erfindung ist es, ein weiteres Spinnverfahren zur Herstellung cellulosischer Fasern zur Verfügung zu stellen, welches wirtschaftlicher arbeitet. Insbesondere soll es die oben beschriebenen Nachteile zumindest mindern. Es soll auch ein Verfahren zur Herstellung cellulosischer Fasern zur Verfügung gestellt werden, welches auch bei Wickelgeschwindigkeiten oberhalb 1000 m/min auch bei empfindlichen cellulosischen Spinnlösungen, wie es beispielsweise bei Lösungen von Cellulose in einem Wasser enthaltenden N-Oxid eines tertiären Amins, insbesondere N-Methylmorpholin -N-oxid (NMMO), der Fall ist, einen stabilen Prozeß liefert.The object of the present invention is another Spinning process for the production of cellulosic fibers for To make available which works more economically. In particular, it should at least address the disadvantages described above reduce. It is also said to be a manufacturing process cellulosic fibers are provided, which also at winding speeds above 1000 m / min sensitive cellulosic spinning solutions, such as it for solutions of cellulose in a water containing N-oxide of a tertiary amine, especially N-methylmorpholine -N-oxide (NMMO), the case is a stable Process supplies.
Diese Aufgabe wird bei dem eingangs genannten Verfahren dadurch gelöst, daß die extrudierte Spinnlösung nach der Gasstrecke in ein auf vorbestimmte Geschwindigkeit beschleunigte, zumindest in etwa in Richtung der extrudierten Spinnlösung laminar fließendes Koagulationsbad eingeführt wird, wobei die Koagulationsflüssigkeit seitlich in den Pfad der Spinnlösung zugeführt wird und die Flußrichtung der Spinnlösung und der Koagulationsflüssigkeit über die gesamte Koagulationsstrecke zumindest in etwa parallel gehalten wird, und daß die erhaltenen Cellulosefasern beim Verlassen der Koagulationsstrecke seitlich umgelenkt und danach aufgewikkelt werden.This task is achieved in the method mentioned at the outset solved that the extruded spinning solution after the gas line accelerated to a predetermined speed, at least approximately in the direction of the extruded spinning solution laminar flowing coagulation bath is introduced, with the coagulation liquid laterally in the path of the Spinning solution is supplied and the direction of flow of the spinning solution and the coagulation liquid over the entire coagulation distance is kept at least approximately in parallel, and that the cellulose fibers obtained on leaving the The coagulation path is laterally deflected and then wound up become.
Die seitliche laminare Zuführung der Koagulationsflüssigkeit kann auf einfache Weise dadurch erreicht werden, daß die eine Seite eines Vorratsbehälters für die Koagulationsflüssigkeit als Überlauf ausgebildet ist, wobei der Überlauf derart ausgeformt ist, daß die Koagulationsflüssigkeit einerseits entlang der Ausformung fließt und andererseits die Koagulationsflüssigkeit von der Waagrechten in die Flußrichtung der Spinnlösung umlenkt. Diese Ausformung kann im einfachen Fall die Form eines Viertelkreises oder einer Parabel aufweisen, wobei jedoch darauf geachtet werden muß, daß vom Auslauf bis zum Übergang zur Flußrichtung der Spinnlösung eine stete Kurve gebildet ist, um zu gewährleisten, daß Turbulenzen weitgehend vermieden werden, sodaß die Spinnlösung in einen laminaren Koagulationsflüssigkeits-Strom eintauchen kann. Günstig ist es, wenn der Überlauf nach der Übergangsstelle in die Flußrichtung der Spinnlösung noch bis zum Ende der Koagulationsstrecke parallel zur Flußrichtung der Spinnlösung weitergeführt wird, wobei dann die Unterkante des Überlaufes dazu benutzt werden kann, den entstandenen cellulosischen Faden umzulenken, indem von einer seitlich versetzten Aufwickelvorrichtung der entstandene Faden über die untere Kante des Überlaufes gezogen wird.The lateral laminar supply of the coagulation liquid can be achieved in a simple manner in that the one Side of a storage container for the coagulation liquid is designed as an overflow, the overflow being such is formed that the coagulation liquid on the one hand flows along the formation and on the other hand the Coagulation liquid from the horizontal in the flow direction redirects the spinning solution. This shape can be done in simple Fall in the form of a quarter circle or parabola have, but it must be ensured that from Run out until the transition to the direction of flow of the spinning solution a constant curve is formed to ensure that turbulence largely avoided, so that the spinning solution Immerse in a laminar coagulation fluid stream can. It is favorable if the overflow after the transition point in the direction of flow of the spinning solution until the end the coagulation path parallel to the direction of flow of the spinning solution is continued, then the lower edge of the Overflow can be used to the resulting redirect cellulosic thread by a sideways offset take-up of the resulting thread over the lower edge of the overflow is drawn.
Das erfindungsgemäße Verfahren eignet sich zur Herstellung von Fasern, wobei unter dem Begriff Fasern Monofilamente, Multifilamentfäden, aber auch Hohlfäden verstanden werden. Das Verfahren ist gleichermaßen auch zur Herstellung von porösen Fasern geeignet. Die Fasern können runden Querschnitt, aber auch profilierten Querschnitt aufweisen.The method according to the invention is suitable for production of fibers, the term fibers being monofilaments, Multifilament threads, but also hollow threads can be understood. The process is also equally suitable for the production of porous ones Fibers suitable. The fibers can have a round cross-section, but also have a profiled cross section.
Die erfindungsgemäße Herstellung cellulosischer Fasern gelingt vorzüglich, wenn die Koagulationsflüssigkeit einseitig der Spinnlösung in einer konstanten Schichtdicke im Bereich von 1,0 bis 5 mm zugeführt wird. Hierbei ist es von besonderem Vorteil, wenn die Schichtdicke etwa 1 bis 3 mal so dick eingestellt wird wie der größte Durchmesser der extrudierten Spinnlösung. Bei dem oben näher beschriebenen Überlauf, kann die Schichtdicke besonders einfach dadurch gewährleistet werden, wenn man dem Vorratsbehälter für die Koagulationsflüssigkeit eine solche Menge an Koagulationsflüssigkeit zuführt, daß sich am tangentialen Auslauf auf dem Überlauf die gewünschte Schichtdicke einstellt. Natürlich muß hierbei dafür gesorgt werden, daß die Koagulationsflüssigkeit dem Vorratsbehälter zumindest beruhigt, ohne Turbulenzen im Vorratsbehälter zu verursachen, zugeführt wird. Die Mittel, die hierzu erforderlich sind, sind dem Fachmann hinreichend bekannt und brauchen insofern nicht näher erläutert werden. The production of cellulosic fibers according to the invention succeeds excellent if the coagulation fluid is one-sided of the spinning solution in a constant layer thickness in the range from 1.0 to 5 mm is supplied. Here it is special Advantage if the layer thickness is about 1 to 3 times as thick is set as the largest diameter of the extruded Spinning solution. With the overflow described in more detail above, can this ensures the layer thickness is particularly simple if you have the reservoir for the coagulation liquid supplies such an amount of coagulation fluid, that at the tangential outlet on the overflow sets the desired layer thickness. Of course you have to do this be made sure that the coagulation liquid is the reservoir at least calm, without turbulence in the storage container to cause is fed. The means that are necessary for this, are well known to the person skilled in the art and therefore do not need to be explained in more detail.
Bei dem erfindungsgemäßen Verfahren ist es empfehlenswert, wenn die Geschwindigkeit der Koagulationsflüssigkeit am Eintauchpunkt der Spinnlösung auf einen Wert zwischen 30 bis 200 m/min, vorzugsweise zwischen 50 und 80 m/min, eingestellt wird, wobei die Herstellung der cellulosischen Fasern dann besonders gut gelingt, wenn die Koagulationsstrecke auf eine Länge von 0,5 bis 8 cm, bevorzugt auf eine Länge von 1 bis 4 cm, eingestellt wird.In the method according to the invention, it is recommended that when the speed of the coagulation liquid at the immersion point of the spinning solution to a value between 30 and 200 m / min, preferably between 50 and 80 m / min is, the production of the cellulosic fibers then works particularly well when the coagulation path is on a Length of 0.5 to 8 cm, preferably to a length of 1 to 4 cm.
Die Geschwindigkeit am Eintauchpunkt läßt sich bei dem oben näher beschriebenen Verfahren durch den Höhenunterschied zwischen dem Flüssigkeitsspiegel im Vorratsbehälter und dem Eintauchpunkt der Spinnlösung, dem Punkt, an dem der Überlauf in die Flußrichtung der Spinnlösung übergeht, bestimmen. Die am Eintauchpunkt herrschende Geschwindigkeit bestimmt sich dann aus der Wurzel aus dem Produkt aus zwei mal Erdbeschleunigung mal Höhenunterschied (die mit sich selbst multiplizierte Geschwindigkeit entspricht also dem Produkt aus zwei mal Erdbeschleunigung multipliziert mit dem Höhenunterschied). Wird ein solcher Überlauf verwendet, wird die Koagulationsstrecke in einfacher Weise über die Strecke des Überlaufs bestimmt, die sich zwischen dem Eintauchpunkt und der Unterkante des Überlaufs ergibt.The speed at the immersion point can be seen at the above procedure described in more detail by the height difference between the liquid level in the reservoir and the Immersion point of the spinning solution, the point at which the overflow in the flow direction of the spinning solution, determine. The The speed prevailing at the immersion point is determined then from the root of the product of two times gravitational acceleration times height difference (which multiplied by itself So speed corresponds to the product twice the acceleration of gravity multiplied by the difference in altitude). If such an overflow is used, the coagulation path becomes in a simple way over the route of the Overflow determined between the immersion point and the lower edge of the overflow.
Um die Koagulationsflüssigkeit am Ausgang der Koagulationsstrecke besonders gut von dem entstandenen cellulosischen Faden zu entfernen, hat es sich besonders bewährt, wenn die koagulierten Cellulosefasern in einem Wickel zwischen 45 und 60° zur Flußrichtung der Koagulationsflüssigkeit nach der Koagulationsstrecke umgelenkt werden. Es empfiehlt sich hierbei, die erhaltenen Cellulosefasern plötzlich aus der Flußrichtung der Koagulationsflüssigkeit nach der Koagulationsstrecke umzulenken. Plötzlich im Sinne der vorliegenden Erfindung bedeutet, daß der Weg der erhaltenen Fasern in einem sehr kurzen Bereich, der lediglich wenige Millimeter umfaßt, ihre Bewegungsrichtung ändern. Hierzu ist es von Vorteil, wenn die erhaltenen Cellulosefasern nach der Koagulationsstrecke derart plötzlich aus der Flußrichtung der Koagulationsflüssigkeit umgelenkt werden, daß sie im Umlenkbereich einen Radius von 0,2 bis 2 mm, bevorzugt einen Radius zwischen 0,3 und 1 mm, bilden. Dies kann bei dem oben erwähnten Überlauf dadurch erreicht werden, daß die Unterkante des Überlaufes mit einem entsprechenden Radius versehen wird.To the coagulation liquid at the exit of the coagulation section particularly good from the resulting cellulosic To remove thread, it has proven particularly useful if the coagulated cellulose fibers in a roll between 45 and 60 ° to the flow direction of the coagulation liquid after the Coagulation route can be diverted. It is advisable here, the cellulose fibers obtained suddenly from the Direction of flow of the coagulation liquid after the coagulation distance redirect. Suddenly in the sense of the present Invention means that the path of the fibers obtained in one very short area, only a few millimeters, change their direction of movement. For this it is an advantage if the cellulose fibers obtained after the coagulation route so suddenly from the direction of flow of the coagulation liquid are deflected that they are in the deflection area a radius of 0.2 to 2 mm, preferably a radius between 0.3 and 1 mm. This can be done with the above Overflow can be achieved in that the lower edge the overflow is provided with a corresponding radius.
Für eine Lösung von Cellulose in einem Wasser enthaltenden N-Oxid eines tertiären Amins, insbesondere von N-Methylmorpholin -N-oxid (NMMO), als Spinnlösung hat sich das erfindungsgemäße Verfahren als besonders vorteilhaft herausgestellt.For a solution of cellulose in a water containing N-oxide of a tertiary amine, especially of N-methylmorpholine -N-oxide (NMMO), as a spinning solution The method according to the invention was found to be particularly advantageous.
Die Erfindung wird anhand einer Figur und anhand der nachfolgenden Beispielen näher erläutert.The invention is based on a figure and the following Examples explained in more detail.
In der schematischen Figur ist mit 1 eine Spinndüse dargestellt,
aus welcher eine Spinnlösung 2 in ein Gas, beispielsweise
Umgebungsluft gesponnen wird, welche dann in eine
nach unten strömende Koagulationsflüssigkeit eintaucht und in
dieser bis zum Ablenkpunkt 4 verbleibt, wonach der inzwischen
koagulierte Faden 5 in Richtung der Aufwicklung 6 plötzlich
umgelenkt wird und danach über die Aufwickelvorrichtung 6,
beispielsweise auf eine nicht extra dargestellte, sich auf
der Aufwicklung befindliche Spule, aufgewickelt wird. Bei der
plötzliche Umlenkung an der Umlenkstelle 4 fließt der weitaus
überwiegende Teil der Koagulationsflüssigkeit nach unten
weiter (siehe Strom 10 mit Pfeil), sodaß vom Faden 5 zumindest
überwiegend die Koagulationsflüssigkeit entfernt ist. Es
hat sich hierbei herausgestellt, daß es günstig ist, wenn der
Faden unter einem Winkel, der sich zwischen dem Strom 10 und
dem Faden 5 ergibt, von 45 und 60 ° abgezogen wird.In the schematic figure, 1 represents a spinneret,
from which a
Für die Koagulationsflüssigkeit 7 ist ein Vorratsbehälter 8
vorgesehen, in den über nicht gezeigte Mittel eine konstante
Menge an Koagulationsflüssigkeit möglichst turbulenzfrei zugeführt
wird. Zur Erreichung des möglichst laminaren Stromes
der Koagulationsflüssigkeit 7/3 am Eintauchpunkt ist der
Vorratsbehälter 8 der Koagulationsflüssigkeit 7 zur Flußrichtung
der Spinnlösung 2 hin über einen Überlauf 9 begrenzt,
wobei durch die ständige und konstante Zugabe von
Koagulationsflüssigkeit 7 in den Vorratsbehälter 8 sich eine
bestimmte Dicke des zur Spinnlösung 2 fließenden, zumindest
überwiegend laminaren Koagulationsflüssigkeits-Stromes einstellt.
Die Bestimmung der Geschwindigkeit, die die Koagulationsflüssigkeit
am Eintauchpunkt der Spinnlösung 2 aufweist,
ergibt sich über den Höhenunterschied h zwischen Flüssigkeitsspiegel
der Koagulationsflüssigkeit 7 im Vorratsbehälter
8 und dem Übergang der Kurve des Überlaufs 9 in die senkrechte
Anordnung. Wie schon erwähnt errechnet sich die Geschwindigkeit
der Koagulationsflüssigkeit am Eintauchpunkt
über die Wurzel aus dem Produkt aus zwei mal Erdbeschleunigung
mal Höhenunterschied h.A
Nachfolgend wird die Erfindung anhand von Vergleichsbeispielen und erfindungsgemäßen Beispielen näher erläutert.The invention is described below on the basis of comparative examples and examples according to the invention explained in more detail.
Die eingesetzte Spinnlösung enthält in allen Beispielen 15%
Cellulose, 10% Wasser und 75% NMMMO, welche aus Zellstoff
V65, zu beziehen von Buckeye auf die für die Herstellung von
NMMO-Spinnlösungen bekannte Weise hergestellt wurde. Die auf
einer Temperatur von 120 °C gehaltene Spinnlösung wurde in
Luft gesponnen. Der Düsenlochdurchmesser der verwendeten
Spinndüse betrug 200 µm, wobei der in der Tabelle angegebene
Massenstrom m durch die Spinndüse extrudiert wurde. Die
Spinnlösung tauchte nach einer Gasstrecke von 18 cm in ein
Koagulationsbad ein und wurde am Ende des Bades unter einem
Winkel von 60 ° zur eigentlichen Fließrichtung der Spinnlösung
in Richtung einer Aufwickelvorrichtung abgezogen und
dort bei einer Geschwindigkeit vsp des Fadens aufgewickelt,
die so ausgewählt wurde, daß der Faden ohne zu brechen, aufgewickelt
werden konnte. Es handelt sich also bei Vsp jeweils
um die maximal mögliche Aufwickelgeschwindigkeit, bei der bei
der Herstellung der Fäden noch kein Bruch auftrat. Bei den
Beispielen 1 bis 3 (Vergleichsbeispiele) wurde ein stehendes
Fällbad eingesetzt (Geschwindigkeit der Fällbadflüssigkeit am
Eintauchpunkt entspricht uE = 0 m/min), während bei den Beispielen
4 bis 6 die in der Figur beschriebene Vorrichtung zum
Einsatz kam, wobei die Geschwindigkeit uE am Eintauchpunkt
der Spinnlösung in die Koagulationsflüssigkeit herrschte. Die
weiteren Prozeßdaten und Ergebnisse sind in der nachfolgenden
Tabelle zusammengefaßt.
Aus den Beispielen geht hervor, daß bei Anwendung des Erfindungsgemäßen Verfahrens mit deutlich höherer Aufwickelgeschwindigkeit gearbeitet werden kann als bei Verwendung eines herkömmlichen stehenden Fällbades.The examples show that when using the invention Process with significantly higher winding speed can be worked as when using a conventional standing baths.
Claims (12)
- A process for manufacturing cellulose fibers by extrusion of a spinning solution, containing dissolved cellulose, into a gaseous medium through a predetermined gas zone, with subsequent immersion in and guidance through a coagulation bath over a predetermined coagulation zone, drawing the cellulose fibers obtained and winding them up, characterized in that after the gas zone the extruded spinning solution is immersed in a coagulation bath accelerated to a predetermined velocity and flowing laminarly at least approximately in the direction of the extruded spinning solution, whereby the coagulation liquid is fed laterally into the path of the spinning solution and the flow direction of the spinning solution and the coagulation liquid is kept at least approximately parallel throughout the entire coagulation zone, and in that the cellulose fibers obtained are laterally deflected upon leaving the coagulation zone and then wound up.
- Process according to Claim 1, characterized in that the coagulation liquid is fed into the spinning solution from one side with a constant stream depth ranging from 1.0 to 5 mm.
- Process according to Claim 2, characterized in that the stream depth is adjusted to approximately 1 to 3 times the largest diameter of the extruded spinning solution.
- Process according to one or more of Claims 1 to 3, characterized in that the velocity of the coagulation liquid at the immersion point of the spinning solution is adjusted to a value between 30 and 200 m/min
- Process according to Claim 4, characterized in that the velocity of the coagulation liquid is adjusted to a value between 50 and 80 m/min
- Process according to one or more of Claims 1 to 5, characterized in that the coagulation zone is adjusted to a length of 0.5 to 8 cm.
- Process according to Claim 6, characterized in that the coagulation zone is adjusted to length of 1 to 4 cm.
- Process according to one or more of Claims 1 to 7, characterized in that the coagulated cellulose fibers are deflected after the coagulation zone at an angle between 45° and 60° to the flow direction of the coagulation liquid.
- Process according to one or more of Claims 1 to 8, characterized in that after the coagulation zone the cellulose fibers obtained are abruptly deflected from the flow direction of the coagulation liquid.
- Process according to one or more of Claims 1 to 9, characterized in that after the coagulation zone the cellulose fibers obtained are abruptly deflected from the flow direction of the coagulation liquid in such a way that they form a radius of 0.2 to 2 mm in the deflection area.
- Process according to Claim 10 characterized in that a radius between 0.3 and 1 mm is adjusted.
- Process according to one or more of Claims 1 to 11, characterized in that a solution of cellulose in a water-containing N-oxide of a tertiary amine, particularly N-methylmorpholine-N-oxide (NMMO), is used as a spinning solution.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19512053 | 1995-03-31 | ||
| DE19512053A DE19512053C1 (en) | 1995-03-31 | 1995-03-31 | Process for the production of cellulosic fibers |
| PCT/EP1996/001173 WO1996030566A1 (en) | 1995-03-31 | 1996-03-19 | Method of producing cellulose fibres |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0817873A1 EP0817873A1 (en) | 1998-01-14 |
| EP0817873B1 true EP0817873B1 (en) | 1999-05-06 |
Family
ID=7758404
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP96908070A Revoked EP0817873B1 (en) | 1995-03-31 | 1996-03-19 | Method of producing cellulose fibres |
Country Status (12)
| Country | Link |
|---|---|
| US (1) | US5868985A (en) |
| EP (1) | EP0817873B1 (en) |
| JP (1) | JPH11502573A (en) |
| KR (1) | KR19980703390A (en) |
| AT (1) | ATE179768T1 (en) |
| AU (1) | AU692086B2 (en) |
| CA (1) | CA2216644A1 (en) |
| DE (2) | DE19512053C1 (en) |
| PL (1) | PL322498A1 (en) |
| SK (1) | SK129497A3 (en) |
| TW (1) | TW293042B (en) |
| WO (1) | WO1996030566A1 (en) |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19744371C2 (en) * | 1997-10-08 | 2002-11-14 | Ostthueringische Materialpruef | Method and device for producing cellulose filament yarns |
| KR100306059B1 (en) * | 1999-08-14 | 2001-09-24 | 박호군 | A method and equipment to induct fibre filaments |
| DE19954152C2 (en) * | 1999-11-10 | 2001-08-09 | Thueringisches Inst Textil | Method and device for producing cellulose fibers and cellulose filament yarns |
| WO2003014432A1 (en) * | 2001-08-11 | 2003-02-20 | Tencel Limited | Precipitating bath |
| DE10200406A1 (en) * | 2002-01-08 | 2003-07-24 | Zimmer Ag | Spinning device and process with turbulent cooling blowing |
| DE10204381A1 (en) * | 2002-01-28 | 2003-08-07 | Zimmer Ag | Ergonomic spinning system |
| DE10206089A1 (en) | 2002-02-13 | 2002-08-14 | Zimmer Ag | bursting |
| DE10213007A1 (en) * | 2002-03-22 | 2003-10-09 | Zimmer Ag | Method and device for controlling the indoor climate in a spinning process |
| DE10223268B4 (en) * | 2002-05-24 | 2006-06-01 | Zimmer Ag | Wetting device and spinning system with wetting device |
| DE10314878A1 (en) * | 2003-04-01 | 2004-10-28 | Zimmer Ag | Method and device for producing post-stretched cellulose filaments |
| DE102004024028B4 (en) * | 2004-05-13 | 2010-04-08 | Lenzing Ag | Lyocell method and apparatus with press water return |
| DE102004024030A1 (en) * | 2004-05-13 | 2005-12-08 | Zimmer Ag | Lyocell process with polymerization-degree-dependent adjustment of the processing time |
| DE102004024029A1 (en) * | 2004-05-13 | 2005-12-08 | Zimmer Ag | Lyocell method and apparatus with metal ion content control |
| WO2008036051A1 (en) * | 2006-09-18 | 2008-03-27 | National University Of Singapore | Fiber structures and process for their preparation |
| CA2759693C (en) * | 2009-04-24 | 2015-10-20 | Mitsubishi Rayon Co., Ltd. | Porous composite membrane manufacturing method using flowing coagulating solution |
| US11034817B2 (en) | 2013-04-17 | 2021-06-15 | Evrnu, Spc | Methods and systems for processing mixed textile feedstock, isolating constituent molecules, and regenerating cellulosic and polyester fibers |
| KR101472094B1 (en) * | 2013-12-18 | 2014-12-15 | 주식회사 효성 | Manufacturing method of cellulose fiber controlled degree of crystllity according to solidification rate and cellulose fiber produced by using the same |
| EP3505659A1 (en) * | 2018-08-30 | 2019-07-03 | Aurotec GmbH | Method and device for filament spinning with inflection |
| EP3674455A1 (en) * | 2018-12-28 | 2020-07-01 | Lenzing Aktiengesellschaft | Process for liquid removal from cellulose filaments yarns or fibers |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59228012A (en) * | 1983-06-10 | 1984-12-21 | Asahi Chem Ind Co Ltd | Wet spinning process |
| JPS6119805A (en) * | 1984-07-03 | 1986-01-28 | Asahi Chem Ind Co Ltd | Method of high-speed wet spinning and its device |
| US4869860A (en) * | 1984-08-09 | 1989-09-26 | E. I. Du Pont De Nemours And Company | Spinning process for aromatic polyamide filaments |
| US5417909A (en) * | 1992-06-16 | 1995-05-23 | Thuringisches Institut Fur Textil- Und Kunststoff-Forschung E.V. | Process for manufacturing molded articles of cellulose |
| DE4308524C1 (en) * | 1992-06-16 | 1994-09-22 | Thueringisches Inst Textil | Process for the production of cellulose fibers and filaments by the dry-wet extrusion process |
| DE4409609A1 (en) * | 1994-03-21 | 1994-10-13 | Thueringisches Inst Textil | Process for spinning cellulose fibres and filament yarns |
-
1995
- 1995-03-31 DE DE19512053A patent/DE19512053C1/en not_active Expired - Fee Related
-
1996
- 1996-03-19 KR KR1019970706795A patent/KR19980703390A/en not_active Application Discontinuation
- 1996-03-19 WO PCT/EP1996/001173 patent/WO1996030566A1/en not_active Application Discontinuation
- 1996-03-19 PL PL96322498A patent/PL322498A1/en unknown
- 1996-03-19 EP EP96908070A patent/EP0817873B1/en not_active Revoked
- 1996-03-19 JP JP8528875A patent/JPH11502573A/en active Pending
- 1996-03-19 AT AT96908070T patent/ATE179768T1/en not_active IP Right Cessation
- 1996-03-19 DE DE59601832T patent/DE59601832D1/en not_active Expired - Fee Related
- 1996-03-19 CA CA002216644A patent/CA2216644A1/en not_active Abandoned
- 1996-03-19 SK SK1294-97A patent/SK129497A3/en unknown
- 1996-03-19 AU AU51459/96A patent/AU692086B2/en not_active Ceased
- 1996-03-19 US US08/913,169 patent/US5868985A/en not_active Expired - Fee Related
- 1996-03-21 TW TW085103411A patent/TW293042B/zh active
Also Published As
| Publication number | Publication date |
|---|---|
| AU5145996A (en) | 1996-10-16 |
| DE59601832D1 (en) | 1999-06-10 |
| JPH11502573A (en) | 1999-03-02 |
| AU692086B2 (en) | 1998-05-28 |
| DE19512053C1 (en) | 1996-10-24 |
| EP0817873A1 (en) | 1998-01-14 |
| US5868985A (en) | 1999-02-09 |
| KR19980703390A (en) | 1998-10-15 |
| SK129497A3 (en) | 1998-03-04 |
| PL322498A1 (en) | 1998-02-02 |
| ATE179768T1 (en) | 1999-05-15 |
| CA2216644A1 (en) | 1996-10-03 |
| WO1996030566A1 (en) | 1996-10-03 |
| TW293042B (en) | 1996-12-11 |
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