EP0879906A2 - Process and device for spinning solutions of cellulose carbamate - Google Patents
Process and device for spinning solutions of cellulose carbamate Download PDFInfo
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- EP0879906A2 EP0879906A2 EP98108315A EP98108315A EP0879906A2 EP 0879906 A2 EP0879906 A2 EP 0879906A2 EP 98108315 A EP98108315 A EP 98108315A EP 98108315 A EP98108315 A EP 98108315A EP 0879906 A2 EP0879906 A2 EP 0879906A2
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- Prior art keywords
- precipitation
- spinning
- spinneret
- fibers
- bath
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- 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
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
-
- 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
Definitions
- the invention relates to a method and an apparatus for Spinning cellulose carbamate solutions by extruding the solution through a spinneret into a precipitation bath, coagulating the formed Cellulose carbamate fibers by contact with the precipitation medium and peeling off the fibers after exiting the precipitation bath by mechanical means.
- DE-A 39 04 541 therefore proposes to circulate the precipitation medium through the spinning tube, preferably from below upwards with vertical arrangement, the flow rate of the precipitation medium at the spinning tube outlet is set lower than that Pull-off speed of the fibers, according to a speed ratio from 0.15 to 0.95. This favors the exchange of the Precipitation medium within the spinning tube, but causes one of the threads Pulling direction opposite force, which is the morphology of the thread influenced.
- the object of the present invention is a method and a device for spinning cellulose carbamate solutions create which fibers of high uniformity and good quality allow to manufacture. Also an adjustment to different Spinning speeds must be easy to achieve.
- this object is achieved by a method and a device according to the claims.
- the process is characterized in that the fibers emerge from the outlet the spinneret until it comes out of the coagulation bath rectified flow of the precipitation medium with a given cross section are enveloped, the flow rate of the precipitation medium on The fibers exit the spinneret (plane X1) equal to 0.1 to 0.8 times and the same at the exit of the fibers from the precipitation bath (level X3) is 0.96 to 1.1 times the withdrawal speed of the fibers.
- the Device for carrying out the method is characterized in that they essentially from a precipitation bath tank (15) with a feed line (12) for the precipitation medium and within the container one as Flow body trained, frustoconical spinneret (3) and a frustoconical (5) spinning funnel followed by cylindrical tube (6) protruding from the wall of the precipitation bath tank as well as outside the container of a mechanical fiber draw-off device (9), the spinneret (3) forming a immerses concentric gap in the spinning funnel (5).
- the filaments are very unstable immediately after entering the precipitation bath. At extremely low thread take-off speeds, the threads could be coagulated in a standing precipitation bath. However, with increasing thread take-off speed and thus increasing friction between the thread and the precipitation bath, turbulence increasingly occurs on the nozzle surface and along the filaments, which lead to a deterioration in the thread quality.
- a directed flow U B is impressed on the filament compartments (4). It must be avoided that the impressed flow on the lower edge of the spinneret (3) in the plane X1 detaches and forms a turbulent flow.
- the flow rate (U B ) of the precipitation medium is 0.1 to 0.8 times the withdrawal rate (U AB ) of the fibers at the exit of the fibers from the spinneret (plane X1) and 0.96 to 1.1 times the exit of the fibers the precipitation bath (level X3).
- the flow rate of the precipitation medium at the exit of the fibers from the precipitation bath (level X3) is in any case based on the cross section of the cylindrical spinning tube part with diameter T2. Any conical end piece that adjoins the pipe part in plane X3 in the direction of flow and / or an orifice plate with a variable opening are not taken into account here (flow rate of the precipitation medium here is higher than in plane X3 in accordance with the narrowed cross section).
- the flow rate of the precipitation medium in the plane X3 can also be adjusted by varying the delivery pressure of the pump (11) for the precipitation medium in a closed spinning bath container completely filled with precipitation medium.
- the flow rate of the precipitation medium in the entire tube area from the level X2 to the level X3 is approximately equal to the fiber withdrawal rate (U AB) .
- the flow velocity in plane X1 is corresponding to the larger cross section of the spinning funnel (5) at this point than that in plane X3.
- An adjustment is possible by changing the immersion depth (lt) of the spinneret (3) in the spinning funnel (5) and thus the cross-section of the precipitation medium flow in the plane (X1).
- the cellulose carbamate spinning solution preferably consisting of 5 to 12% by weight of cellulose carbamate in 5 to 10% aqueous sodium hydroxide solution, is at a temperature of about 0 to +30 ° C by the spinning pump (1) via line (2 ) fed to the spinneret (3).
- the threads (4) emerging at the spinneret (3) are flowed diagonally (U B ) at a small angle by the precipitation medium flowing through the spinning funnel (5) from top to bottom and taken along.
- the spinning funnel consists of a frustoconical part (5) and in the plane (X2) adjoining it a cylindrical, tubular part (6) which, as shown here, ends in plane X3.
- the tube can also end with a conical end piece and / or a diaphragm attached to it in plane X3.
- the filaments (4) are drawn off by a mechanical take-off device (9), for example a driven pair of godets, at the speed (U AB ) while the accompanying stream of the precipitation medium flows into the storage container (10).
- the cellulose carbamate fibers are then washed, drawn and saponified to regenerate cellulose fibers at a higher temperature.
- the precipitation medium passes from the storage container (10) by means of a pump (11) via the line (12) into the precipitation bath container (15), which for the purpose of a uniform, turbulence-free inflow of the precipitation medium with an inner wall (13) designed as an overflow, preferably arranged concentrically or parallel to the container wall ) is equipped.
- the precipitation medium flows into the spinning funnel (5) via the wall (13).
- Both aqueous solutions of acids and of alkalis and / or salts can be used as the precipitation medium. Alcohols are also suitable.
- An aqueous solution with 5 to 25% by weight H 2 SO 4 and 5 to 25% by weight Na 2 SO 4 at a temperature of about 20 to 60 ° C. is preferred.
- the precipitation medium is enriched with the salts which form, for example sodium sulfate, as it flows through the spinning funnel (5 and 6).
- These salts can remain in the precipitation medium up to a certain concentration depending on the composition of the precipitation medium. Since the lower end of the spinning funnel (6) is outside the precipitation bath container (15), the composition of the precipitation medium flowing out of the spinning tube part (6) can be easily corrected before it is pumped back into the container (15) via the line (12) , for example by partial discharge via line (18) and fresh supply via line (17).
- the fiber take-off speed (U AB ) depends on the equipment used and in particular the titer of the fibers to be spun. In general, take-off speeds of 30 to 500 m / min, preferably 50 to 350 m / min are well suited.
- the corresponding, preferably approximately the same flow rate of the precipitation medium in the plane (X3) is adjusted by vertically shifting the spinning funnel (5 and 6) in relation to the position of the precipitation bath container (15) and consequently by changing the hydrostatic height (H) of the precipitation medium .
- the flow velocity of the precipitation medium on the plane (X1) is adjusted at the same time by changing the immersion depth (lt) of the spinneret (3) in the spinning funnel (5).
- An additional adjustment can optionally be made by vertically shifting the precipitation bath container (15) with unchanged hydrostatic height (H) and / or by vertically shifting the spinneret (3). Vertical displacement of the precipitation bath container (15) with respect to the position of the spinning funnel and / or changing the length of the tubular part (6) of the spinning funnel are also possible.
- FIG. 2 schematically shows another embodiment of the device according to the invention, preferably used for low fiber draw-off speeds (U AB ).
- the individual elements of the device correspond to those in FIG. 1, but the spinneret and spinning funnel are arranged horizontally.
- the cellulose carbamate spinning solution is fed via line (2) to the spinneret (3) and the spun threads are drawn off from the take-off device (9) through the spinning funnel (5 and 6).
- Spinning nozzle (3) and the frustoconical part (5) of the spinning funnel are arranged in the precipitation medium inside the precipitation bath container (15), while the tubular part (6) of the spinning funnel is passed through the wall of the container to the outside.
- the precipitation medium is fed from the storage container (10) to the precipitation bath container (15) by means of the pump (11) via the line (12).
- the feed line (12) and the spinneret area are separated from one another by a permeable wall (14).
- the liquid level or the hydrostatic height (H) in the precipitation bath tank (15) is set via a drain pipe (16) attached to the tank bottom and / or various overflow pipes.
- the precipitating medium flows through the spinning funnel (5) due to the hydrostatic pressure in the spinning direction and exits at the end of the spinning tube (6) in the plane (X3), from where it, if necessary after setting the concentration, into the storage container (10) reached.
- the entire spinning funnel (5 and 6) is in relation to the position of the precipitation bath container (15) arranged horizontally. Alternatively or additionally, the spinneret (3) could also be moved horizontally.
- the dimensions of the device according to the invention depend on the intended throughput.
- the spinneret diameter (D) at 10 to 300 to 4000 mm preferably the spinning funnel diameter (T1) at 20 to 500 mm, the spinning tube diameter (T2) at 3 to 150 mm, the cone angle (a) at 5 to 30 °, including the total length of the spinning funnel Spinning tube (5 and 6) at 300 to 4000 mm, preferably up to 2000 mm and the hydrostatic height (H) at 10 to about 4000 mm, preferably up to about 2000 mm.
- construction material come glass as well corrosion-resistant plastics and metals.
- Spinning nozzle (3) and spinning funnel (5 and 6) can not only how described above, arranged vertically or horizontally, but also at an angle to the vertical or horizontal.
- the cellulose carbamate to be spun can be used in any way have been produced, for example by one of the methods of U.S. Patent 5,378,827, DE Patent Applications 4,417,140, 196 35,473 and 197 15 617.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren und eine Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen durch Extrudieren der Lösung durch eine Spinndüse in ein Fällbad, Koagulieren der gebildeten Cellulosecarbamat-Fasern durch Kontakt mit dem Fällmedium und Abziehen der Fasern nach Austritt aus dem Fällbad durch mechanische Mittel.The invention relates to a method and an apparatus for Spinning cellulose carbamate solutions by extruding the solution through a spinneret into a precipitation bath, coagulating the formed Cellulose carbamate fibers by contact with the precipitation medium and peeling off the fibers after exiting the precipitation bath by mechanical means.
Es ist bekannt wässrig-alkalische Lösungen von Cellulosecarbamat in saure, alkalische oder alkoholische Fällbäder in Anlehnung an die bei Viskose-Fasern angewandten Techniken zu verspinnen (EP-Patente 97 685 und 103 618; Britische Patente 2 164 941, 2 164 942 und 2 164 943; O. T. Turunen, Lenzinger Berichte [August 1985], Heft 59, Seiten 111 - 115). Nähere Angaben zur Spinnapparatur sind diesen Publikationen, die sich auf die Zusammensetzung der Fällbäder beziehen, aber nicht zu entnehmen.It is known in alkaline aqueous solutions of cellulose carbamate acidic, alkaline or alcoholic precipitation baths based on the Techniques used to spin viscose fibers (EP patents 97 685 and 103 618; British Patents 2,164,941, 2,164,942 and 2,164,943; O. T. Turunen, Lenzinger reports [August 1985], issue 59, pages 111 - 115). More detailed information on the spinning apparatus can be found in these publications, the refer to the composition of the precipitation baths, but not to remove.
Für das Erspinnen von Viskose-Fasern sind verschiedene Techniken
bekannt, unter anderem das Rohrspinnen, bei dem die Fasern nach
Austritt aus der Spinndüse durch ein horizontales, zylindrisches Rohr
innerhalb des Fällbades geführt werden (Z. A. Rogowin, Chemiefasern,
Thieme-Verlag [1982], Seite 133), und das Trichterspinnen, bei dem die
Fasern nach Austritt aus der Spinndüse zusammen mit dem Fällmedium
durch einen senkrechten, über die gesamte Länge konischen Trichter
geleitet werden (K. Götze, Chemiefasern nach dem Viskoseverfahren,
Springer-Verlag, 3. Auflage, Band 2, Seiten 602 - 607). Ähnlich
aufgebaute Spinntrichter sind auch für das Trocken-Naßverspinnen von
Celluloselösungen in wässrigem N-Methylmorpholin-N-oxid (NMMO)
beschrieben (DE-Patente 42 19 658 C und 195 15 136 A).There are various techniques for spinning viscose fibers
known, among other things, the tube spinning, in which the fibers after
Exit from the spinneret through a horizontal, cylindrical tube
within the precipitation bath (e.g. Rogowin, man-made fibers,
Thieme-Verlag [1982], page 133), and funnel spinning, in which the
Fibers after leaving the spinneret together with the precipitation medium
through a vertical funnel that is conical over its entire length
are managed (K. Götze, man-made fibers using the viscose process,
Springer-Verlag, 3rd edition,
Wesentlicher Nachteil des Rohrspinnverfahrens ist der mangelnde Austausch des Fällmediums innerhalb des Rohres und die dadurch bedingte Anreicherung des Lösungsmittels und eventueller Spaltprodukte aus der Spinnlösung im Rohr. In der DE-A 39 04 541 wird daher vorgeschlagen, das Fällmedium durch das Spinnrohr zu zirkulieren, bevorzugt von unten nach oben bei vertikaler Anordnung, wobei die Strömungsgeschwindigkeit des Fällmediums am Spinnrohraustritt niedriger eingestellt wird als die Abzugsgeschwindigkeit der Fasern, entsprechend einem Geschwindigkeitsverhältnis von 0,15 bis 0,95. Dies begünstigt zwar den Austausch des Fällmediums innerhalb des Spinnrohres, bewirkt aber am Faden eine der Abzugsrichtung entgegengesetzte Kraft, die die Morphologie des Fadens beeinflußt. Beim Spinntrichterverfahren ist hingegen die Strömungsgeschwindigkeit des Fällmediums innerhalb des Trichters so hoch, daß die Fäden infolge der Reibung Faser/Flüssigkeit eine deutliche Verstreckung erfahren. In beiden Fällen sind die frisch extrudierten Fäden unmittelbar nach Austritt aus der Spinndüse und vor Eintritt in das Spinnrohr oder den Spinntrichter an der Düsenoberfläche bevorzugt auftretenden Turbulenzen ausgesetzt, was zu einer Verschlechterung der Fadengleichmäßigkeit führt.The main disadvantage of the tube spinning process is the lack Exchange of the precipitation medium within the pipe and the resulting Enrichment of the solvent and any fission products from the Spinning solution in the tube. DE-A 39 04 541 therefore proposes to circulate the precipitation medium through the spinning tube, preferably from below upwards with vertical arrangement, the flow rate of the precipitation medium at the spinning tube outlet is set lower than that Pull-off speed of the fibers, according to a speed ratio from 0.15 to 0.95. This favors the exchange of the Precipitation medium within the spinning tube, but causes one of the threads Pulling direction opposite force, which is the morphology of the thread influenced. In contrast, in the spinning funnel process Flow rate of the precipitation medium inside the funnel high that the threads due to the friction fiber / liquid experienced significant stretching. In both cases they are fresh extruded threads immediately after exiting the spinneret and before Entry into the spinning tube or the spinning funnel on the surface of the nozzle exposed to turbulence, which leads to a Deterioration of the thread uniformity leads.
Während beim Verspinnen von Cellulosexanthogenat-Lösungen zu Viskosefasern bei Eintritt in das Fällbad gleichzeitig eine Koagulation und eine Verseifung des Xanthogenates zu Regenerat-Cellulosefasern mit deutlich höherer Festigkeit und Kohärenz erfolgt, erfährt das Cellulosecarbamat lediglich eine Koagulation. Die frisch ersponnenen Cellulosecarbamat-Fasern sind folglich sehr viel anfälliger gegenüber Turbulenzen oder sonstigen Störungen sowie gegen Verstreckungskräfte innerhalb des Fällbades als Regenerat-Cellulosefasern. Eine unmittelbare Übertragung der bei Viskose oder Cellulose-NMMO-Lösungen angewandten Spinntechniken auf das Verspinnen von Cellulosecarbamat-Lösungen ist daher nicht möglich bzw. führt zu Fasern schlechter Qualität.While spinning cellulose xanthate solutions too Viscose fibers coagulate when entering the precipitation bath and saponification of the xanthate to regenerate cellulose fibers experience significantly higher strength and coherence Cellulose carbamate is just a coagulation. The freshly spun Cellulose carbamate fibers are therefore much more susceptible to Turbulence or other disturbances as well as against stretching forces within the precipitation bath as regenerated cellulose fibers. A immediate transfer of viscose or cellulose NMMO solutions spinning techniques applied to the spinning of cellulose carbamate solutions is therefore not possible or leads to poorer fibers Quality.
Der vorliegenden Erfindung liegt die Aufgabe zugrunde, ein Verfahren und eine Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen zu schaffen, welche Fasern hoher Gleichmäßigkeit und guter Qualität herzustellen erlauben. Auch sollte eine Anpassung an unterschiedliche Spinngeschwindigkeiten leicht zu vollziehen sein.The object of the present invention is a method and a device for spinning cellulose carbamate solutions create which fibers of high uniformity and good quality allow to manufacture. Also an adjustment to different Spinning speeds must be easy to achieve.
Die Lösung dieser Aufgabe erfolgt erfindungsgemäß durch ein Verfahren und eine Vorrichtung gemäß den Angaben der Patentansprüche. Das Verfahren ist dadurch gekennzeichnet, daß die Fasern vom Austritt aus der Spinndüse bis zum Austritt aus dem Fällbad von einem gleichgerichteten Strom des Fällmediums mit vorgegebenem Querschnitt eingehüllt sind, wobei die Strömungsgeschwindigkeit des Fällmediums am Austritt der Fasern aus der Spinndüse (Ebene X1) gleich dem 0,1 bis 0,8fachen und am Austritt der Fasern aus dem Fällbad (Ebene X3) gleich dem 0,96 bis 1,1fachen der Abzugsgeschwindigkeit der Fasern ist. Die Vorrichtung zur Ausführung des Verfahrens ist dadurch gekennzeichnet, daß sie im wesentlichen aus einem Fällbadbehälter (15) mit Zuleitung (12) für das Fällmedium und innerhalb des Behälters einer als Strömungskörper ausgebildeten, kegelstumpfförmigen Spinndüse (3) und einem kegelstumpfförmigen (5) Spinntrichter mit anschließendem, durch die Wandung des Fällbadbehälters hinausragenden, zylindrischen Rohr (6) sowie außerhalb des Behälters einer mechanischen Faserabzugsvorrichtung (9) besteht, wobei die Spinndüse (3) unter Ausbildung eines konzentrischen Spaltes in den Spinntrichter (5) eintaucht. Bevorzugt weist die Spinndüse (3) den gleichen, sich in Strömungsrichtung der zu verspinnenden Lösung verjüngenden Kegelwinkel (a) auf, wie der Spinntrichter.According to the invention, this object is achieved by a method and a device according to the claims. The The process is characterized in that the fibers emerge from the outlet the spinneret until it comes out of the coagulation bath rectified flow of the precipitation medium with a given cross section are enveloped, the flow rate of the precipitation medium on The fibers exit the spinneret (plane X1) equal to 0.1 to 0.8 times and the same at the exit of the fibers from the precipitation bath (level X3) is 0.96 to 1.1 times the withdrawal speed of the fibers. The Device for carrying out the method is characterized in that that they essentially from a precipitation bath tank (15) with a feed line (12) for the precipitation medium and within the container one as Flow body trained, frustoconical spinneret (3) and a frustoconical (5) spinning funnel followed by cylindrical tube (6) protruding from the wall of the precipitation bath tank as well as outside the container of a mechanical fiber draw-off device (9), the spinneret (3) forming a immerses concentric gap in the spinning funnel (5). Prefers the spinneret (3) has the same, in Flow direction of the tapered cone angle of the solution to be spun (a) on how the spinning funnel.
Die Erfindung wird nachfolgend unter Bezug auf die beispielhaft gegebenen, nicht maßstabsgerechten Prinzipskizzen näher erörtert. Hierbei stellt
- Fig. 1
- eine erfindungsgemäße Vorrichtung mit vertikaler Spinnanordnung und
- Fig. 2
- eine erfindungsgemäße Vorrichtung mit horizontal er Spinnanordnung dar.
- Fig. 1
- a device according to the invention with a vertical spinning arrangement and
- Fig. 2
- a device according to the invention with a horizontal spinning arrangement.
Beim Spinnen von Cellulosecarbamat sind die Filamente unmittelbar nach Eintritt in das Fällbad sehr labil. Bei extrem niedrigen Fadenabzugsgeschwindigkeiten könnte das Koagulieren der Fäden in einem stehenden Fällbad durchgeführt werden. Mit zunehmender Fadenabzugsgeschwindigkeit und somit steigender Reibung zwischen Faden und Fällbad treten jedoch vermehrt Turbulenzen an der Düsenoberfläche und längs der Filamente auf, die zu einer Verschlechterung der Fadenqualität führen. Um diese Turbulenzen zu unterbinden und die Faden/Flüssigkeit-Reibung zu reduzieren, wird erfindungsgemäß von außen eine gerichtete Strömung (UB) auf den Filamentfächer (4) aufgeprägt. Dabei muß vermieden werden, daß die aufgeprägte Strömung an der Unterkante der Spinndüse (3) in der Ebene X1 ablöst und eine turbulente Strömung bildet. Dies wird erreicht, indem man die Filamente (4) im Konus (5) eines Spinntrichters durch die im vorderen Boden der Spinndüse (Ebene X1) angeordneten Düsenbohrungen einer als Strömungskörper ausgebildeten, kegelstumpfförmigen Spinndüse (3) spinnt. Dabei werden die Filamente (4) direkt unterhalb der Spinndüse (3) unter einem möglichst kleinen Winkel vom Fällmedium angeströmt und mitgenommen. Dazu muß die Spinndüse (3) unter Ausbildung eines konzentrischen Spaltes mit der Spaltbreite (d) in den Spinntrichter (5) eintauchen. Bevorzugt weisen Spinndüse (3) und Trichterkonus (5) den gleichen, sich in Strömungsrichtung des Fällbades verjüngenden Kegelwinkel (a) auf. Die Strömungsgeschwindigkeit (UB) des Fällmediums beträgt das 0,1 bis 0,8fache der Abzugsgeschwindigkeit (UAB) der Fasern am Austritt der Fasern aus der Spinndüse (Ebene X1) und das 0,96 bis 1,1fache am Austritt der Fasern aus dem Fällbad (Ebene X3). Die Strömungsgeschwindigkeit des Fällmediums am Austritt der Fasern aus den Fällbad (Ebene X3) ist in jedem Fall bezogen auf den Querschnitt des zylindrischen Spinnrohrteils mit Durchmesser T2. Ein eventuell in Strömungsrichtung an den Rohrteil in der Ebene X3 anschließendes konusförmiges Endstück und/oder eine Blende mit variablen Öffnung bleiben hierbei unberücksichtigt (Strömungsgeschwindigkeit des Fällmediums hier entsprechend dem verengten Querschnitt höher als in Ebene X3).When spinning cellulose carbamate, the filaments are very unstable immediately after entering the precipitation bath. At extremely low thread take-off speeds, the threads could be coagulated in a standing precipitation bath. However, with increasing thread take-off speed and thus increasing friction between the thread and the precipitation bath, turbulence increasingly occurs on the nozzle surface and along the filaments, which lead to a deterioration in the thread quality. In order to prevent this turbulence and to reduce the thread / liquid friction, according to the invention a directed flow (U B ) is impressed on the filament compartments (4). It must be avoided that the impressed flow on the lower edge of the spinneret (3) in the plane X1 detaches and forms a turbulent flow. This is achieved by spinning the filaments (4) in the cone (5) of a spinning funnel through the nozzle bores in the front bottom of the spinneret (plane X1) of a truncated cone-shaped spinneret (3) designed as a flow body. The filaments (4) flow directly below the spinneret (3) from the precipitation medium at the smallest possible angle and are carried along. For this purpose, the spinneret (3) must be immersed in the spinning funnel (5), forming a concentric gap with the gap width (d). The spinneret (3) and funnel cone (5) preferably have the same cone angle (a) that tapers in the direction of flow of the precipitation bath. The flow rate (U B ) of the precipitation medium is 0.1 to 0.8 times the withdrawal rate (U AB ) of the fibers at the exit of the fibers from the spinneret (plane X1) and 0.96 to 1.1 times the exit of the fibers the precipitation bath (level X3). The flow rate of the precipitation medium at the exit of the fibers from the precipitation bath (level X3) is in any case based on the cross section of the cylindrical spinning tube part with diameter T2. Any conical end piece that adjoins the pipe part in plane X3 in the direction of flow and / or an orifice plate with a variable opening are not taken into account here (flow rate of the precipitation medium here is higher than in plane X3 in accordance with the narrowed cross section).
Die Strömungsgeschwindigkeit (UB) des Fällmediums in der Ebene X3 ist
über die hydrostatische Höhe (H) des Fällbades, entsprechend
Fig. 1 zeigt eine vertikale Spinnanordnung mit einer Spinnrichtung von oben nach unten, die besonders für höhere Faserabzugsgeschwindigkeiten geeignet ist. Die Cellulosecarbamat-Spinnlösung, bestehend vorzugsweise aus 5 bis 12 Gew.-% Cellulosecarbamat in 5 bis 10%iger wässriger Natriumhydroxid-Lösung, wird mit einer Temperatur von etwa 0 bis +30 °C durch die Spinnpumpe (1) über die Leitung (2) der Spinndüse (3) zugeführt. Die an der Spinndüse (3) austretenden Fäden (4) werden durch das von oben nach unten den Spinntrichter (5) durchströmende Fällmedium unter kleinem Winkel diagonal angeströmt (UB) und mitgenommen. Der Spinntrichter besteht aus einem oben kegelstumpfförmigen Teil (5) und in der Ebene (X2) daran anschließend einem zylindrischen, rohrförmigen Teil (6), welcher, wie hier gezeigt, in Ebene X3 endet. Wahlweise kann das Rohr aber auch mit einem in der Ebene X3 daran anschließenden, konischen Endstück und/oder einer Blende enden. Die Filamente (4) werden von einer mechanischen Abzugsvorrichtung (9), beispielsweise einem angetriebenen Galettenpaar, mit der Geschwindigkeit (UAB) abgezogen, während der sie begleitende Strom des Fällmediums in den Vorratsbehälter (10) abfließt. Die Cellulosecarbamat-Fasern werden danach gewaschen, verstreckt und bei höherer Temperatur zu Regeneratcellulose-Fasern verseift.1 shows a vertical spinning arrangement with a spinning direction from top to bottom, which is particularly suitable for higher fiber take-off speeds. The cellulose carbamate spinning solution, preferably consisting of 5 to 12% by weight of cellulose carbamate in 5 to 10% aqueous sodium hydroxide solution, is at a temperature of about 0 to +30 ° C by the spinning pump (1) via line (2 ) fed to the spinneret (3). The threads (4) emerging at the spinneret (3) are flowed diagonally (U B ) at a small angle by the precipitation medium flowing through the spinning funnel (5) from top to bottom and taken along. The spinning funnel consists of a frustoconical part (5) and in the plane (X2) adjoining it a cylindrical, tubular part (6) which, as shown here, ends in plane X3. Alternatively, the tube can also end with a conical end piece and / or a diaphragm attached to it in plane X3. The filaments (4) are drawn off by a mechanical take-off device (9), for example a driven pair of godets, at the speed (U AB ) while the accompanying stream of the precipitation medium flows into the storage container (10). The cellulose carbamate fibers are then washed, drawn and saponified to regenerate cellulose fibers at a higher temperature.
Das Fällmedium gelangt vom Vorratsbehälter (10) mittels Pumpe (11) über die Leitung (12) in den Fällbadbehälter (15), der zwecks gleichmäßigem, turbulenzfreien Zulauf des Fällmediums mit einer als Überlauf ausgebildeten, bevorzugt konzentrisch oder parallel zur Behälterwandung angeordneten Innenwand (13) ausgerüstet ist. Über die Wand (13) fließt das Fällmedium in den Spinntrichter (5). Als Fällmedium verwendbar sind sowohl wässrige Lösungen von Säuren als auch von Alkalien und/oder Salzen. Auch Alkohole sind geeignet. Bevorzugt wird eine wässrige Lösung mit 5 bis 25 Gew. -% H2SO4 und 5 bis 25 Gew.-% Na2SO4 bei einer Temperatur von etwa 20 bis 60 °C. Durch Reaktion mit der alkalischen Spinnlösung reichert sich das Fällmedium beim Durchströmen des Spinntrichters (5 und 6) mit den sich dabei bildenden Salzen, zum Beispiel Natriumsulfat, an. Bis zu einer gewissen, von der Zusammensetzung des Fällmediums abhängigen Konzentration können diese Salze im Fällmedium verbleiben. Da sich das untere Ende des Spinntrichters (6) außerhalb des Fällbadbehälters (15) befindet, kann die Zusammensetzung des aus dem Spinnrohrteil (6) ausfließenden Fällmediums leicht korrigiert werden, bevor es über die Leitung (12) in den Behälter (15) zurückgepumpt wird, zum Beispiel durch partielle Ausschleusung über Leitung (18) und Frischzufuhr über Leitung (17).The precipitation medium passes from the storage container (10) by means of a pump (11) via the line (12) into the precipitation bath container (15), which for the purpose of a uniform, turbulence-free inflow of the precipitation medium with an inner wall (13) designed as an overflow, preferably arranged concentrically or parallel to the container wall ) is equipped. The precipitation medium flows into the spinning funnel (5) via the wall (13). Both aqueous solutions of acids and of alkalis and / or salts can be used as the precipitation medium. Alcohols are also suitable. An aqueous solution with 5 to 25% by weight H 2 SO 4 and 5 to 25% by weight Na 2 SO 4 at a temperature of about 20 to 60 ° C. is preferred. As a result of reaction with the alkaline spinning solution, the precipitation medium is enriched with the salts which form, for example sodium sulfate, as it flows through the spinning funnel (5 and 6). These salts can remain in the precipitation medium up to a certain concentration depending on the composition of the precipitation medium. Since the lower end of the spinning funnel (6) is outside the precipitation bath container (15), the composition of the precipitation medium flowing out of the spinning tube part (6) can be easily corrected before it is pumped back into the container (15) via the line (12) , for example by partial discharge via line (18) and fresh supply via line (17).
Die Faserabzugsgeschwindigkeit (UAB) richtet sich nach dem verwendeten Equipment und insbesondere dem Titer der zu erspinnenden Fasern. Allgemein sind Abzugsgeschwindigkeiten von 30 bis 500 m/min, vorzugsweise 50 bis 350 m/min gut geeignet. Die entsprechende, vorzugsweise etwa gleich hohe Strömungsgeschwindigkeit des Fällmediums in der Ebene (X3) wird durch vertikales Verschieben des Spinntrichters (5 und 6) in bezug auf die Position des Fällbadbehälters (15) und folglich durch Verändern der hydrostatischen Höhe (H) des Fällmediums eingestellt. Die Anströmgeschwindigkeit des Fällmediums auf der Ebene (X1) wird dabei gleichzeitig durch Verändern der Eintauchtiefe (lt) der Spinndüse (3) in den Spinntrichter (5) angepaßt. Eine zusätzliche Anpassung kann gegebenenfalls durch vertikales Verschieben des Fällbadbehälters (15) bei unveränderter hydrostatischer Höhe (H) und/oder durch vertikal es Verschieben der Spinndüse (3) vorgenommen werden. Auch ein vertikales Verschieben des Fällbadbehälters (15) in bezug auf die Position des Spinntrichters und/oder ein Verändern der Länge des rohrförmigen Teils (6) des Spinntrichters sind möglich. The fiber take-off speed (U AB ) depends on the equipment used and in particular the titer of the fibers to be spun. In general, take-off speeds of 30 to 500 m / min, preferably 50 to 350 m / min are well suited. The corresponding, preferably approximately the same flow rate of the precipitation medium in the plane (X3) is adjusted by vertically shifting the spinning funnel (5 and 6) in relation to the position of the precipitation bath container (15) and consequently by changing the hydrostatic height (H) of the precipitation medium . The flow velocity of the precipitation medium on the plane (X1) is adjusted at the same time by changing the immersion depth (lt) of the spinneret (3) in the spinning funnel (5). An additional adjustment can optionally be made by vertically shifting the precipitation bath container (15) with unchanged hydrostatic height (H) and / or by vertically shifting the spinneret (3). Vertical displacement of the precipitation bath container (15) with respect to the position of the spinning funnel and / or changing the length of the tubular part (6) of the spinning funnel are also possible.
Fig. 2 zeigt schematisch eine andere, vorzugsweise für niedrige Faserabzugsgeschwindigkeiten (UAB) eingesetzte Ausführung der erfindungsgemäßen Vorrichtung. Die einzelnen Elemente der Vorrichtung entsprechen denen in Fig. 1, Spinndüse und Spinntrichter sind jedoch horizontal angeordnet.2 schematically shows another embodiment of the device according to the invention, preferably used for low fiber draw-off speeds (U AB ). The individual elements of the device correspond to those in FIG. 1, but the spinneret and spinning funnel are arranged horizontally.
Die Cellulosecarbamat-Spinnlösung wird über Leitung (2) der Spinndüse (3) zugeführt und die ersponnenen Fäden von der Abzugsvorrichtung (9) durch den Spinntrichter (5 und 6) abgezogen. Spinndüse (3) und der kegelstumpfförmige Teil (5) des Spinntrichters sind innerhalb des Fällbadbehälters (15) im Fällmedium angeordnet, während der rohrförmige Teil (6) des Spinntrichters durch die Wandung des Behälters nach außen durchgeführt ist. Das Fällmedium wird vom Vorratsbehälter (10) mittels der Pumpe (11) über die Leitung (12) dem Fällbadbehälter (15) zugeführt. Zur Vermeidung von Turbulenzen innerhalb des Fällbadbehälters (15) sind Zuleitung (12) und Spinndüsenbereich durch eine permeable Wand (14) von einander getrennt. Die Einstellung des Flüssigkeitsniveaus bzw. der hydrostatischen Höhe (H) im Fällbadbehälter (15) erfolgt über eine am Behälterboden angebrachte Abflußleitung (16) und/oder verschiedene Überlaufleitungen. Das Fällmedium fließt auf Grund des hydrostatischen Druckes in Spinnrichtung durch den Spinntrichter (5) und tritt am Ende des Spinnrohres (6) in der Ebene (X3) wieder aus, von wo es, gegebenenfalls nach Konzentrations-Einstellung, in den Vorratsbehälter (10) gelangt. Zur Einstellung der Strömungsgeschwindigkeit (UB) des Fällmediums in der Ebene (X1) bzw. der Eintauchtiefe (lt) der Spinndüse (3) in den Spinntrichter (5) ist der gesamte Spinntrichter (5 und 6) in bezug auf die Position des Fällbadbehälters (15) horizontal verschiebbar angeordnet. Alternativ oder zusätzlich könnte auch die Spinndüse (3) horizontal verschoben werden. The cellulose carbamate spinning solution is fed via line (2) to the spinneret (3) and the spun threads are drawn off from the take-off device (9) through the spinning funnel (5 and 6). Spinning nozzle (3) and the frustoconical part (5) of the spinning funnel are arranged in the precipitation medium inside the precipitation bath container (15), while the tubular part (6) of the spinning funnel is passed through the wall of the container to the outside. The precipitation medium is fed from the storage container (10) to the precipitation bath container (15) by means of the pump (11) via the line (12). In order to avoid turbulence within the precipitation bath container (15), the feed line (12) and the spinneret area are separated from one another by a permeable wall (14). The liquid level or the hydrostatic height (H) in the precipitation bath tank (15) is set via a drain pipe (16) attached to the tank bottom and / or various overflow pipes. The precipitating medium flows through the spinning funnel (5) due to the hydrostatic pressure in the spinning direction and exits at the end of the spinning tube (6) in the plane (X3), from where it, if necessary after setting the concentration, into the storage container (10) reached. To set the flow rate (U B ) of the precipitation medium in the plane (X1) or the immersion depth (lt) of the spinneret (3) in the spinning funnel (5), the entire spinning funnel (5 and 6) is in relation to the position of the precipitation bath container (15) arranged horizontally. Alternatively or additionally, the spinneret (3) could also be moved horizontally.
Die Abmessungen der erfindungsgemäßen Vorrichtung richten sich nach dem beabsichtigten Durchsatz. Bei industriellen Anlagen liegt beispielsweise der Spinndüsendurchmesser (D) bei 10 bis 300 bis 4000 mm, vorzugsweise der Spinntrichterdurchmesser (T1) bei 20 bis 500 mm, der Spinnrohrdurchmesser (T2) bei 3 bis 150 mm, der Kegelwinkel (a) bei 5 bis 30°, die Gesamtlänge des Spinntrichters einschließlich Spinnrohr (5 und 6) bei 300 bis 4000 mm, vorzugsweise bis 2000 mm und die hydrostatische Höhe (H) bei 10 bis etwa 4000 mm, vorzugsweise bis etwa 2000 mm. Als Konstruktionsmaterial kommen Glas sowie korrosionsbeständige Kunststoffe und Metalle in Betracht.The dimensions of the device according to the invention depend on the intended throughput. In industrial plants for example the spinneret diameter (D) at 10 to 300 to 4000 mm, preferably the spinning funnel diameter (T1) at 20 to 500 mm, the spinning tube diameter (T2) at 3 to 150 mm, the cone angle (a) at 5 to 30 °, including the total length of the spinning funnel Spinning tube (5 and 6) at 300 to 4000 mm, preferably up to 2000 mm and the hydrostatic height (H) at 10 to about 4000 mm, preferably up to about 2000 mm. As construction material come glass as well corrosion-resistant plastics and metals.
Spinndüse (3) und Spinntrichter (5 und 6) können nicht nur, wie vorstehend geschildert, vertikal oder horizontal angeordnet sein, sondern auch schräg zur Vertikalen oder zur Horizontalen.Spinning nozzle (3) and spinning funnel (5 and 6) can not only how described above, arranged vertically or horizontally, but also at an angle to the vertical or horizontal.
Das zu verspinnende Cellulosecarbamat kann in beliebiger Weise hergestellt worden sein, beispielsweise nach einem der Verfahren des US-Patentes 5 378 827, der DE-Patentanmeldungen 4 417 140, 196 35 473 und 197 15 617.The cellulose carbamate to be spun can be used in any way have been produced, for example by one of the methods of U.S. Patent 5,378,827, DE Patent Applications 4,417,140, 196 35,473 and 197 15 617.
Claims (12)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE19721609 | 1997-05-23 | ||
DE19721609A DE19721609A1 (en) | 1997-05-23 | 1997-05-23 | Method and device for spinning cellulose carbamate solutions |
Publications (3)
Publication Number | Publication Date |
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EP0879906A2 true EP0879906A2 (en) | 1998-11-25 |
EP0879906A3 EP0879906A3 (en) | 1998-12-30 |
EP0879906B1 EP0879906B1 (en) | 2001-12-19 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP98108315A Expired - Lifetime EP0879906B1 (en) | 1997-05-23 | 1998-05-07 | Process and device for spinning solutions of cellulose carbamate |
Country Status (5)
Country | Link |
---|---|
US (2) | US5968433A (en) |
EP (1) | EP0879906B1 (en) |
AT (1) | ATE211190T1 (en) |
DE (2) | DE19721609A1 (en) |
ES (1) | ES2165641T3 (en) |
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DE10060879B4 (en) * | 2000-12-07 | 2005-08-04 | Zimmer Ag | Spinning funnel device |
WO2005080660A1 (en) * | 2004-02-17 | 2005-09-01 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for producing non-wovens, a corresponding non-woven and the production thereof |
WO2005080661A1 (en) | 2004-02-17 | 2005-09-01 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for the production of non-wovens, non-wovens, and use thereof |
DE10060877B4 (en) * | 2000-12-07 | 2006-01-26 | Zimmer Ag | Spinntrichtervorrichtung with center feed |
WO2007000319A1 (en) * | 2005-06-27 | 2007-01-04 | Fraunhofer-Gesellschaft Zur Förderung Der Angewanddten Forschung E.V. | Bonded fabrics, method for the production thereof and their use |
EP2110467A1 (en) * | 2008-04-14 | 2009-10-21 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Cellulose carbamate spinning solution, method for producing a cellulose carbamate non-woven fabric, cellulose carbamate non-woven fabric and applications |
US8454884B2 (en) | 2008-04-14 | 2013-06-04 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung E.V. | Method of producing cellulose carbamate blown film and use of the same |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN100516326C (en) * | 2007-08-20 | 2009-07-22 | 中国科学院新疆理化技术研究所 | Process for preparing cellulose carbamate fibre |
DE102008018743A1 (en) * | 2008-04-14 | 2009-10-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Cellulose carbamate spinning solution, cellulose carbamate fiber and process for their preparation and uses |
CN111534869A (en) * | 2020-05-10 | 2020-08-14 | 西南大学 | Miniature wet spinning drafting device |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1660144B1 (en) * | 1964-03-25 | 1972-06-29 | Asahi Chemical Ind | Spinning funnel for wet draw spinning of copper ammonia silk at high speed |
EP0383250A2 (en) * | 1989-02-15 | 1990-08-22 | Akzo Nobel N.V. | Process and apparatus for producing synthetic fibres by the wet-spinning method using a spinning-tube |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US710819A (en) * | 1902-04-01 | 1902-10-07 | Edmund Thiele | Manufacture of filaments from cellulose solutions. |
US957460A (en) * | 1908-05-07 | 1910-05-10 | Emil Elsaesser | Machine for spinning viscous liquids. |
BE365456A (en) * | 1928-11-19 | |||
NL87315C (en) * | 1955-09-07 | |||
US2872701A (en) * | 1955-11-14 | 1959-02-10 | American Viscose Corp | Artificial yarn producing apparatus |
US3481390A (en) * | 1966-05-02 | 1969-12-02 | United Aircraft Corp | Process for making composite fibers |
US4178431A (en) * | 1976-05-28 | 1979-12-11 | Ube Industries, Ltd. | Aromatic copolyamide fiber from benzidine sulfone or diamino phenanthridone |
FI64603C (en) * | 1981-12-30 | 1983-12-12 | Neste Oy | EXTENSION OF CELLULOSE EXTENSION |
FI64605C (en) * | 1982-03-30 | 1983-12-12 | Neste Oy | FOERFARANDE FOER BEHANDLING AV FIBER AV CELLULOSADERIVAT |
FI69851C (en) * | 1984-09-27 | 1986-05-26 | Neste Oy | FOERFARANDE FOER UTFAELLNING AV CELLULOSAKARBAMAT |
FI69852C (en) * | 1984-09-27 | 1986-05-26 | Neste Oy | CYCLIC FAR OIL FRAMING PROCESSING AND ENCOALIZATION OF CELLULOSE CARBAMATE FOR UTFAELLING AV CARBAMATE OCH FOERAOTERVINNING AV KEMIKALIERNA |
FI69853C (en) * | 1984-09-27 | 1986-05-26 | Neste Oy | CYCLIC FAR OIL FRAMING PROCESSING AND ENCOALIZATION OF CELLULOSE CARBAMATE FOR UTFAELLING AV CARBAMATE OCH FOERAOTERVINNING AV KEMIKALIERNA |
DE4219658C3 (en) * | 1992-06-16 | 2001-06-13 | Ostthueringische Materialpruef | Process for the production of cellulose fiber filaments and films by the dry-wet extrusion process |
DE19515136C2 (en) * | 1995-04-25 | 1999-12-16 | Ostthueringische Materialpruef | Spinning funnel |
-
1997
- 1997-05-23 DE DE19721609A patent/DE19721609A1/en not_active Withdrawn
-
1998
- 1998-03-26 US US09/048,654 patent/US5968433A/en not_active Expired - Fee Related
- 1998-05-07 DE DE59802501T patent/DE59802501D1/en not_active Expired - Fee Related
- 1998-05-07 ES ES98108315T patent/ES2165641T3/en not_active Expired - Lifetime
- 1998-05-07 AT AT98108315T patent/ATE211190T1/en not_active IP Right Cessation
- 1998-05-07 EP EP98108315A patent/EP0879906B1/en not_active Expired - Lifetime
-
1999
- 1999-06-25 US US09/344,744 patent/US6234778B1/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1660144B1 (en) * | 1964-03-25 | 1972-06-29 | Asahi Chemical Ind | Spinning funnel for wet draw spinning of copper ammonia silk at high speed |
EP0383250A2 (en) * | 1989-02-15 | 1990-08-22 | Akzo Nobel N.V. | Process and apparatus for producing synthetic fibres by the wet-spinning method using a spinning-tube |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10060879B4 (en) * | 2000-12-07 | 2005-08-04 | Zimmer Ag | Spinning funnel device |
DE10060877B4 (en) * | 2000-12-07 | 2006-01-26 | Zimmer Ag | Spinntrichtervorrichtung with center feed |
WO2005080660A1 (en) * | 2004-02-17 | 2005-09-01 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for producing non-wovens, a corresponding non-woven and the production thereof |
WO2005080661A1 (en) | 2004-02-17 | 2005-09-01 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for the production of non-wovens, non-wovens, and use thereof |
WO2007000319A1 (en) * | 2005-06-27 | 2007-01-04 | Fraunhofer-Gesellschaft Zur Förderung Der Angewanddten Forschung E.V. | Bonded fabrics, method for the production thereof and their use |
EP2110467A1 (en) * | 2008-04-14 | 2009-10-21 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Cellulose carbamate spinning solution, method for producing a cellulose carbamate non-woven fabric, cellulose carbamate non-woven fabric and applications |
US8263507B2 (en) | 2008-04-14 | 2012-09-11 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung, E.V. | Cellulose carbamate spinning solution, method for producing a cellulose carbamate nonwoven, and use of the same |
US8454884B2 (en) | 2008-04-14 | 2013-06-04 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung E.V. | Method of producing cellulose carbamate blown film and use of the same |
Also Published As
Publication number | Publication date |
---|---|
US5968433A (en) | 1999-10-19 |
ATE211190T1 (en) | 2002-01-15 |
DE19721609A1 (en) | 1998-11-26 |
US6234778B1 (en) | 2001-05-22 |
EP0879906A3 (en) | 1998-12-30 |
EP0879906B1 (en) | 2001-12-19 |
ES2165641T3 (en) | 2002-03-16 |
DE59802501D1 (en) | 2002-01-31 |
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