EP0879906B1 - Verfahren und Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen - Google Patents
Verfahren und Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen Download PDFInfo
- Publication number
- EP0879906B1 EP0879906B1 EP98108315A EP98108315A EP0879906B1 EP 0879906 B1 EP0879906 B1 EP 0879906B1 EP 98108315 A EP98108315 A EP 98108315A EP 98108315 A EP98108315 A EP 98108315A EP 0879906 B1 EP0879906 B1 EP 0879906B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- spinning
- precipitating
- bath
- fibres
- medium
- 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.)
- Expired - Lifetime
Links
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Classifications
-
- 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 speed (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 with variable opening are not taken into account here (flow speed of the precipitation medium here, corresponding to the constricted cross section, is higher than in plane X3).
- 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 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 through 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).
- 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.
Landscapes
- 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)
Description
- Fig. 1
- eine erfindungsgemäße Vorrichtung mit vertikaler Spinnanordnung und
- Fig. 2
- eine erfindungsgemäße Vorrichtung mit horizontaler Spinnanordnung dar.
Claims (12)
- Verfahren 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, 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.
- Verfahren gemäß Anspruch 1, dadurch gekennzeichnet, daß der Querschnitt des Stromes des Fällmediums vom Austritt der Fasern aus der Spinndüse in Strömungsrichtung zunächst abnimmt und dann konstant bleibt.
- Verfahren gemäß Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Strömungsgeschwindigkeit des Fällmediums am Austritt der Fasern aus dem Fällbad (Ebene X3) durch Verändern der hydrostatischen Höhe des Fällbades eingestellt wird.
- Verfahren gemäß Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Strömungsgeschwindigkeit des Fällmediums am Austritt der Fasern aus dem Fällbad (Ebene X3) durch Verändern des Förderdruckes des Fällmediums bei abgeschlossenem, vollständig gefülltem Fällbad eingestellt wird.
- Verfahren gemäß einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Strömungsgeschwindigkeit des Fällmediums am Austritt der Fasern aus der Spinndüse durch Verändern des Querschnittes des Stromes des Fällmediums an dieser Stelle eingestellt wird.
- Vorrichtung zur Ausführung des Verfahrens des Anspruches 1, 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 Spinntrichter (5) 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.
- Vorrichtung gemäß Anspruch 6, dadurch gekennzeichnet, daß die Spinndüse (3) den gleichen, sich in Strömungsrichtung der zu verspinnenden Lösung verjüngenden Kegelwinkel (a) aufweist, wie der Spinntrichter.
- Vorrichtung gemäß Anspruch 6 oder 7, dadurch gekennzeichnet, daß die Breite (d) des konzentrischen Spaltes durch Verändern der Eintauchtiefe (lt) der Spinndüse (3) in den Spinntrichter (5) eingestellt wird.
- Vorrichtung gemäß einem der Ansprüche 6 bis 8, dadurch gekennzeichnet, daß der Kegelwinkel (a) 5 bis 30° beträgt.
- Vorrichtung gemäß einem der Ansprüche 6 bis 9, dadurch gekennzeichnet, daß Spinndüse (3) und Spinntrichter (5 und 6) in vertikaler Richtung angeordnet sind.
- Vorrichtung gemäß einem der Ansprüche 6 bis 9, dadurch gekennzeichnet, daß Spinndüse (3) und Spinntrichter (5 und 6) in horizontaler Richtung angeordnet sind.
- Vorrichtung gemäß Anspruch 10, dadurch gekennzeichnet, daß der Spinntrichter (5 und 6) in bezug auf die Position des Fällbadbehälters in vertikaler Richtung verschiebbar ist.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19721609 | 1997-05-23 | ||
DE19721609A DE19721609A1 (de) | 1997-05-23 | 1997-05-23 | Verfahren und Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0879906A2 EP0879906A2 (de) | 1998-11-25 |
EP0879906A3 EP0879906A3 (de) | 1998-12-30 |
EP0879906B1 true EP0879906B1 (de) | 2001-12-19 |
Family
ID=7830283
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98108315A Expired - Lifetime EP0879906B1 (de) | 1997-05-23 | 1998-05-07 | Verfahren und Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen |
Country Status (5)
Country | Link |
---|---|
US (2) | US5968433A (de) |
EP (1) | EP0879906B1 (de) |
AT (1) | ATE211190T1 (de) |
DE (2) | DE19721609A1 (de) |
ES (1) | ES2165641T3 (de) |
Families Citing this family (21)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6705850B1 (en) * | 2000-03-06 | 2004-03-16 | Tei Biosciences, Inc. | Apparatus for biopolymer coagulation in a uniform flow |
DE10060879B4 (de) * | 2000-12-07 | 2005-08-04 | Zimmer Ag | Spinntrichtervorrichtung |
DE10060877B4 (de) * | 2000-12-07 | 2006-01-26 | Zimmer Ag | Spinntrichtervorrichtung mit Mitteneinspeisung |
DE10127189C1 (de) * | 2001-06-05 | 2003-04-17 | Zimmer Ag | Verfahren und Vorrichtung zur Herstellung von Celluloseformkörpern unter Einsatz eines elektrischen Feldes |
DE10200405A1 (de) | 2002-01-08 | 2002-08-01 | Zimmer Ag | Spinnvorrichtung und -verfahren mit Kühlbeblasung |
DE10204381A1 (de) | 2002-01-28 | 2003-08-07 | Zimmer Ag | Ergonomische Spinnanlage |
DE10206089A1 (de) | 2002-02-13 | 2002-08-14 | Zimmer Ag | Bersteinsatz |
DE10314878A1 (de) * | 2003-04-01 | 2004-10-28 | Zimmer Ag | Verfahren und Vorrichtung zur Herstellung nachverstreckter Cellulose-Spinnfäden |
JP2005116593A (ja) * | 2003-10-03 | 2005-04-28 | Ube Ind Ltd | 熱電変換装置 |
DE102004007617B4 (de) * | 2004-02-17 | 2007-02-08 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Herstellung eines Vliesstoffes, Vliesstoff und dessen Verwendung |
DE102004007618A1 (de) * | 2004-02-17 | 2005-09-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Herstellung von Vliesstoffen, Vliesstoff und dessen Verwendung |
DE102004007616B4 (de) * | 2004-02-17 | 2005-12-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Herstellung von Fasern und anderen Formkörpern aus Cellulosecarbamat und/oder regenerierter Cellulose |
US20070298670A1 (en) * | 2004-02-17 | 2007-12-27 | Peter Weigel | Method for Producing Non-Wovens, a Corresponding Non-Woven and the Production Thereof |
DE102004024030A1 (de) | 2004-05-13 | 2005-12-08 | Zimmer Ag | Lyocell-Verfahren mit polymerisationsgradabhängiger Einstellung der Verarbeitungsdauer |
DE102005029793B4 (de) * | 2005-06-27 | 2007-04-26 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Vliesstoffe, Verfahren zu deren Herstellung sowie deren Verwendung |
CN100554318C (zh) * | 2007-06-20 | 2009-10-28 | 中国科学院新疆理化技术研究所 | 低碱含量纤维素氨基甲酸酯溶液的制备方法 |
CN100516326C (zh) * | 2007-08-20 | 2009-07-22 | 中国科学院新疆理化技术研究所 | 纤维素氨基甲酸酯纤维的制备方法 |
DE102008018743A1 (de) * | 2008-04-14 | 2009-10-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Cellulosecarbamat-Spinnlösung, Cellulosecarbamatfaser sowie Verfahren zu deren Herstellung und Verwendungszwecke |
DE102008018746A1 (de) * | 2008-04-14 | 2009-10-15 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Cellulosecarbamat-Spinnlösung, Verfahren zur Herstellung eines Cellulosecarbamat-Vliesstoffes, Cellulosecarbamat-Vliesstoff sowie Verwendungszwecke |
DE102008018745A1 (de) * | 2008-04-14 | 2009-10-15 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Cellulosecarbamat-Spinnlösung, Cellulosecarbamat-Blasfolie sowie Verfahren zu deren Herstellung und Verwendungsmöglichkeiten |
CN111534869A (zh) * | 2020-05-10 | 2020-08-14 | 西南大学 | 一种微型化湿法纺丝牵伸装置 |
Family Cites Families (16)
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 (de) * | 1928-11-19 | |||
BE550185A (de) * | 1955-09-07 | |||
US2872701A (en) * | 1955-11-14 | 1959-02-10 | American Viscose Corp | Artificial yarn producing apparatus |
DE1660144B1 (de) * | 1964-03-25 | 1972-06-29 | Asahi Chemical Ind | Spinntrichter zum Nassstreckspinnen von Kupferammoniakseide mit hoher Geschwindigkeit |
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 (fi) * | 1981-12-30 | 1983-12-12 | Neste Oy | Foerfarande foer utfaellning av cellulosaderivat |
FI64605C (fi) * | 1982-03-30 | 1983-12-12 | Neste Oy | Foerfarande foer behandling av fibrer av cellulosaderivat |
FI69852C (fi) * | 1984-09-27 | 1986-05-26 | Neste Oy | Cykliskt foerfarande foer framstaellning av en alkaliloesning av cellulosakarbamat foer utfaellning av karbamatet och foeraotervinning av kemikalierna |
FI69851C (fi) * | 1984-09-27 | 1986-05-26 | Neste Oy | Foerfarande foer utfaellning av cellulosakarbamat |
FI69853C (fi) * | 1984-09-27 | 1986-05-26 | Neste Oy | Cykliskt foerfarande foer framstaellning av en alkaliloesning av cellulosakarbamat foer utfaellning av karbamatet och foeraotervinning av kemikalierna |
DE3904541A1 (de) * | 1989-02-15 | 1990-08-16 | Akzo Gmbh | Verfahren und vorrichtung zur herstellung kuenstlicher faeden nach dem nassspinnverfahren mit spinnrohr |
DE4219658C3 (de) * | 1992-06-16 | 2001-06-13 | Ostthueringische Materialpruef | Verfahren zur Herstellung von Cellulosefasern -filamenten und -folien nach dem Trocken-Naßextrusionsverfahren |
DE19515136C2 (de) * | 1995-04-25 | 1999-12-16 | Ostthueringische Materialpruef | Spinntrichter |
-
1997
- 1997-05-23 DE DE19721609A patent/DE19721609A1/de not_active Withdrawn
-
1998
- 1998-03-26 US US09/048,654 patent/US5968433A/en not_active Expired - Fee Related
- 1998-05-07 AT AT98108315T patent/ATE211190T1/de not_active IP Right Cessation
- 1998-05-07 ES ES98108315T patent/ES2165641T3/es not_active Expired - Lifetime
- 1998-05-07 DE DE59802501T patent/DE59802501D1/de not_active Expired - Fee Related
- 1998-05-07 EP EP98108315A patent/EP0879906B1/de not_active Expired - Lifetime
-
1999
- 1999-06-25 US US09/344,744 patent/US6234778B1/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
EP0879906A2 (de) | 1998-11-25 |
EP0879906A3 (de) | 1998-12-30 |
US5968433A (en) | 1999-10-19 |
DE59802501D1 (de) | 2002-01-31 |
ES2165641T3 (es) | 2002-03-16 |
US6234778B1 (en) | 2001-05-22 |
DE19721609A1 (de) | 1998-11-26 |
ATE211190T1 (de) | 2002-01-15 |
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