EP1268888A1 - Procede et dispositif pour produire des fibres de cellulose et des fils continus de cellulose - Google Patents

Procede et dispositif pour produire des fibres de cellulose et des fils continus de cellulose

Info

Publication number
EP1268888A1
EP1268888A1 EP01957604A EP01957604A EP1268888A1 EP 1268888 A1 EP1268888 A1 EP 1268888A1 EP 01957604 A EP01957604 A EP 01957604A EP 01957604 A EP01957604 A EP 01957604A EP 1268888 A1 EP1268888 A1 EP 1268888A1
Authority
EP
European Patent Office
Prior art keywords
capillary
cellulose
precipitation bath
spinning
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP01957604A
Other languages
German (de)
English (en)
Other versions
EP1268888B1 (fr
Inventor
Christoph Michels
Birgit Kosan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Original Assignee
Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE2000111948 external-priority patent/DE10011948C2/de
Application filed by Thueringisches Institut fuer Textil und Kunststoff Forschung eV filed Critical Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Publication of EP1268888A1 publication Critical patent/EP1268888A1/fr
Application granted granted Critical
Publication of EP1268888B1 publication Critical patent/EP1268888B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/04Dry spinning methods

Definitions

  • the main application relates to a process for producing cellulose fibers or filaments from cellulose by the dry-wet extrusion process with aqueous amine oxides, in particular N-methylmorpholine-N-oxide as solvent, in which a) cellulose or a cellulose mixture with a Cuoxam -DP dispersed in the range from 250 to 3000 in aqueous amine oxide, b) the dispersion obtained at elevated temperature with dehydration and shear in a homogeneous solution with a zero shear viscosity in the range from 600 to 6000 Pa-s and a relaxation time in the range from Transferred from 0.3 to 50 s at 85 ° C.
  • c) the solution is fed to at least one spinneret and previously passed through a flow chamber common to the nozzle (s), in which its residence time is at least equal to its relaxation time at the spinning temperature, d) the solution in each spinneret is deformed into at least one capillary and the capillary (s) of each nozzle is distorted h leads a non-precipitating medium and then with precipitation of the cellulose threads through a precipitation bath, and e) separates the cellulose threads at the end of the precipitation bath section by deflection from the precipitation bath streams and withdraws the threads.
  • the main application relates to a device for the production of cellulose fibers or filaments from cellulose by the dry-wet extrusion process with aqueous amine oxides as solvent with a spin pack with a spinneret plate, spinnerets and a common one arranged above the spinneret plate and the spinnerets arranged in a row Inflow chamber, the volume of which corresponds to the relationship V> vy ⁇ , where V is the volume of the inflow chamber in cm 3, v is the volume flow of the cellulose solution in cm3 / s and ⁇ the
  • the main application was based on the task of creating a method and a device by means of which the spinning of fibers and the multiple spinning of filament yarns with good mechanical fiber properties is possible with high capillary density, spinning security and take-off speed.
  • the uniformity and uniformity of the volume flows through each nozzle should be increased compared to the known methods.
  • the gap width a with the relaxation time the spinning solution at the frequency maximum of the relaxation time spectrum at the spinning temperature and the take-off speed v 3 (equation II) and on the other hand correlates with the distance x between two adjacent nozzle holes, the length of the precipitation bath path w and the nozzle hole diameter D (equation III). Since the relaxation time in seconds and the residence time of the deformed solution in gap a are in the millisecond range, it should be possible to achieve much larger gap widths than previously in practical operation. For the spinning of fibers and filaments, the maximum adjustable gap, ie the stretch on which the "solution thread" is more or less strongly oriented according to the draft ratio, is of particular importance.
  • the rate of stretch and thus the thread tension decrease. This has a positive effect on the mechanical fiber parameters, in particular the elongation at break and the loop tearing force.
  • the spinning security decreases with increasing gap width, since the risk of touching the capillaries increases. This is especially true when spinning fibers, where you work with the highest possible capillary density. It is therefore essential to set a maximum gap that does justice to spinning safety, but also results in optimal mechanical fiber parameters. The Decreasing the thread tension is also a prerequisite for increasing the take-off speed, especially when spinning filament yarns.
  • the object of the present invention is therefore in the sense of the main application to create a method and a device by which the spinning of fibers and the multiple spinning of filament yarns with good mechanical fiber properties is possible with high capillary density, spinning security and take-off speed.
  • the mechanical fiber properties namely the elongation at break and the loop tearing force, are to be improved while maintaining the spinning safety.
  • an increase in the take-off speed is to be made possible, in particular when spinning filament yarns.
  • the invention object is also achieved in that, in stage) d Kapillarenschar immediately prior to its entry into the coagulation bath with a gas flows against, wherein the coagulation bath at the interface to the air gap and the gas stream have the same direction of flow components.
  • the effect of increasing the maximum gap width is thus also achieved if the gas flow and the precipitation bath flow have horizontal flow components which are in the same direction.
  • the flow of capillaries is flown with a flat, flat gas stream that extends over the entire width of the row of capillary groups. It is important that the gas flow becomes effective at the immersion points of the capillary sheets in the precipitation bath.
  • the object is further achieved according to the invention in the device mentioned at the outset in that in the gap a at least one slot nozzle with an angle * directed at an angle * to the direction of the capillary in the region 45 ° ⁇ c ⁇ 90 ° for the inflow of capillaries before they enter the Precipitation bath is arranged.
  • the slot width can be, for example, 0.05 to 5 mm, for example 1 mm.
  • the slot length corresponds at least to the length of the row of capillary inflows. These are preferably arranged in a row (not in a plurality of rows which are staggered one behind the other) so that all the sheets are flowed through in the same way by the gas stream.
  • the device mentioned at the outset is preferably characterized in that the upper bath container on the one hand of the capillary sheets has at least one inlet opening for precipitation bath liquid and on the other hand the capillary sheets at least have an overflow and the slot die with respect to the row of capillary sheets is on the same side as the inlet opening (s) is arranged.
  • the precipitation bath liquid and the gas stream in the gap have rectified horizontal flow components, which increases the maximum Gap width is conducive.
  • the slot die is preferably mechanically connected to the at least one overflow.
  • the slot gas nozzle is therefore always at the same (small) distance from the precipitation bath surface regardless of the vertical setting of the overflow and thus the size of the gap width.
  • the device mentioned above for the production of cellulose fibers or filaments is further characterized according to the invention in that the width of the gap a and the relaxation time of the spinning solution satisfy the following relationship a ⁇ ⁇ 5 + 16 ⁇ ] y- m '- ⁇ (II.) in which a is the gap width in mm, ⁇ is the relaxation time at the maximum frequency of the relaxation spectrum of the spinning solution, v is the withdrawal speed
  • the dimensions of the spinnerets, the gap width a and the precipitation bath path w preferably satisfy the relationship
  • 1 shows the relaxation time spectrum of a spinning solution with 12% by mass of cellulose (Cuoxam-DP 480) at the spinning temperature of 85.degree.
  • Figure 2 is a schematic representation of an apparatus for producing cellulose fibers and filaments.
  • Figure 3 is a schematic plan view of the device shown in Figure 2.
  • FIGS. 2 and 3 show the upper precipitation bath container 1 of a spinning device according to the invention.
  • the spinnerets 6, of which only one is visible in FIG. 2, are provided with inflow chambers, as is described and illustrated in more detail in the main application.
  • the outlet sides of the spinnerets 6 are at a distance from the precipitation bath surface 7 which forms the air gap a.
  • the bottom 10 of the precipitation bath container 1 is equipped, according to the arrangement of the nozzles 6, with a plurality of thread guide elements 11, through which the thread bundles 12 emerge from the container 1 together with precipitation bath liquid flows 14.
  • the thread bundles 12 of all the thread guide elements 11 are deflected by the precipitation bath streams 14 at an angle and wound up with a suitable tension.
  • the precipitation bath streams 14 enter the lower precipitation bath container (not shown) and are pumped back into the upper precipitation bath container 1 by means of a pump (not shown) via line 16.
  • the precipitation bath path w passed by the thread bundles 12 extends from the bath surface to the point below the thread guide elements 11 where the thread bundles 12 separate from the precipitation bath liquid flows 14.
  • the line 16 opens into a calming chamber 18 (not shown) partially filled with packing elements, from which the precipitation bath liquid flows through the openings 19 into the actual container 1. From Figure 3 it can be seen that the thread guide elements 11 are arranged in a row in the bottom 10 and the thread bundles 12 run parallel to one another parallel to the take-off godet (not shown).
  • the precipitation bath container 1 has two overflows 9 which are vertically adjustable and thus determine the precipitation bath level and the width of the gap a.
  • a nozzle tube 20 with a slot 21 extending over the row of nozzles 6 or the row of capillary sheets 26 is attached to the overflows 9 by means of the holder 23.
  • a weak air flow is applied to the nozzle tube 20 on both sides via the line 24, which can be adjusted via a needle valve (not shown).
  • the air stream 25 leaves the slot 21 (outlet opening 150 mm x 1 mm) linearly over the entire width and inclined to the bath surface 7, so that the capillary sheets come into contact with the air stream immediately before they enter the precipitation bath.
  • the slot nozzle is about 10 mm above the surface of the precipitation bath.
  • the maximum operationally adjustable gap width a increases, and when using nozzles with a diameter of 200 ⁇ m, this gap width decreases.
  • cone nozzles (0 20 mm) with the same number of holes, i.e. decreasing capillary density, an increase in the maximum adjustable gap can be observed.
  • a press-moist mixture (dry content 50.2%) consisting of 188 g spruce sulfite pulp (Cuoxam-DP 480), 10 g cotton linters pulp (Cuoxam-DP 1907) and 0.4 g stabilizer is in 1850 g NMM0 ( Dry content 75%) dispersed, introduced into a kneader with a vertical kneader shaft, 1255 g of water were distilled off under vacuum and shear at a temperature of 90 ° C. and by further “shear stirring” into a microscopically homogeneous cellulose solution of the composition 11.0% cellulose, 77, 1% NMM0 and 11.9% water transferred.
  • the relaxation time at a spinning temperature of 85 ° C was 3.0 s, the zero shear viscosity was 3450 Pa-s.
  • the solution is formed into threads in a piston spinning apparatus, the hot water-heated spinneret holder of which can accommodate either four spinner cones with 12.5 mm (30 mm pitch from nozzle center to nozzle center) or 3 spinning cones with 20.0 mm diameter (40 mm pitch).
  • the spinning box according to FIGS. 2 and 3 is located below the spinning part.
  • the maximum gap width a was without and inventive J max-making in accordance with established incident air flow. After spinning, the filaments were wound up, washed, cut into stacks of 50 mm, finished and dried. They were then subjected to the textile test. The results are shown in Tables 1 and 2. Air was applied in the manner described above with reference to FIGS. 2 and 3. The nozzle outlet opening was 150 mm x 1 mm. The capillaries were contacted with the air stream immediately before entering the precipitation bath. The air nozzle was slanted downward. The slot nozzle was approx. 10 mm above the surface of the precipitation bath.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
EP01957604A 2000-03-11 2001-03-06 Procede et dispositif pour produire des fibres de cellulose et des fils continus de cellulose Expired - Lifetime EP1268888B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE2000111948 DE10011948C2 (de) 1999-11-10 2000-03-11 Verfahren und Vorrichtung zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen
DE10011948 2000-03-11
PCT/DE2001/000901 WO2001068958A1 (fr) 2000-03-11 2001-03-06 Procede et dispositif pour produire des fibres de cellulose et des fils continus de cellulose

Publications (2)

Publication Number Publication Date
EP1268888A1 true EP1268888A1 (fr) 2003-01-02
EP1268888B1 EP1268888B1 (fr) 2005-11-09

Family

ID=7634388

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01957604A Expired - Lifetime EP1268888B1 (fr) 2000-03-11 2001-03-06 Procede et dispositif pour produire des fibres de cellulose et des fils continus de cellulose

Country Status (8)

Country Link
US (1) US6887409B2 (fr)
EP (1) EP1268888B1 (fr)
KR (1) KR100760642B1 (fr)
CN (1) CN1205364C (fr)
AT (1) ATE309400T1 (fr)
AU (1) AU2001281467A1 (fr)
DE (2) DE50107999D1 (fr)
WO (1) WO2001068958A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10062083B4 (de) * 2000-12-13 2008-04-10 Ostthüringische Materialprüfgesellschaft Für Textil Und Kunststoffe Mbh Verfahren zur Herstellung von Celluloseendlosformkörpern
DE10112050B4 (de) * 2001-03-14 2004-02-12 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. Verfahren und Vorrichtung zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen
KR100966111B1 (ko) * 2005-03-15 2010-06-28 주식회사 효성 셀룰로오스 멀티 필라멘트의 제조방법
DE102005040000B4 (de) * 2005-08-23 2010-04-01 Lenzing Ag Mehrfachspinndüsenanordnung und Verfahren mit Absaugung und Beblasung
KR101577090B1 (ko) 2011-03-30 2015-12-11 코오롱인더스트리 주식회사 방사용 응고장치
TWI667378B (zh) 2014-01-03 2019-08-01 奧地利商蘭精股份有限公司 纖維素纖維
EP3505659A1 (fr) * 2018-08-30 2019-07-03 Aurotec GmbH Procédé et dispositif de filage des filaments à déviation

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5984655A (en) * 1994-12-22 1999-11-16 Lenzing Aktiengesellschaft Spinning process and apparatus
GB9500387D0 (en) * 1995-01-10 1995-03-01 Courtaulds Fibres Ltd Manufacture of extruded articles
CN1142205C (zh) * 1997-12-14 2004-03-17 纺织品和合成材料研究协会图林根研究所 规则多孔珠状纤维素的制备方法、珠状纤维素及其用途
DE19954152C2 (de) * 1999-11-10 2001-08-09 Thueringisches Inst Textil Verfahren und Vorrichtung zur Herstellung von Cellulosefasern und Cellulosefilamentgarnen
DE10009471B4 (de) * 2000-02-28 2006-07-27 Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. Verfahren zur Herstellung einer Lösung erhöhter thermischer Stabilität von Cellulose in wässrigem Aminoxid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0168958A1 *

Also Published As

Publication number Publication date
KR20020081580A (ko) 2002-10-28
DE10190965D2 (de) 2003-05-08
DE50107999D1 (de) 2005-12-15
US20030116882A1 (en) 2003-06-26
US6887409B2 (en) 2005-05-03
KR100760642B1 (ko) 2007-10-04
CN1416481A (zh) 2003-05-07
AU2001281467A1 (en) 2001-09-24
WO2001068958A1 (fr) 2001-09-20
EP1268888B1 (fr) 2005-11-09
ATE309400T1 (de) 2005-11-15
CN1205364C (zh) 2005-06-08

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