EP0031078B1 - Fibres et filaments synthétiques de titre très fin et procédé de filage à sec pour leur fabrication - Google Patents

Fibres et filaments synthétiques de titre très fin et procédé de filage à sec pour leur fabrication Download PDF

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Publication number
EP0031078B1
EP0031078B1 EP80107777A EP80107777A EP0031078B1 EP 0031078 B1 EP0031078 B1 EP 0031078B1 EP 80107777 A EP80107777 A EP 80107777A EP 80107777 A EP80107777 A EP 80107777A EP 0031078 B1 EP0031078 B1 EP 0031078B1
Authority
EP
European Patent Office
Prior art keywords
spinning
filaments
dtex
dmf
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.)
Expired
Application number
EP80107777A
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German (de)
English (en)
Other versions
EP0031078A2 (fr
EP0031078B2 (fr
EP0031078A3 (en
Inventor
Ulrich Dr. Reinehr
Toni Herbertz
Hermann Josef Jungverdorben
Joachim Dross
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.)
Bayer AG
Original Assignee
Bayer AG
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
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Application filed by Bayer AG filed Critical Bayer AG
Priority to AT80107777T priority Critical patent/ATE20909T1/de
Publication of EP0031078A2 publication Critical patent/EP0031078A2/fr
Publication of EP0031078A3 publication Critical patent/EP0031078A3/de
Application granted granted Critical
Publication of EP0031078B1 publication Critical patent/EP0031078B1/fr
Publication of EP0031078B2 publication Critical patent/EP0031078B2/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • D01D5/08—Melt spinning methods
    • D01D5/098—Melt spinning methods with simultaneous stretching
    • 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
    • D01D5/04—Dry 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2973—Particular cross section
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2973—Particular cross section
    • Y10T428/2978—Surface characteristic

Definitions

  • Such fine-titer fibers which generally have a final fiber titer between 0.4-0.8 dtex, have compared to conventional synthetic fibers, e.g. Acrylic fibers, which are in the titre range from 1.3 dtex, have a number of advantages such as: high gloss, appealing chandelier, elegance in the fabric, soft feel, high flexibility and pliability as well as high fiber strength, due to the high number of fine fibers in the yarn cross-section.
  • the object of the present invention was to produce fine-titer acrylic fibers by a dry spinning process.
  • the spinning solution in the spinning shaft must be subjected to a high degree of warpage.
  • the warping (V) during spinning is defined as the ratio of the take-off speed to the ejection speed
  • the present invention therefore relates to a process for the production of synthetic fibers and threads from spinning solutions with a solids content of 25 to 35% of thread-forming acrylonitrile polymers with at least 85% by weight of acrylonitrile units in polar organic solvents after a dry spinning process at a spinning shaft temperature of preferably between 30 ° C.
  • the process according to the invention is in principle a dry spinning process which can be carried out with the same equipment as a process by which coarser titers are spun. So can for example, with the usual spinnerets with hole diameters of about 0.15 to 0.8 mm, preferably 0.2 to 0.4 mm, and in usual spinning shafts. With average K values of the polymers of about 80, the spinning solutions thus have viscosities of about 20 to 100 falling ball seconds at 80 ° C. (for the falling ball method, see K. Jost, Rheologica Acta (1958) Vol. 1, No. 2-3, page 303).
  • the viscosity stability of the spinning solution is important so that the high warpage, which is preferably 30 to 500 but can also be higher, can be exerted by the process according to the invention.
  • a viscosity-stable spinning solution can be prepared by keeping the solution at a certain minimum temperature for a certain time before spinning.
  • the spinning solution should not have a temperature of above 150 ° C, the spinning shaft temperature should not exceed 200 ° C and the spinning air temperature at most about 400 ° C should be.
  • a non-dumbbell-shaped cross-sectional shape of the fine-titer fibers is always obtained by the process according to the invention if the spinning conditions are chosen to be as mild as possible and the work is carried out with high delays.
  • the spinning solution for example, is cooled to temperatures of about 20 ° C. to about 100 ° C. after the viscosity-stabilizing thermal treatment and before spinning, at the same time the spinning shaft temperature is set to a value between about 30 ° C. and preferably below the boiling point of the solvent used and with Spinning air worked up to about 300 ° C.
  • the fiber cross section also has an intermediate shape, e.g. a bean or kidney shape.
  • the spinning solution had a viscosity of 30 ball falling seconds measured at 80 ° C. This value remained unchanged after 1, 3 and 5 hours.
  • the spinning solution was then cooled to 35 ° C. and dry spun from a 720 hole nozzle with nozzle hole diameters of 0.2 mm.
  • the shaft temperature was 50 ° C, the air temperature 200 ° C and the air volume 40 m 3 / h.
  • the take-off speed was 400 m / min.
  • the dwell time of the threads in the spinning shaft was 0.87 seconds. 19.8 ccm / min were conveyed from the spinning pump.
  • the total spin titer was 144 dtex and the residual solvent content of DMF in the spun material was 9.9% by weight, based on polymer solids.
  • the DMF evaporation rate is then calculated to be 0.305
  • the single spin titer was 0.2 dtex.
  • the warpage V was 457.
  • the threads were wetted with oil-containing preparation at the shaft exit, wound on bobbins, folded into a cable, stretched 1: 3.6 times in boiling water and aftertreated in the usual way to give fibers with a final titre of 0.07 dtex.
  • the fiber capillaries were embedded in methyl methacrylate and cross-cut.
  • the light microscopic images produced in the differential interference contrast method showed that the sample cross sections are completely uniform and round.
  • the mean thread diameter was determined with the fiber measuring eyepiece.
  • the fibers had an extremely high gloss. When examined in a scanning electron microscope, the fibers showed smooth surfaces with longitudinal stripes. The striations were completely parallel to the fiber axis and, unlike those with conventional acrylic fibers, were not interrupted.
  • An acrylonitrile copolymer with the chemical composition of Example 1 was, as described there, dissolved in DMF, filtered and the spinning solution was cooled to 40 ° C. in front of the nozzle. Then, dry spinning was carried out from a 720-hole nozzle with a nozzle hole diameter of 0.2 mm.
  • the shaft temperature was 50 ° C
  • the withdrawal speed was 250 m / min and the dwell time of the threads in the spinning shaft was 1.39 seconds. 52.8 ccm / min were conveyed from the spinning pump.
  • the total spin titer was 648 dtex.
  • the residual solvent content in the spun material was 10.8%.
  • the DMF evaporation rate was 0.856
  • the single spin titer was 0.9 dtex.
  • the delay was 107.
  • the threads were again wetted with oil-containing preparation, wound on spools, folded into a cable, stretched 1: 3.6 times in boiling water and aftertreated in the usual way to give fibers with a final titer of 0.3 dtex.
  • the fiber cross sections were again completely uniform and circular.
  • the fibers also had a very high gloss again and showed a smooth surface in the scanning electron microscope with striations that were longitudinally striped parallel to the fiber axis.
  • An acrylonitrile copolymer with the chemical composition from Example 1 was dissolved in DMF as described there.
  • the spinning solution was then filtered, cooled to 90 ° C. and dry-spun from a 720-hole nozzle with a nozzle hole diameter of 0.2 mm.
  • the shaft temperature was 150 ° C, the air temperature 200 ° C and the air volume 40 m 3 / h.
  • the take-off speed was 180 m / min. It was spun on a shorter-sized spinning shaft, so that a residence time of 1.66 sec. revealed.
  • the spinning pump became 82.8 ccm / min. promoted.
  • the total spin titer was 1304 dtex.
  • the residual solvent content in the spinning material was 13.5%.
  • the DMF evaporation rate was 1.225
  • the single spin titer was 1.8 dtex.
  • the warpage was 48.
  • the threads were post-treated with 1: 4, 0-fold stretching to fibers with a final titer of 0.6 dtex.
  • the fibers had a round to slightly bean-shaped cross-sectional profile. Her shine was again extraordinarily high. In the scanning electron microscope, striations and striations running on the surface parallel to the fiber axis were again observed, which showed no interruptions.
  • the single spin titer was 1.81 dtex.
  • the warping was 80.
  • the threads were again wetted with oil-containing preparation, collected on bobbins, folded into a cable, stretched 1: 4.0 times in boiling water and post-treated into fibers in the usual way.
  • the final fiber titer was 0.56 dtex.
  • the fibers show the typical dumbbell shape.
  • part of the batch from Example 5a was cooled to 40 ° C. in front of the nozzle and dry-spun from a 1050-hole nozzle with a nozzle hole diameter of 0.25 mm.
  • the shaft temperature was 190 ° C, the air temperature 380 ° C and the air volume 40 m 3 / h.
  • the take-off speed was 250 m / min and the dwell time of the threads in the spinning shaft was 2.11 seconds. 161 ccm / min were conveyed from the spinning pump.
  • the total spin titer was 1891 dtex.
  • the residual solvent content in the spinning material was 8.8%.
  • the DMF evaporation rate was 1.727
  • the single spin titer was 1.80 dtex.
  • the warpage was 80.
  • the threads were post-treated as described in Example 5a.
  • the final fiber titer was 0.58 dtex.
  • the fibers in turn show the typical dumbbell shape.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Claims (5)

1. Procédé de fabrication de fils et de fibres acryliques à partir de solutions à filer d'une teneur de 25 à 35% en matières solides à base de polymérisats d'acrylonitrile formant des fils avec des motifs unitaires d'actylonitrile d'au moins 85% en poids, dans des solvants organiques polaires, selon un procédé de filage à sec, à une température de gaine, de préférence, entre 30°C et une valeur en dessous du point d'ébullition du solvant de filage utilisé et une température d'air de filage de 300°C au maximum, et en traitant ultérieurement le produit filé d'une manière connue en soi en fils ou fibres finis, caractérisé en ce qu'on utilise des solutions à filer thermiquement prétraitées dont la viscosité se modifie au maximum de 5% pendant la durée du filage; en ce que la solution à filer est filée avec un étirage d'au moins 20 et en ce que des fils d'un titre individuel de 3 décitex et moins sont produits au cours du filage.
2. Procédé selon la revendication 1, caractérisé en ce que du diméthylformamide est utilisé comme solvant de filage.
3. Procédé selon la revendication 1, caractérisé en ce que la solution à filer est filée avec un étirage de 30-500.
4. Fils et fibres acryliques en polymérisats d'acrylonitrile avec des motifs unitaires d'acrylonitrile d'au moins 85% en poids, caractérisés en ce qu'ils sont lisses dans le sens longitudinal; en ce que leur surface présente, parallèlement à l'axe des fibres, des stries et des rayures longitudinales et en ce qu'ils ont un titre individuel de 3 décitex au maximum.
5. Fils et fibres selon la revendication 4, caractérisés en ce qu'ils ont des sections droites rondes allant jusqu'à la forme d'un haricot.
EP80107777A 1979-12-21 1980-12-10 Fibres et filaments synthétiques de titre très fin et procédé de filage à sec pour leur fabrication Expired - Lifetime EP0031078B2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT80107777T ATE20909T1 (de) 1979-12-21 1980-12-10 Feinsttitrige synthesefasern und -faeden und trockenspinnverfahren zu ihrer herstellung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2951803 1979-12-21
DE19792951803 DE2951803A1 (de) 1979-12-21 1979-12-21 Feinsttitrige synthesefasern und -faeden und trockenspinnverfahren zu ihrer herstellung

Publications (4)

Publication Number Publication Date
EP0031078A2 EP0031078A2 (fr) 1981-07-01
EP0031078A3 EP0031078A3 (en) 1983-05-25
EP0031078B1 true EP0031078B1 (fr) 1986-07-23
EP0031078B2 EP0031078B2 (fr) 1992-06-03

Family

ID=6089296

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80107777A Expired - Lifetime EP0031078B2 (fr) 1979-12-21 1980-12-10 Fibres et filaments synthétiques de titre très fin et procédé de filage à sec pour leur fabrication

Country Status (6)

Country Link
US (2) US4400339A (fr)
EP (1) EP0031078B2 (fr)
JP (1) JPS56101909A (fr)
AT (1) ATE20909T1 (fr)
DE (2) DE2951803A1 (fr)
IE (1) IE52101B1 (fr)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3225266A1 (de) * 1982-07-06 1984-01-12 Bayer Ag, 5090 Leverkusen Kontinuierliches trockenspinnverfahren fuer acrylnitrilfaeden und - fasern
DE3225267A1 (de) * 1982-07-06 1984-01-12 Bayer Ag, 5090 Leverkusen Herstellung loesungsmittelarmer polyacrylnitril-spinnfaeden
JPS616160A (ja) * 1984-06-19 1986-01-11 東レ株式会社 繊維補強水硬性物質
DE3424343A1 (de) * 1984-07-03 1986-01-16 Bayer Ag, 5090 Leverkusen Verfahren und vorrichtung zum trockenspinnen
RU2096537C1 (ru) * 1989-06-28 1997-11-20 Мишлэн Решерш Э Текник Монофиламент из ароматического полиамида и способ его получения
US5715804A (en) * 1994-07-29 1998-02-10 Yamaha Corporation Hybrid bow string formed from strands of polyethylene resin and polyparabenzamide/polybenzobisoxazole resin
JPH0842995A (ja) * 1994-07-29 1996-02-16 Yamaha Corp 洋弓用弦
EP1314808B1 (fr) * 1995-11-30 2006-01-04 Kimberly-Clark Worldwide, Inc. Multicouche à base de microfibres très fines
DE19829164A1 (de) 1998-06-30 2000-03-30 Bayer Faser Gmbh Elastanfäden und Verfahren zu ihrer Herstellung
US7175903B1 (en) * 2000-11-17 2007-02-13 Pliant Corporation Heat sealable polyvinyl chloride films
CN109629027B (zh) * 2017-10-09 2021-10-22 中国石油化工股份有限公司 一种干法腈纶1.33dtex短纤维的生产方法
US11180867B2 (en) 2019-03-20 2021-11-23 University Of Kentucky Research Foundation Continuous wet-spinning process for the fabrication of PEDOT:PSS fibers with high electrical conductivity, thermal conductivity and Young's modulus

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE364509A (fr) * 1928-10-29
US1950026A (en) * 1929-07-02 1934-03-06 Celanese Corp Manufacture of artificial filaments or threads
US2072100A (en) * 1929-11-27 1937-03-02 Celanese Corp Spinning of artificial filaments
BE514101A (fr) * 1951-10-09
US3097415A (en) * 1959-02-20 1963-07-16 Acrylonitrile fiber and process for
NL253933A (fr) * 1959-07-18
US3531368A (en) * 1966-01-07 1970-09-29 Toray Industries Synthetic filaments and the like
JPS4711254U (fr) * 1971-03-03 1972-10-11
SE403141B (sv) * 1973-02-05 1978-07-31 American Cyanamid Co Smeltspinningsforfarande for framstellning av en akrylnitrilpolymerfiber
JPS539301A (en) * 1976-07-12 1978-01-27 Mitsubishi Rayon Co Production of leather like sheet structre
DE2657144C2 (de) * 1976-12-16 1982-12-02 Bayer Ag, 5090 Leverkusen Verfahren zur Herstellung hydrophiler Fasern
DE2658916A1 (de) * 1976-12-24 1978-07-06 Bayer Ag Polyacrylnitril-filamentgarne
JPS5394625A (en) * 1977-01-20 1978-08-18 Asahi Chem Ind Co Ltd Production of acrylic fiber
JPS53147818A (en) * 1977-05-26 1978-12-22 Asahi Chem Ind Co Ltd Production of acrylic fiber
JPS602405B2 (ja) * 1977-09-22 1985-01-21 三菱レイヨン株式会社 アクリロニトリル系異繊度単糸混合連続フイラメント糸の製造法
US4205039A (en) * 1977-11-17 1980-05-27 American Cyanamid Company Process for melt-spinning acrylonitrile polymer fiber
US4219523A (en) * 1978-08-30 1980-08-26 American Cyanamid Company Melt-spinning acrylonitrile polymer fiber from low molecular weight polymers
JPS56377A (en) * 1979-06-15 1981-01-06 Teijin Ltd Production of suede like raised fabric

Also Published As

Publication number Publication date
EP0031078A2 (fr) 1981-07-01
EP0031078B2 (fr) 1992-06-03
IE52101B1 (en) 1987-06-24
IE802680L (en) 1981-06-21
DE3071670D1 (en) 1986-08-28
US4497868A (en) 1985-02-05
US4400339A (en) 1983-08-23
JPS56101909A (en) 1981-08-14
DE2951803A1 (de) 1981-07-02
DE2951803C2 (fr) 1989-03-16
JPH0128125B2 (fr) 1989-06-01
ATE20909T1 (de) 1986-08-15
EP0031078A3 (en) 1983-05-25

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