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WO1997020974A1 - Fibre a base d'ethylene/chlorotrifluoroethylene et procede de preparation - Google Patents

Fibre a base d'ethylene/chlorotrifluoroethylene et procede de preparation Download PDF

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Publication number
WO1997020974A1
WO1997020974A1 PCT/KR1996/000223 KR9600223W WO9720974A1 WO 1997020974 A1 WO1997020974 A1 WO 1997020974A1 KR 9600223 W KR9600223 W KR 9600223W WO 9720974 A1 WO9720974 A1 WO 9720974A1
Authority
WO
WIPO (PCT)
Prior art keywords
ethylene
chlorotrifluoroethylene
fiber
component
polymer
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.)
Ceased
Application number
PCT/KR1996/000223
Other languages
English (en)
Inventor
Kwang-Seok Han
Jin-Ho Yoon
Young-Geun Choi
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.)
SK Discovery Co Ltd
Original Assignee
Sunkyung Industries Ltd
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 KR1019960052567A external-priority patent/KR970043409A/ko
Application filed by Sunkyung Industries Ltd filed Critical Sunkyung Industries Ltd
Publication of WO1997020974A1 publication Critical patent/WO1997020974A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • 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
    • D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/32—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising halogenated hydrocarbons as the major constituent

Definitions

  • the present invention relates, in general, to fiber prepared from ethylene/chlorotrifluoroethylene polymer alone or in combination with different types of polymers a n d , m o r e p a r t i c u l a r l y , t o ethylene/chlorotri luoroethylene fiber applicable for automotive upholstery fabric, medical drapes and gowns, and outwear garments for leisure and sports. Also, the present invention is concerned with a method for preparing the ethylene/chlorotrifluoroethylene fiber.
  • the above objective could be accomplished by a provision of ethylene/chlorotrifluoroethylene fibers prepared from ethylene/chlorotrifluoroethylene copolymer alone or in combination with other polymers, which have a melt flow index (MI) of 50-1,000 g/10 min.
  • MI melt flow index
  • ethylene/chlorotrifluoroethylene fiber means all fiber prepared by spinning ethylene/chlorotrifluoroethylene polymer alone, sheath-core type fiber prepared by spinning a composite in which ethylene/chlorotrifluoroethylene polymer is the sheath component with another polymer of core component, and sea and island type fiber prepared by spinning a composite which comprises ethylene/chlorotrifluoroethylene polymer as the island component and an elutable polymer as the sea component.
  • the ethylene/chlorotrifluoroethylene polymer used in the present invention has preferably a melt flow index of 50-1,000 g/10 min and more preferably 50-500 g/10 min when measuring the amount which flows through a 0.0825 inch orifice for 10 min at 275°C under a load of 2,160 g according to ASTM D-1238.
  • a melt flow index 50-1,000 g/10 min and more preferably 50-500 g/10 min when measuring the amount which flows through a 0.0825 inch orifice for 10 min at 275°C under a load of 2,160 g according to ASTM D-1238.
  • the ethylene/chlorotrifluoroethylene polymer has an MI less than 50 g/10 min, yarn breakage occurs under the spinneret and thus, it is impossible to take up the yarn.
  • the MI exceeds 1,000 g/10 min, the physical properties proper to fiber cannot be obtained.
  • the ethylene/chlorotrifluoroethylene fiber of the present invention is of the sheath-core type in which the ethylene/chlorotrifluoroethylene polymer is used as the sheath component while using a different type of polymer as the core component
  • preferred examples of the different type of polymer include polyesters, polyamides and polyolefins.
  • This composite fiber is advantageous in that the production cost is low while maintaining the e x c e l l e n t p r o p e r t i e s o f t h e ethylene/chlorotrifluoroethylene.
  • Sheath-core type fiber consists of a core component positioned at the center and a sheath component surrounding the core part.
  • the core component has an area of 30-70 % with the sheath component correspondingly ranging from 30 to 70 % in area. Within this range, good processability and characteristics of ethylene/chlorotrifluoroethylene can be accomplished. For example, if the sheath component is below 30 %, that is, the core component exceeds 70 %, the core component is biased toward one side, being laid bare, or microscopic cracks are generated on the surface of composite fiber, deleteriously affecting chemical resistance. On the other hand, the sheath component is above 70 %, that is, the core component is below 30 %, the effect of reducing production cost is not so large.
  • a s a f o r e m e n t i o n e d , t h e ethylene/chlorotrifluoroethylene fiber of the present invention may be of the sea and island type in which the ethylene/chlorotrifluoroethylene polymer is used as the island component with an elutable polymer as the sea component.
  • the preferred examples of the elutable polymer include polyesters, polyamides and polyolefins.
  • the island component is used at an amount of 60-80 % by weight with the amount of the sea component ranging correspondingly from 20-40 % by weight. The less the amount of the sea component is, the better. However, if the sea component is below 20 % by weight, the islands adhere to each other. On the other hand, if the island component is above 40 % by weight, it is economically unfavorable.
  • the sea and island type fiber according to the present invention may be treated with a suitable solvent in an ordinary elution process to give ultrafine ethylene/chlorotrifluoroethylene fiber with a size of about 0.01-0.1 denier.
  • This ultrafine fiber may be prepared into filaments for textile and knitwear or into staple fibers for suede. These products show good performance in water repellence, oil repellence and chemical resistance.
  • the fiber of the present i nven tion i s prepared by spi nning ethylene/chlorotrifluoroethylene polymer with an MI of 50- 1,000 g/10 min, alone or in combination with a different type of polymer.
  • the spinning is carried out preferably at a speed of 400-1,300 m/min and at a temperature of 280- 320°C and more preferably 290-310°C.
  • the spinning temperature is lower than 280°C, the resulting fiber is poor in the take-up process and drawability.
  • the spinning is performed at a temperature higher than 320°C, it is highly likely to deteriorate the fiber.
  • Spinning speed higher than 1,300 m/min leads to a decrease in drawability.
  • As-spun fiber is preferably drawn at the draw ratio ranging from 1.8 to 3.5. For example, if the draw ratio is less than 1.8, the resulting fiber is poor in strength. On the other hand, if the draw ratio exceeds 3.5, fibrils are generated, making it difficult to carrying out the drawing process.
  • the drawing temperature and the thermal treatment temperature are preferably controlled at 40-
  • the ethylene/chlorotrifluoroethylene fiber prepared as above-illustrated processes can be weaved and therefore, applied for automotive upholstery fabric, medical drapes and gowns, and out wear garments for leisure and sports requiring chemical resistance, flame resistance, anti-contamination, and water repellence.
  • a better understanding of the present invention may be obtained in light of following examples which are set forth to illustrate, but are not to be construed to limit, the present invention.
  • Undrawn fiber of 190 denier was prepared by spinning ethylene/chlorotrifluoroethylene polymer having an MI of 75 through a 24-hole spinneret with a diameter of 0.1 mm at 300°C at a spinning speed of 700 m/min in an output rate of 15 g/min in a screw extruder. As-spun fiber was drawn at a draw ration of 2.5 at a drawing temperature of 80°C and at a thermal treatment temperature of 130°C to give 75D/24F fiber. This ethylene/chlorotrifluoroethylene fiber was tested for strength and elongation and the results are given as shown in Table 1 below.
  • Example I-l The same procedure as Example I-l, except for using ethylene/chlorotrifluoroethylene polymer with an MI of 52 at a spinning temperature of 310°C, was repeated.
  • Example I-l The same procedure as Example I-l was repeated, except that ethylene/chlorotrifluoroethylene polymer with an MI of 130 was used at a spinning temperature of 310°C at a spinning speed of 1,200 m/min and the draw ratio was
  • Example I-l The same procedure as Example I-l was repeated, except that the spinning temperature was 270°C. Yarn breakage was occurred, and it was impossible to take-up.
  • Spinning was carried out in a similar manner to that of Example 1-2, except that the winding speed was 1,500 m/min. Just below the spinneret, yarn breakage was occurred, and it was impossible to take-up.
  • ethylene/chlorotrifluoroethylene polymer was spun at a head temperature of 300°C through an ordinary sheath-core spinneret. Then, it was drawn at a draw ratio of 2.0 at a speed of 400 m/min using an ordinary drawing machine in which the heat roller and the heat plate were heated at a temperature of 90°C and 190°C, respectively.
  • Oxygen index was measured according to ASTM D-2863.
  • sheath-core fiber of 150 denier/36 filament in which the cross sectional area ratio of the sheath component to the core component was 50:50 was prepared.
  • the sheath-core fiber was tested for chemical resistance and flame resistance and the results are given as shown in Table 2 below.
  • sheath-core fiber of 150 denier/36 filament in which the cross sectional area ratio of the sheath component to the core component was 50:50 was prepared.
  • the sheath-core fiber was tested for chemical resistance and flame resistance and the results are given as shown in Table 2 below.
  • sheath-core fiber of 150 denier/36 filament in which the cross sectional area ratio of the sheath component to the core component was 20:80 was prepared.
  • the sheath-core fiber was tested for chemical resistance and flame resistance and the results are given as shown in Table 2 below.
  • sheath-core fiber of 150 denier/36 filament in which the cross sectional area ratio of the sheath component to the core component was 20:80 was prepared.
  • the sheath-core fiber was tested for chemical resistance and flame resistance and the results are given as shown in Table 2 below.
  • fiber of 150 denier/36 filament was prepared from polyester with an intrinsic viscosity of 0.63. The fiber was tested for
  • fiber of 150 denier/36 filament was prepared from nylon showing a
  • undrown fiber which consists of 24 island monofilaments and sea component was obtained by spinning at a temperature of 305"C through an ordinary sea and island type spinning spinneret in a screw extruder.
  • As-spun fiber was drawn at a draw ratio of 2.8 at a draw temperature of 92°C and a thermal treatment temperature of 185°C in an ordinary drawing machine to give fiber of 75D/36F having a strength of 3.28 g/d and an elongation of 26%.
  • This drawn fiber was knitted by circular knitting machine and then, treated in 2% NaOH solution at 100°C for 30 min to elute the sea component, which led to a fine yarn only consisted of the island component.
  • U s i ng a s a n is l a nd co mp on en t ethylene/chlorotrifluoroethylene with an MI of 75 (measured at 275°C under a load of 2,160 g according to ASTM . D-1238) and as a core component polyester with an intrinsic viscosity of 0.63 and an MI of 95, sea and island fiber in which the ratio of the island component to the sea component was 30/70 was prepared. The processability of spinning and drawing was good. After elution of the sea component, the island component had a maximal fineness of 0.036 denier.
  • sea and island fiber in which the ratio of the island component to the sea component was 80/20 was prepared.
  • the fiber obtained was good in spinnability and drawability.
  • the island component After elution of the sea component, the island component had a maximal fineness of 0.07 denier.
  • Example III-l The same procedure as that of Example III-l was repeated, except for the ratio of the island component to the sea component was 90/10.
  • the formation of cross section was poor because the island components adhered to each other. Spinnability and drawability was also poor.
  • Example III-l The same procedure as that of Example III-l was repeated, except for the ratio of the island component to the sea component was 10/90. Performance in fiber forma . tion was good. However, it was economically unfavorable because the sea component to be removed at an eluting process was too much.
  • the fiber of Examples III-l and III-2 and Comparative Examples III-l and III-2 was compared from a point of view of performance in fiber formation and cross section and the results are given as shown in Table 3 below.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Multicomponent Fibers (AREA)

Abstract

L'invention a trait à une fibre à base d'éthylène/chlorotrifluoroéthylène préparée par une mise en rotation d'éthylène/chlorotrifluoroéthylène à indice de fluage compris entre 50 et 1 000 g/10 min., seul ou en association avec un type différent de polymère. Il est possible de transformer cette fibre en fibres à multifilaments dont les caractéristiques satisfont aux exigences en matière de tissage et qui, partant, se prêtent à des applications telles que la production de tissus de capitonnage de voitures, d'étoffes et de blouses à usage médical ainsi que de vêtements d'extérieur pour les loisirs et le sport.
PCT/KR1996/000223 1995-12-02 1996-11-30 Fibre a base d'ethylene/chlorotrifluoroethylene et procede de preparation Ceased WO1997020974A1 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
KR1995/46206 1995-12-02
KR19950046206 1995-12-02
KR1995/49236 1995-12-13
KR19950049236 1995-12-13
KR19950051267 1995-12-18
KR1995/51267 1995-12-18
KR1019960052567A KR970043409A (ko) 1995-12-02 1996-11-07 에틸렌/클로로트플루오르에틸렌 섬유 및 그 제조방법
KR1996/52567 1996-11-07

Publications (1)

Publication Number Publication Date
WO1997020974A1 true WO1997020974A1 (fr) 1997-06-12

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR1996/000223 Ceased WO1997020974A1 (fr) 1995-12-02 1996-11-30 Fibre a base d'ethylene/chlorotrifluoroethylene et procede de preparation

Country Status (1)

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WO (1) WO1997020974A1 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000042244A1 (fr) * 1998-12-30 2000-07-20 Solutia Inc. Fibres a energie superficielle faible
US6174601B1 (en) 1997-09-12 2001-01-16 Ausimont Usa, Inc. Bicomponent fibers in a sheath-core structure comprising fluoropolymers and methods of making and using same
US6287689B1 (en) 1999-12-28 2001-09-11 Solutia Inc. Low surface energy fibers
US6316103B1 (en) 1996-09-13 2001-11-13 Ausimont Usa, Inc. Bicomponent fibers in a sheath-core structure comprising fluoropolymers and methods of making and using same
US6630087B1 (en) 2001-11-16 2003-10-07 Solutia Inc. Process of making low surface energy fibers
CN112480296A (zh) * 2019-09-12 2021-03-12 浙江省化工研究院有限公司 一种亲水改性的乙烯-三氟氯乙烯共聚物、其制备方法及应用
CN114618233A (zh) * 2020-12-14 2022-06-14 浙江省化工研究院有限公司 一种ectfe熔喷过滤材料及其制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995012014A1 (fr) * 1993-10-25 1995-05-04 Exxon Chemical Patents Inc. Soufflage a l'etat fondu de copolymeres d'ethylene et d'ethylene fluore
US5422159A (en) * 1994-12-08 1995-06-06 Ausimont U.S.A., Inc. Fluorpolymer sheets formed from hydroentangled fibers

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995012014A1 (fr) * 1993-10-25 1995-05-04 Exxon Chemical Patents Inc. Soufflage a l'etat fondu de copolymeres d'ethylene et d'ethylene fluore
US5422159A (en) * 1994-12-08 1995-06-06 Ausimont U.S.A., Inc. Fluorpolymer sheets formed from hydroentangled fibers

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6316103B1 (en) 1996-09-13 2001-11-13 Ausimont Usa, Inc. Bicomponent fibers in a sheath-core structure comprising fluoropolymers and methods of making and using same
US6174601B1 (en) 1997-09-12 2001-01-16 Ausimont Usa, Inc. Bicomponent fibers in a sheath-core structure comprising fluoropolymers and methods of making and using same
WO2000042244A1 (fr) * 1998-12-30 2000-07-20 Solutia Inc. Fibres a energie superficielle faible
US6287689B1 (en) 1999-12-28 2001-09-11 Solutia Inc. Low surface energy fibers
US6630087B1 (en) 2001-11-16 2003-10-07 Solutia Inc. Process of making low surface energy fibers
CN112480296A (zh) * 2019-09-12 2021-03-12 浙江省化工研究院有限公司 一种亲水改性的乙烯-三氟氯乙烯共聚物、其制备方法及应用
CN112480296B (zh) * 2019-09-12 2023-10-27 浙江省化工研究院有限公司 一种亲水改性的乙烯-三氟氯乙烯共聚物、其制备方法及应用
CN114618233A (zh) * 2020-12-14 2022-06-14 浙江省化工研究院有限公司 一种ectfe熔喷过滤材料及其制备方法

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