EP1845179B1 - Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern - Google Patents

Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern Download PDF

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Publication number
EP1845179B1
EP1845179B1 EP06007926A EP06007926A EP1845179B1 EP 1845179 B1 EP1845179 B1 EP 1845179B1 EP 06007926 A EP06007926 A EP 06007926A EP 06007926 A EP06007926 A EP 06007926A EP 1845179 B1 EP1845179 B1 EP 1845179B1
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EP
European Patent Office
Prior art keywords
fibres
process according
coaxial conductor
conductor
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.)
Active
Application number
EP06007926A
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German (de)
English (en)
French (fr)
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EP1845179A1 (de
Inventor
Mathias Dr. Kaiser
Rudolf Dr. Emmerich
Ralf Dreher
Lukas Dr. Alberts
Christian Dr. Hunyar
Peter Dr. Elsner
Frank Dr. Henning
Klaus-Dieter Dr. Nauenburg
Bernd Dr. Wohlmann
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.)
Teijin Ltd
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Toho Tenax Co 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 to ES06007926T priority Critical patent/ES2348590T3/es
Application filed by Toho Tenax Co Ltd filed Critical Toho Tenax Co Ltd
Priority to EP06007926A priority patent/EP1845179B1/de
Priority to DE502006007528T priority patent/DE502006007528D1/de
Priority to AT06007926T priority patent/ATE475728T1/de
Priority to AU2007237521A priority patent/AU2007237521B2/en
Priority to JP2009504606A priority patent/JP5191004B2/ja
Priority to CA2649131A priority patent/CA2649131C/en
Priority to US12/226,325 priority patent/US20090277772A1/en
Priority to BRPI0710157A priority patent/BRPI0710157B1/pt
Priority to CN2007800135079A priority patent/CN101421448B/zh
Priority to PCT/EP2007/002909 priority patent/WO2007118596A1/de
Priority to TW096112685A priority patent/TWI372798B/zh
Priority to ARP070101532A priority patent/AR060505A1/es
Publication of EP1845179A1 publication Critical patent/EP1845179A1/de
Application granted granted Critical
Publication of EP1845179B1 publication Critical patent/EP1845179B1/de
Active legal-status Critical Current
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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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/32—Apparatus therefor
    • D01F9/328—Apparatus therefor for manufacturing filaments from polyaddition, polycondensation, or polymerisation products
    • 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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • 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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • D01F9/225—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles from stabilised polyacrylonitriles

Definitions

  • the invention relates to a method for the continuous production of carbon fibers, wherein stabilized precursor fibers are carbonized and graphitized with the aid of high-frequency electromagnetic waves.
  • Stabilized precursor fibers are fibers which have been converted into infusible fibers by methods known per se. Only such infusible fibers are suitable for the subsequent carbonation steps required to produce carbon fibers.
  • Fibers, yarns and strands of stabilized precursor fibers are poor electrical conductors and moderate absorbers of high-frequency electromagnetic Waves such as microwaves. With the irradiation of the high-frequency electromagnetic waves, the transition to complete carbonization and increasing graphitization begins, resulting in a large increase in the electrical conductivity of the treated fibers.
  • the fiber behaves like a wire in the waveguide and leads to strong distortions and disturbances of the electric field in the waveguide or in the resonator arrangement. Without control, inhomogeneities and perturbations occur that affect the homogeneity and process stability of the graphitization, or in extreme cases can lead to the ignition of discharges and arcing or the thermal vaporization of the fiber.
  • the object of the present invention is to provide a simple process for the continuous production of carbon fibers, in which stabilized precursor fibers are carbonized and graphitized with the aid of high-frequency electromagnetic waves, which can be carried out economically and with reasonable outlay in terms of process control.
  • the stabilized precursor fibers are continuously fed as an inner conductor of a coaxial conductor consisting of outer conductor and inner conductor and through a treatment zone, in the treatment zone the stabilized precursor fibers high-frequency electromagnetic waves are supplied, which absorb the Precursorfasern whereby the precursor fibers are heated and converted into carbon fibers, and that the stabilized precursor fibers or the carbon fibers are conducted under a protective gas atmosphere through the coaxial conductor and the treatment zone.
  • the high-frequency electromagnetic waves are preferably microwaves.
  • the decoupling of microwave energy from a rectangular waveguide is for example off DE 10 2004 021 016 A1 known, wherein both the outer conductor and the inner conductor are fixed components of the coaxial conductor.
  • This type of coupling is used to bring microwave energy into hot process spaces, since with the help of coaxial conductors microwave power can be transmitted with high power density.
  • the microwave energy which is supplied from a waveguide, coupled via a suitable device, for example via a coupling cone in the coaxial conductor.
  • a protective gas atmosphere around the stabilized precursor fibers in the outcoupling region and in the coaxial conductor can be maintained in a simple manner, for example, by arranging a tube permeable to the energy of the high-frequency electromagnetic waves or microwaves within the outer conductor of the coaxial conductor and the treatment zone and the stabilized precursor fibers as Inner conductor as well as the protective gas are passed through this tube.
  • the resulting carbon fibers become increasingly more conductive, decoupling the microwave energy more and more into the coaxial junction and preventing further treatment of the carbon fibers.
  • the coupled-out microwave energy already starts the treatment of the stabilized precursor fibers in the coaxial conductor, so that when the stabilized precursor fibers are passed through the coaxial conductor, a self-regulating system is established.
  • the method according to the invention is characterized in that the stabilized precursor fibers are guided through the coaxial conductor at such a speed that they carbonize or graphitise on leaving the coaxial conductor and thus are carbon fibers.
  • pre-carbonated precursor fibers are used to carry out the process according to the invention.
  • stabilized precursor fibers produced very particularly from polyacrylonitrile are particularly suitable for this purpose.
  • gas used is nitrogen.
  • the speed with which the stabilized precursor fibers are guided through the coaxial conductor is controlled by measuring the electrical resistance of the resulting carbon fiber. It has been found that the level of electrical resistance can draw conclusions about the quality of the carbon fibers.
  • precursor fibers which are already precarbonized still have an electrical resistance which is in the region of 30 M ⁇ , while carbon fibers with good properties in terms of strength, elongation and modulus have an electrical resistance which is within the range of a few ⁇ , for example in the range of 10 to 50 ⁇ .
  • the measurement of the electrical resistance is carried out via two copper electrodes, which are arranged on the fibers at a distance of 50 cm.
  • oxygen is added to the protective gas atmosphere.
  • the treatment step of the oxidation which is usually carried out after completion of the carbonization or graphitization, can be carried out in the process according to the invention directly during carbonization.
  • the addition of oxygen can be effected, for example, by the fact that the air contained between the fibers in the supplied precursor fibers is not removed before introduction into the coaxial conductor. But it is also readily possible to supply oxygen in a targeted uniform dosage of the inert gas atmosphere.
  • the process according to the invention can be carried out particularly advantageously when the stabilized precursor fibers are separated by two or more arranged consisting of coaxial conductor and treatment zone reactors are performed.
  • stabilized precursor fibers 1 are guided as an inner conductor 2 through a coaxial conductor with an outer conductor 3.
  • a tube 4 Arranged around the inner conductor 2 and within the outer conductor 3 and inside the resonator 9 is a tube 4 which is permeable to high-frequency electromagnetic waves or microwaves and into which protective gas is injected to produce a protective gas atmosphere.
  • the microwave energy supplied in a waveguide 5 is transmitted via coupling cone 6 (FIG. FIG. 1 ) or via a cavity resonator 9 (FIG. FIG.
  • the microwave supply via a coaxial conductor the inner conductor 11 is T-shaped and electrically conductive, whereby the microwave to the treatment zone 10th is redirected.
  • This inner conductor 11 may for example be tubular.
  • carbon fibers 7 are produced from the stabilized precursor fibers 1.
  • a field distribution of the microwave energy in the form of standing waves in the coaxial conductor is achieved.
  • Further embodiments which are suitable for carrying out the method according to the invention are, for example, in DE 26 16 217 . EP 0 508 867 or WO 00/075 955 described.
  • the stabilized precursor fibers used were stabilized precursor polycarboxylate-precursor fibers, which were precarbonated, which were combined into a strand of 12,000 filaments.
  • a cylindrical resonator For coupling the microwave energy, a cylindrical resonator became similar FIG. 2 used with walls made of aluminum Muegge Electronics GmbH. This has a diameter of 100 mm and is designed to connect rectangular waveguide R 26 type with a microwave generator with a microwave power of 3 kW. The microwave energy generated is decoupled into a coaxial conductor whose outer jacket has an inner diameter of 100 mm.
  • the precarbonated stabilized precursor fibers were passed through the apparatus described above under a protective gas atmosphere using nitrogen, wherein the resulting carbon fibers were withdrawn from the apparatus at different rates.
  • the used Microwave energy was set to 2 kW.
  • the obtained carbon fibers had the following properties off speed tensile strenght module elongation m / h MPa GPa % 50 3200 220 1.4 150 3100 218 1.4 240 3500 217 1.5 420 2700 180 1.4
EP06007926A 2006-04-15 2006-04-15 Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern Active EP1845179B1 (de)

Priority Applications (13)

Application Number Priority Date Filing Date Title
EP06007926A EP1845179B1 (de) 2006-04-15 2006-04-15 Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern
DE502006007528T DE502006007528D1 (de) 2006-04-15 2006-04-15 Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern
AT06007926T ATE475728T1 (de) 2006-04-15 2006-04-15 Verfahren zur kontinuierlichen herstellung von kohlenstofffasern
ES06007926T ES2348590T3 (es) 2006-04-15 2006-04-15 Procedimiento para la producción continua de fibra de carbono.
US12/226,325 US20090277772A1 (en) 2006-04-15 2007-03-31 Process for Continous Production of Carbon Fibres
CA2649131A CA2649131C (en) 2006-04-15 2007-03-31 Process for continuous production of carbon fibres
AU2007237521A AU2007237521B2 (en) 2006-04-15 2007-03-31 Process for continuous production of carbon fibers
BRPI0710157A BRPI0710157B1 (pt) 2006-04-15 2007-03-31 processo para a produção contínua de fibras de carbono
CN2007800135079A CN101421448B (zh) 2006-04-15 2007-03-31 用于连续制造碳纤维的方法
PCT/EP2007/002909 WO2007118596A1 (de) 2006-04-15 2007-03-31 Verfahren zur kontinuierlichen herstellung von kohlenstofffasern
JP2009504606A JP5191004B2 (ja) 2006-04-15 2007-03-31 炭素繊維の連続製造法
TW096112685A TWI372798B (en) 2006-04-15 2007-04-11 Process for continuous production of carbon fibres
ARP070101532A AR060505A1 (es) 2006-04-15 2007-04-11 Proceso para la produccion continua de fibras de carbono

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP06007926A EP1845179B1 (de) 2006-04-15 2006-04-15 Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern

Publications (2)

Publication Number Publication Date
EP1845179A1 EP1845179A1 (de) 2007-10-17
EP1845179B1 true EP1845179B1 (de) 2010-07-28

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EP06007926A Active EP1845179B1 (de) 2006-04-15 2006-04-15 Verfahren zur kontinuierlichen Herstellung von Kohlenstofffasern

Country Status (13)

Country Link
US (1) US20090277772A1 (es)
EP (1) EP1845179B1 (es)
JP (1) JP5191004B2 (es)
CN (1) CN101421448B (es)
AR (1) AR060505A1 (es)
AT (1) ATE475728T1 (es)
AU (1) AU2007237521B2 (es)
BR (1) BRPI0710157B1 (es)
CA (1) CA2649131C (es)
DE (1) DE502006007528D1 (es)
ES (1) ES2348590T3 (es)
TW (1) TWI372798B (es)
WO (1) WO2007118596A1 (es)

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DE102015110777A1 (de) 2015-07-03 2017-01-05 Deutsches Zentrum für Luft- und Raumfahrt e.V. Verfahren und Anlage zur Herstellung von Kohlenstofffasern
WO2023180971A1 (en) * 2022-03-25 2023-09-28 Aspen Aerogels, Inc. Apparatus and method for heating at pyrolytic temperatures using microwave radiation

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RU2416682C1 (ru) 2009-07-28 2011-04-20 Марина Владимировна Соболева Способ стабилизации углеродсодержащего волокна и способ получения углеродного волокна
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TWI384098B (zh) 2009-12-30 2013-02-01 高模數碳纖維及其製造方法
KR101219721B1 (ko) * 2010-12-21 2013-01-08 한국에너지기술연구원 연속식 하이브리드 탄소섬유 제조방법
KR101219724B1 (ko) * 2010-12-21 2013-01-08 한국에너지기술연구원 하이브리드 탄소섬유 제조방법
JP5682714B2 (ja) 2012-11-22 2015-03-11 三菱レイヨン株式会社 炭素繊維束の製造方法
JP6063045B2 (ja) 2013-07-26 2017-01-18 東邦テナックス株式会社 炭素化方法及び炭素繊維の製造方法
CN106460243B (zh) * 2014-03-31 2019-08-06 国立大学法人东京大学 碳纤维制造装置及碳纤维制造方法
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JP6486169B2 (ja) * 2015-03-31 2019-03-20 帝人株式会社 加熱方法、炭素繊維の製造方法及び炭素繊維並びに加熱装置
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JP6151844B1 (ja) 2016-12-26 2017-06-21 弘治 大石橋 マイクロ波加熱装置
JP2018115395A (ja) * 2017-01-16 2018-07-26 永虹先進材料股▲ふん▼有限公司 炭化繊維製造方法
KR102405323B1 (ko) * 2018-07-23 2022-06-07 주식회사 엘지화학 마이크로웨이브를 이용한 탄소 섬유 탄화 장치
CN109594151A (zh) * 2018-12-25 2019-04-09 中国科学院合肥物质科学研究院 一种优化碳纤维石墨化的设备
CN109944057A (zh) * 2019-03-08 2019-06-28 常熟市翔鹰特纤有限公司 一种聚丙烯腈长丝微波致密化装置
CN112301548B (zh) * 2020-10-15 2021-10-29 厦门大学 一种中空珠链结构的纤维膜及其制备方法和制备装置
CN112575412A (zh) * 2020-12-17 2021-03-30 太仓旭云特种纤维科技有限公司 聚丙烯晴短纤维连续碳化方法
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WO2023180971A1 (en) * 2022-03-25 2023-09-28 Aspen Aerogels, Inc. Apparatus and method for heating at pyrolytic temperatures using microwave radiation

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AU2007237521A8 (en) 2008-11-27
AR060505A1 (es) 2008-06-25
AU2007237521B2 (en) 2011-01-20
CN101421448A (zh) 2009-04-29
WO2007118596A1 (de) 2007-10-25
AU2007237521A1 (en) 2007-10-25
CA2649131A1 (en) 2007-10-25
TWI372798B (en) 2012-09-21
ATE475728T1 (de) 2010-08-15
ES2348590T3 (es) 2010-12-09
US20090277772A1 (en) 2009-11-12
BRPI0710157B1 (pt) 2016-12-13
JP2009533562A (ja) 2009-09-17
BRPI0710157A2 (pt) 2011-08-23
DE502006007528D1 (de) 2010-09-09
CN101421448B (zh) 2012-05-23
CA2649131C (en) 2013-03-12
TW200745395A (en) 2007-12-16
EP1845179A1 (de) 2007-10-17

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