US20200332444A1 - Carbon fiber formed from chlorinated polyvinyl chloride, and method for preparing same - Google Patents

Carbon fiber formed from chlorinated polyvinyl chloride, and method for preparing same Download PDF

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Publication number
US20200332444A1
US20200332444A1 US16/757,042 US201916757042A US2020332444A1 US 20200332444 A1 US20200332444 A1 US 20200332444A1 US 201916757042 A US201916757042 A US 201916757042A US 2020332444 A1 US2020332444 A1 US 2020332444A1
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Prior art keywords
fiber
polyvinyl chloride
chlorinated polyvinyl
carbon fiber
cpvc
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Sung Ho Yoon
Seong Hwa Hong
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YUSUNG TELECOM Co Ltd
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YUSUNG TELECOM Co Ltd
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Assigned to YUSUNG TELECOM CO., LTD. reassignment YUSUNG TELECOM CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HONG, SEONG HWA, YOON, SUNG HO
Publication of US20200332444A1 publication Critical patent/US20200332444A1/en
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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
    • 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
    • D01F6/08—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 halogenated hydrocarbons
    • 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
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02—Heat treatment
    • 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
    • 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
    • D01D5/12—Stretch-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
    • 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
    • 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
    • D01F6/08—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 halogenated hydrocarbons
    • D01F6/10—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 halogenated hydrocarbons from polyvinyl chloride or polyvinylidene chloride
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/10—Inorganic fibres based on non-oxides other than metals
    • D10B2101/12—Carbon; Pitch

Definitions

  • the present invention relates to a carbon fiber formed from chlorinated polyvinyl chloride and a method for preparing the same, and more particularly to a carbon fiber obtained by carbonizing chlorinated polyvinyl chloride as a starting material, and a method for preparing the same.
  • Carbon fiber is very valuably used as a reinforcing fiber for composite materials in general industrial applications such as automobiles, civil engineering, construction, pressure vessels, windmill blades, etc., as well as high-tech industry fields such as sports, aviation, aerospace. etc.
  • a carbon fiber using polyacrylonitrile (PAN), pitch and cellulose as a precursor is prepared by spinning the precursor to obtain a fiber for a carbon fiber precursor, heating the resultant fiber under an oxidative atmosphere, carrying out an oxidative stabilization process to convert the fiber into an anti-flammable fiber so as to prevent a fiber shape from being deformed and destroyed in a further process of carbonization and graphitization, and heating the anti-flammable fiber under an inert atmosphere to carry out a carbonization and graphitization process.
  • PAN polyacrylonitrile
  • the oxidative stabilization process described for the preparation of a carbon fiber carries out oxidation over a long period of time in order to express the strength of the prepared carbon fiber.
  • oxidation is performed for a long time in a relatively high elongation state, which is known a main reason for longer preparation and costs.
  • an oxygen functional group and crosslink applied to this oxidation process can cause defects on the surface and inside of the carbon fiber generated during a carbonization and graphitization process, thus inhibiting the final crystallinity and physical properties of the carbon fiber.
  • a technical object of the present invention is to provide a carbon fiber with excellent mechanical properties and a method for preparing the carbon fiber by using chlorinated polyvinyl chloride without a stabilization process by oxidation.
  • the present invention provides,
  • a carbon fiber that has an average fiber diameter of 1 to 100 ⁇ m and is obtained by spinning a solution of chlorinated polyvinyl chloride to obtain a chlorinated polyvinyl chloride fiber, elongating the chlorinated polyvinyl chloride fiber without an oxidative stabilization process, and preheating and carbonizing the elongated polyvinyl chloride fiber.
  • the average fiber diameter may be 10 to 20 ⁇ m
  • tensile strength may be 1000 to 2500 MPa
  • tensile modulus may be 70 to 140 GPa.
  • a method for preparing a carbon fiber that has an average fiber diameter of 1 to 100 ⁇ m including: spinning a solution of chlorinated polyvinyl chloride (CPVC) to obtain a chlorinated polyvinyl chloride fiber;
  • CPVC chlorinated polyvinyl chloride
  • FIG. 1 is a view showing the results of thermogravimetric analysis on polyvinyl chloride (PVC) and chlorinated polyvinyl chloride (CPVC).
  • FIG. 2 is a view showing the results of thermogravimetric analysis on a CPVC fiber obtained by spinning a solution according to Example 1.
  • FIG. 3 is a view showing a 13 C-NMR spectrum of intermediate products, in which polyvinyl chloride (PVC), chlorinated polyvinyl chloride (CPVC) and CPVC fiber are carbonized at 200° C., 400° C. and 1000° C.
  • PVC polyvinyl chloride
  • CPVC chlorinated polyvinyl chloride
  • CPVC fiber carbonized at 200° C., 400° C. and 1000° C.
  • FIGS. 4 and 5 are views showing the results of scanning electron microscopic analysis on a carbon fiber obtained according to Example 1 and a carbon fiber obtained according to Comparative Example 1, respectively.
  • a method for preparing a carbon fiber having an average fiber diameter of 1 to 100 ⁇ m including: spinning a solution of chlorinated polyvinyl chloride (CPVC) to obtain a chlorinated polyvinyl chloride fiber; elongating the chlorinated polyvinyl chloride fiber without an oxidative stabilization process to prepare an elongated chlorinated polyvinyl chloride fiber; preheating the elongated chlorinated polyvinyl chloride fiber at 150 to 450° C. under an inert gas atmosphere; and carbonizing the preheated product at 950 to 2000° C.
  • CPVC chlorinated polyvinyl chloride
  • a composition for solution spinning may be prepared first by adding and mixing chlorinated polyvinyl chloride in at least one solvent selected from N,N-dimethylformamide (DMF), dimethylacetamide (DMAc), tetrahydrofuran (THF), nitric acid, sulfuric acid, dimethyl sulfoxide and dioxane.
  • Solution spinning may be performed by using the composition for solution spinning obtained as above.
  • a content of chlorinated polyvinyl chloride may be 1 to 90 wt %, preferably 10 to 50 wt %, and more preferably 20 to 35 wt %.
  • a viscosity of the composition for solution spinning may be about 10 cP to about 100,000 cP. In this case, a conventional device used for solution spinning may be used.
  • chlorinated polyvinyl chloride which is known as a flame retardant, may be used as a carbon fiber precursor and may go through sequential processes of elongating the CPVC fiber obtained by spinning a solution of CPVC without an oxidative stabilization process, and preheating and carbonizing the elongated polyvinyl chloride fiber.
  • a fibrous form may be maintained during heat treatment at a high temperature for carbonization just by preheating the CPVC fiber without an oxidative stabilization process as described above.
  • the carbon fiber obtained according to the preparation method of the present invention may have a clean surface without any defects on the surface and inside thereof by oxidation and may be an isotropic carbon fiber, but having a high degree of fiber axis orientation of graphite crystallites similar to that of a PAN-based carbon fiber.
  • the carbon fiber may show not only mechanical properties such as relatively high strength, elastic modulus and the like, but also less preparation costs and preparation time compared to a conventional carbon fiber.
  • the properties and the like of the CPVC which is a starting material, need to be controlled and a process of elongating the CPVC fiber needs to be adjusted before the preheating.
  • a content of chlorine may be 57.7 to 84.5 wt %, for example, 63 to 68 wt % and an average degree of polymerization may be 400 to 800, for example, 600 to 700.
  • the fluidity of chlorinated polyvinyl chloride may be 0.005 cc/sec or more, for example, 0.007 to 0.05 cc/sec.
  • the average degree of polymerization of CPVC was obtained by dissolving 200 g of resin in 50 ml of nitrobenzene, measuring a specific viscosity of the resultant polymer solution in a 30° C. constant-temperature bath by using an Ubbelohde viscometer, and calculating the resultant specific viscosity according to JIS-K6720-2.
  • An average fiber diameter of the solution-spun chlorinated polyvinyl chloride fiber may be in a range of 30 to 100 ⁇ m, for example, 35 to 55 ⁇ m.
  • the average fiber diameter of the solution-spun chlorinated polyvinyl chloride fiber is in the range described above, it is possible to obtain a carbon fiber having a desired elongation rate and excellent mechanical properties without a partial destruction of a fibrous form in subsequent processes.
  • the solution-spun chlorinated polyvinyl chloride fiber may be elongated in air at a temperature of 120 to 150° C., for example, 130 to 140° C.
  • an elongation rate is not particularly limited, but the elongation may be performed within a range in which the solution-spun chlorinated polyvinyl chloride fiber is not cut.
  • the elongation may be performed in such a way that the elongation rate of the solution-spun chlorinated polyvinyl chloride fiber may be 0.01 to 200%, for example, 100 to 200%, for example, 150 to 200% at a temperature of 120 to 150° C., for example, 130 to 140° C. in air.
  • a chlorinated polyvinyl chloride fiber with an improved tensile strength by controlling an average fiber diameter to be within a desired range, and it is also possible to prepare a carbon fiber that has a smooth surface without defects, etc. in a finally obtained carbon fiber or without a partial destruction of a fibrous form during a carbonization process and has excellent mechanical properties such as tensile strength and elastic modulus.
  • the preheating of the elongated chlorinated polyvinyl chloride fiber may be performed at 150 to 450° C., for example, 300 to 450° C. under an inert gas atmosphere. Then, the preheated product may be carbonized.
  • the carbonizing refers to a process of heat-treating the preheated carbon fiber at a high temperature of 950 to 2000° C., for example, 950 to 1100° C.
  • This carbonization process may be performed under an inert gas atmosphere such as nitrogen, argon, etc.
  • a heating rate may be 1 to 5° C./min and a preheating time may be variable depending on a preheating temperature, which may be, for example, 0.1 to 3 hours.
  • a heating rate may be 1 to 50° C./min and a time for heat treatment at a high temperature may vary depending a temperature for the heat treatment, but may be, for example, in a range of 0.1 to 3 hours.
  • an elongation process may be performed in such a way that an elongation rate may be 0.1 to 5.0% in a carbonization process.
  • the method for preparing a carbon fiber of the present invention may be fine to omit an oxidative stabilization process compared to the case of using other carbon fiber precursors.
  • a preparation process may become simple and preparation costs and time may be reduced with a high yield.
  • a carbon fiber that has an average fiber diameter of 1 to 100 ⁇ m and is obtained by spinning a solution of chlorinated polyvinyl chloride to obtain a chlorinated polyvinyl chloride fiber, elongating the chlorinated polyvinyl chloride fiber without an oxidative stabilization process, and preheating and carbonizing the elongated polyvinyl chloride fiber.
  • the carbon fiber may be obtained according to the method for preparing a carbon fiber as described above.
  • An average fiber diameter of the carbon fiber may be 1 to 100 ⁇ m, for example, 10 to 20 ⁇ m.
  • the carbon fiber may not only have very excellent mechanical properties with a tensile strength of 1000 to 2500 MPa and a tensile modulus of 70 to 140 GPa, but also have a high degree of crystallinity and a high degree of fiber axis orientation of carbon or graphite crystallites in the range of 60 to 80% with regard to the fiber axis.
  • CPVC H-17 grade, degree of polymerization (DP, JIS K 6720-2): 750 ⁇ 50 and content of chlorine: 63 wt %, Hanhwa Chemical Co. Ltd.
  • DP degree of polymerization
  • N,N-dimethylformamide a mixed solvent of tetrahydrofuran and N,N-dimethylformamide at a volume ratio of 1:1 so as to prepare 30 wt % of a carbon fiber precursor solution.
  • the carbon fiber precursor solution was subjected to wet solution spinning in acetone and vacuum-dried at 120° C. so as to obtain a CPVC fiber having an average fiber diameter of about 51 ⁇ m.
  • the CPVC fiber having an average fiber diameter of about 51 ⁇ m was elongated 150% at 140° C. to obtain the CPVC fiber having an average fiber diameter of 42 ⁇ m, after which a preheating process was performed under a nitrogen atmosphere by raising a temperature up to 450° C. at a heating rate of 3° C./min and heat-treating the elongated CPVC fiber for 30 minutes. Then, the resultant product, which underwent the preheating process, was subjected to carbonization by raising a temperature up to 1000° C.
  • the carbon fiber prepared as above had an average fiber diameter of 16.2 ⁇ m.
  • the average fiber diameter of the carbon fiber was measured by using a laser measuring instrument (M550A; Anritsu Devices Co. Ltd.).
  • a carbon fiber was prepared according to the same method as shown in Example 1 with an exception of changing an elongation rate of the CPVC fiber into 200% in the process of elongating the CPVC fiber having an average fiber diameter of about 51 ⁇ m.
  • An average fiber diameter of the carbon fiber prepared according to Example 2 was about 14.1 ⁇ m.
  • a carbon fiber was prepared according to the same method as shown in Example 1 with an exception of using CPVC having a chlorine content of about 69 wt %.
  • a carbon fiber was prepared according to the same method as shown in Example 1 with an exception of changing an average degree of polymerization of CPVC into 400 to 500.
  • a carbon fiber was prepared according to the same method as shown in Example 1 with an exception of carrying out a preheating process under a nitrogen atmosphere by raising a temperature up to 300° C. at a heating rate of 3° C./min and heat-treating for 30 minutes.
  • a carbon fiber was prepared according to the same method as shown in Example 1 with an exception of carrying out an elongation process of the CPVC fiber having an average fiber diameter of about 51 ⁇ m at 120° C. and 150° C. respectively.
  • a carbon fiber was prepared according to the same method as shown in Example 1 with an exception of omitting the elongation process of the CPVC fiber having an average fiber diameter of about 51 ⁇ m.
  • An average fiber diameter of the carbon fiber prepared according to Comparative Example 1 was about 21 ⁇ m.
  • thermogravimetric analysis was performed on polyvinyl chloride (PVC) and chlorinated polyvinyl chloride (CPVC).
  • the thermogravimetric analysis was performed under an nitrogen atmosphere by using TGA 6300; (EXSTAR SII, SEIKO Co. Ltd., Japan) under the condition that a temperature was raised from 25° C. to 1000° C. (heating rate: 5° C./min) and nitrogen was supplied at about 200 mL/min.
  • the results of the thermogravimetric analysis were shown in FIG. 1 .
  • CPVC was decomposed at 250 to 330° C. through dehydrochlorination to form polyene-type molecules, and was subjected(?) to a solid state carbonization process in a temperature range of 310 to 650° C. so as to form a 3 D crosslinked and polycondensed aromatic compound. And it could be understood that the resultant compound is finally converted into a carbon material through heat-treatment at 650° C. or more.
  • thermogravimetric analysis was performed on the CPVC fiber obtained by spinning a solution according to Example 1.
  • the thermogravimetric analysis was performed by using TGA 6300; (EXSTAR SII, SEIKO Co. Ltd., Japan) under the condition that a temperature was raised from 25 to 350° C. (heating rate: 3° C./min and 5° C./min) and air was supplied at about 100 mL/min.
  • the results of the thermogravimetric analysis were shown in FIG. 2 .
  • 13 C-NMR analysis was performed on carbonized intermediate products in which chlorinated polyvinyl chloride (CPVC) and the CPVC fiber were carbonized at 1000° C.
  • 13 C-NMR was performed by using ECA400 (JEOL Co. Ltd.) and the results thereof are shown in FIG. 3 . From this analysis, it is possible to understand a molecular structure and a carbonization yield of the intermediate products in which PVC, CPVC and CPVC fiber were heat-treated at 200° C., 300° C., 400° C. and 1000° C. under a nitrogen atmosphere.
  • a scanning electron microscope (SEM) analysis was performed on the carbon fiber obtained according to Example 1 and the carbon fiber obtained according to Comparative Example 1.
  • the SEM analysis was performed at an accelerated voltage of about 10 kV by using 6400F (JEOL Co. Ltd., Japan).
  • the results of SEM analysis on the CPVC fiber obtained by spinning the solution according to Example 1 and the carbon fiber obtained according to Comparative Example 1 are the same as shown in FIGS. 4 and 5 , respectively.
  • the carbon fiber obtained according to Example 1 has a very even surface in a very smooth state with almost no defects compared to the carbon fiber obtained according to Comparative Example 1.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Fibers (AREA)
US16/757,042 2018-08-13 2019-08-06 Carbon fiber formed from chlorinated polyvinyl chloride, and method for preparing same Abandoned US20200332444A1 (en)

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KR1020180094556A KR102022914B1 (ko) 2018-08-13 2018-08-13 염소화 폴리염화비닐로부터 형성된 탄소섬유 및 그 제조방법
KR10-2018-0094556 2018-08-13
PCT/KR2019/009764 WO2020036356A1 (ko) 2018-08-13 2019-08-06 염소화 폴리염화비닐로부터 형성된 탄소섬유 및 그 제조방법

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KR102111089B1 (ko) * 2018-11-19 2020-05-15 영남대학교 산학협력단 저가 탄소 섬유, 저가 탄소 섬유용 전구체 섬유 및 그 제조 방법
KR102202362B1 (ko) * 2019-11-22 2021-01-13 영남대학교 산학협력단 기계적 특성이 우수한 저가형 탄소섬유 및 이의 제조방법

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JPS5620616A (en) * 1979-07-23 1981-02-26 Nippon Carbon Co Ltd Production of carbon fiber
KR100529004B1 (ko) * 2003-09-23 2005-11-15 (주)우노파이버 폴리비닐클로라이드 섬유 및 그 제조방법
KR100603022B1 (ko) * 2005-03-29 2006-07-24 한국과학기술연구원 할로겐화 고분자로부터 제조된 다공성 초극세 탄소섬유 및그 제조방법
KR100702156B1 (ko) * 2005-12-14 2007-04-02 한국과학기술연구원 초극세 다공성 흑연성 탄소섬유 및 그 제조방법
CN102505188B (zh) * 2011-11-10 2013-07-10 中国科学院宁波材料技术与工程研究所 一种以聚偏氯乙烯为基体制备活性碳纤维的方法
TWI589741B (zh) * 2012-01-23 2017-07-01 茵芬提亞公司 穩定木質素纖維以進一步轉換成碳纖維之方法
KR101407236B1 (ko) * 2012-05-23 2014-06-13 전남대학교산학협력단 그래핀 함유 흑연나노섬유 및 그 제조방법, 이를 포함하는 리튬이차전지의 전극물질
JP2015232193A (ja) * 2014-06-11 2015-12-24 国立大学法人群馬大学 カーボンファイバー前駆体の製造方法、カーボンファイバー前駆体、カーボンファイバーの製造方法
US20170275786A1 (en) * 2014-10-08 2017-09-28 Georgia Tech Research Corporation High strength and high modulus carbon fibers

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WO2020036356A1 (ko) 2020-02-20
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