KR101538455B1 - Method for Producing Complex Carbonized Fiber - Google Patents

Method for Producing Complex Carbonized Fiber Download PDF

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Publication number
KR101538455B1
KR101538455B1 KR1020140062898A KR20140062898A KR101538455B1 KR 101538455 B1 KR101538455 B1 KR 101538455B1 KR 1020140062898 A KR1020140062898 A KR 1020140062898A KR 20140062898 A KR20140062898 A KR 20140062898A KR 101538455 B1 KR101538455 B1 KR 101538455B1
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South Korea
Prior art keywords
fiber
acrylic
fibers
producing
present
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KR1020140062898A
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Korean (ko)
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유소희
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유소희
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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
    • 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
    • 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
    • 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
    • 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
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/061—Load-responsive characteristics elastic
    • 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
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/063—Load-responsive characteristics high strength

Abstract

The present invention relates to a method for producing a composite carbon fiber, and more particularly, to a method for producing a composite carbon fiber in which glass fiber or metal fiber is added to an acrylic fiber so that tensile force can be improved. A method for producing a composite carbon fiber includes: preparing an acrylic fiber; Mixing the acrylic yarn and glass fiber or metal fiber to form a yarn; And firing and carbonizing the warped material, wherein the glass fiber or metal fiber is 3 to 10 wt% based on the weight of the acrylic fiber.

Description

TECHNICAL FIELD [0001] The present invention relates to a method for producing a composite carbon fiber,

The present invention relates to a method for producing a composite carbon fiber, and more particularly, to a method for producing a composite carbon fiber in which glass fiber or metal fiber is added to an acrylic fiber so that tensile force can be improved.

The fibrous material that carbonizes the inactive groups of organic fibers is called carbon fiber and can be generally light, strong and excellent reinforcement. The carbonized fibers are fired at 200 to 500 ° C according to the decomposition temperature to produce carbon fibers and carbon fibers heat-treated at 800 to 1200 ° C. while the content of the carbon fibers is 90 to 98% And a fiber produced by heat treatment at 2500 to 3000 占 폚.

Carbon fibers can be used as warming, welding protective films or fire extinguishers and can be made from polyvinyl alcohol, polyacrylonitrile or rayon.

Prior art relating to carbonized fibers is disclosed in Japanese Patent Laid-Open No. 1991-0018597, which is an acrylic fiber for producing oxidized fibers and a method for producing the same. The prior art is made of a copolymer obtained by copolymerizing 90 wt% or more of acrylonitrile, an unsaturated ester or vinyl monomer as the elongation improving monomer, and an unsaturated carboxylic acid or a salt thereof as a monomer for improving thermal stability , An acrylic fiber for producing oxidized fibers having a molecular weight distribution width of 1.7 or less, an elongation of 25 to 30% and an orientation degree of 90% or more.

Other prior art related to carbon fibers is disclosed in published patent application No. 2002-0051383

Activated alumina complex activated carbon fibers and a method for producing the same. Said prior art method comprising uniformly dispersing from 0.01 to 50 parts by weight of activated alumina at 100 parts by weight of pitch at a temperature of 20 to 80 DEG C higher than the pitch softening point; Radiating the pitch fiber at a temperature of 5 to 80 DEG C higher than the softening point of the pitch and thermally stabilizing the pitch fiber at 200 to 350 DEG C in an air atmosphere; And activating the thermally stabilized pitch fibers at 700 to 850 ° C for 10 minutes to 10 hours, thereby producing activated alumina complex activated carbon fibers.

The acrylic fiber or the carbon fiber for producing the oxidized fiber disclosed in the prior art has a disadvantage in that the tensile force is weak and the flame-retardant temperature is not high.

The present invention has been made to solve the problems of the prior art and has the following purpose.

Prior Art 1: Published Japanese Patent Application No. 1991-0018597 (published by Hanil Synthetic Fiber Co., Ltd., November 30, 1991) Acrylic fiber for producing oxidized fiber and method for producing the same Prior Art 2: Open Patent No. 2002-0051383 (published by Pohang Institute of Science and Technology, June 29, 2002) Activated alumina complex activated carbon fiber and method for producing the same

It is an object of the present invention to provide a method for producing a composite carbon fiber in which glass fibers and metal fibers are added to acrylic fibers to improve tensile strength.

According to a preferred embodiment of the present invention, a method of producing a composite carbon fiber comprises the steps of: preparing an acrylic yarn; Mixing the acrylic yarn and glass fiber or metal fiber to form a yarn; And firing and carbonizing the warped material, wherein the glass fiber or metal fiber is 3 to 10 wt% based on the weight of the acrylic fiber.

According to another preferred embodiment of the present invention, the metal fiber is made of stainless steel or tungsten.

According to another preferred embodiment of the present invention, the step of calcining and carbonizing further comprises a vermiculite coating or a silica coating processing step.

The manufacturing method according to the present invention has the advantage that the carbonization is performed after the carbonization is performed, thereby simplifying the manufacturing process. In addition, the carbonized fibers produced by the production method according to the present invention have an advantage that the tensile strength is high and the instantaneous flash point is higher than that of known carbonized fibers.

FIG. 1 schematically shows a method for producing a composite carbon fiber according to the present invention.
FIGS. 2A and 2B show test results of the composite carbon fibers produced according to the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the embodiments shown in the accompanying drawings, but the present invention is not limited thereto. In the following description, components having the same reference numerals in different drawings have similar functions, so that they will not be described repeatedly unless necessary for an understanding of the invention, and the known components will be briefly described or omitted. However, It should not be understood as being excluded from the embodiment of Fig.

FIG. 1 schematically shows a method for producing a composite carbon fiber according to the present invention.

A method for producing a composite carbon fiber according to the present invention includes the steps of preparing an acrylic yarn (S11); (S12) mixing the acrylic yarn and the glass fiber or the metal fiber to form a yarn; And sintering and carbonizing the warped material (S13), wherein the glass fiber or metal fiber is 3 to 10 wt% based on the weight of the acrylic fiber.

The carbonized fiber according to the present invention can be used as a heat insulating material, a fire extinguishing material, a welding protective mat, an insulating curtain, a wire tape, a friction material, a heat resistant work cloth or a safety fireproof heat resistant finish.

The acrylic yarn can be prepared from, for example, a copolymer of 85 to 95 wt% acrylonitrile, 6 to 10 wt% of vinyl acetate, and 0.1 to 1.0 wt% of sodium methacrylate sulfonate. Or acrylic acid may be prepared from a copolymer comprising acrylonitrile, methyl or ethyl, methacrylic acid and sulfonic acid, but is not limited thereto and may be prepared by a variety of methods known in the art.

It is advantageous for the acrylic yarn applied to the production method according to the present invention to have a high heat shrinkage stress. For example, an acrylic yarn according to the present invention may have a heat shrinkage stress of 0.10 to 0.25 g / d, a shrinkage of 20 to 30% and a high heat shrinkage of 30 to 40%. The acrylic resin according to the present invention may have Young's modulus of 250 to 350 kg / mm < 2 >. The acrylic yarn according to the present invention may also have a strength of 3.5 to 4.5 g / d.

The method for producing carbonized fibers according to the present invention is used for heat resistance applications such as a heat insulating material or a protective mat, and is mixed with glass fibers or metal fibers. Therefore, it is advantageous to have thermal stability and at the same time have high heat shrinkage stress or high heat shrinkage. However, the manufacturing method according to the present invention is not particularly limited to the type of acrylic yarn since such characteristics can be controlled in the carbonization process.

When the acrylic yarn is prepared (S11), the acrylic yarn can be mixed with the glass fiber or the metal fiber and can be twisted (S12). The glass fiber or the metal fiber may be 3 to 10 wt% based on the acrylic weight, and the glass fiber and the metal fiber may be glass fiber: metal fiber = 100: 30 to 100, for example, .

The glass fiber has the function of improving the heat insulation, the heat resistance and the insulating property, and the metal fiber mainly has the function of improving the strength and at the same time maintaining the shape of the material during the carbonization process or thermal deformation process. When the amount of the glass fiber or metal fiber is less than 3 wt%, the strength is lowered and the heat shrinkage stress is lowered. On the other hand, if the glass fiber or metal fiber is 10 wt% or more, the durability of the carbon fiber may be reduced due to the difference between the strain of the glass fiber or the metal fiber and the strain of the acrylic fiber. In addition, the glass fiber is preferably larger than the metal fiber, and is intended to appropriately maintain the heat insulating property, the heat resistance and the insulating property of the glass fiber.

The glass fibers can be preferably long fibers and can be, for example, S-glass fibers. The S-glass fiber has a smaller specific gravity than other glass fibers and has an advantage of high tensile strength and elasticity. For example, the glass fiber according to the present invention can be a long fiber made from SiO 2 , Al 2 O 3 , CaO, MgO, B 2 O 3 and Na 2 O. The glass fiber may be surface treated and may be surface treated with a thermoplastic resin such as polyethylene, polystyrene, methyl polymethacrylate or polypropylene.

The metal fibers may be stainless steel or tungsten based metal fibers, for example, having a diameter of 25 to 250 μm, a tensile strength of 700 Mpa or more, and a thermal expansion coefficient of 4.5 to 20 × 10 -6 / K . The present invention can be applied to a method for producing complex carbonized fibers according to the present invention having various kinds and physical properties, and the present invention is not limited to the embodiments shown.

The glass fiber or the carbonized fiber can be formed into a hollow shape together with the acrylic yarn (S12) and can have a certain size and width. The forged material can be carbonized to be made of carbon fiber (S13).

The carbonization can be carried out for 30 to 200 minutes in a carbonization chamber having a temperature of, for example, 200 to 500 DEG C while maintaining a pressure close to a vacuum. A gas such as nitrogen or hydrogen that is discharged during the carbonization process may be discharged by a vacuum pump. Carbonization can be achieved in such a way that, for example, a loosely wound material is wound around the rollers and the tension of the other rollers is adjusted so that the loosened material passes through the carbonization chamber. The firing and carbonization can be performed in a multistage manner. For example, pre-firing can be performed based on the softening point of the resin for surface treatment of acrylic yarn. For example, the pre-firing can be carried out at a temperature of 120 to 250 DEG C for 15 to 20 minutes. The pre-carbonized forging material may then be fired and carbonized at a temperature of 200 to 500 DEG C for 30 to 200 minutes to be made into a composite carbon fiber.

The composite carbon fiber may be coated with silica or vermiculite. The silica coating or the vermiculite coating can be processed, for example, in the form of a colloid. Specifically, silica or vermiculite can be made into nanoparticles using emulsifying groups and into colloidal state in alcohol and silane solutions. And polymethamethylcrylate (PMMA) may be dissolved in the solution to impart the adhesive force. The solution may be made into a gel state and the surface of the complex carbonized fiber may be coated using a coater. By such a coating, the insulation, warmth and strength of the composite carbon fiber can be increased.

An embodiment of the manufacturing method according to the present invention will be described below.

Example

Step 1: The acrylic yarn was prepared from a copolymer of 85 to 95 wt% acrylonitrile, 6 to 10 wt% of vinyl acetate and 0.1 to 1.0 wt% of sodium methacrylate sulfonate, and the produced acrylic yarn had a density of 0.15 g / d A shrinkage stress of 23%, a high heat shrinkage of 32%, a Young's modulus of 280 kg / mm < 2 > and a strength of 4.0 g / d.

Step 2: S-glass fibers of 3 wt% and 3 wt% of stainless steel-based metal fibers were mixed together with acrylic yarn by weight of acrylic yarn.

Step 3: The carbonized material was fired and carbonized at 250 DEG C for 80 minutes to produce complex carbonized fibers.

Complex carbonized fibers were prepared in the same manner as in Example 1, except that 2 wt% of S-glass fiber and 4 wt% of stainless steel metal fiber were used.

Carbon fiber was produced in the same manner as in Example 1, except that tungsten-based metal fibers were used.

350 in the same manner as in Example 1, except that the carbonized fibers were calcined and carbonized at a temperature of 350 ° C.

result

The test results of Examples 1 to 4 are shown in Figs. 2A to 2B.

FIG. 2A shows the test results of Examples 1 and 2, and FIG. 2B shows test results of Examples 3 and 4, respectively.

The composite carbon fibers were found to have a density of 1.8 to 2.2 g / cm 3, a strength of 4.75 to 5.85 MPa, an elastic modulus of 105 to 200 MPa, an elongation of 1.3 to 1.5% and a melting point of 1000 to 1800 ° C. And the thermal conductivity was found to be 1.2 × 10 -2 to 2.0 × 10 -2 W / cm.K.

Such physical properties are 20 to 30 times higher in strength and 5 times more in insulation than carbonaceous fibers known in the art.

The manufacturing method according to the present invention has the advantage that the carbonization is performed after the carbonization is performed, thereby simplifying the manufacturing process. In addition, the carbonized fibers produced by the production method according to the present invention have an advantage that the tensile strength is high and the instantaneous flash point is higher than that of known carbonized fibers.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention . The invention is not limited by these variations and modifications, but is limited only by the claims appended hereto.

S11: Acrylic yarn preparation
S12: Reinforced fiber mixed yarn
S13: Firing and carbonization

Claims (3)

Preparing an acrylic yarn;
Mixing the acrylic yarn and glass fiber or metal fiber to form a yarn; And
Subjecting the warped material to firing and carbonization,
Wherein the glass fiber or the metal fiber is 3 to 10 wt% based on the weight of the acrylic fiber. The method of producing a complex carbonized fiber according to claim 1, wherein the metal fiber is of a stainless steel type or a tungsten type. [2] The method of claim 1, wherein the calcining and carbonizing further comprises a vermiculite coating or a silica coating treatment.
KR1020140062898A 2014-05-26 2014-05-26 Method for Producing Complex Carbonized Fiber KR101538455B1 (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08218248A (en) * 1995-02-10 1996-08-27 Nippon Gurasufuaibaa Kogyo Kk Cloth for averting spark for welding and cutting by heating
US20070218346A1 (en) * 2006-03-20 2007-09-20 Chunxin Ji Acrylic fiber bonded carbon fiber paper as gas diffusion media for fuel cell
KR20080097040A (en) * 2007-04-30 2008-11-04 윤주영 Method for manufacturing a buffering fabric and a buffering fabric thereby
KR100923417B1 (en) * 2009-03-19 2009-10-23 제이씨텍(주) Method of preparing carbon narrow fabric

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08218248A (en) * 1995-02-10 1996-08-27 Nippon Gurasufuaibaa Kogyo Kk Cloth for averting spark for welding and cutting by heating
US20070218346A1 (en) * 2006-03-20 2007-09-20 Chunxin Ji Acrylic fiber bonded carbon fiber paper as gas diffusion media for fuel cell
KR20080097040A (en) * 2007-04-30 2008-11-04 윤주영 Method for manufacturing a buffering fabric and a buffering fabric thereby
KR100923417B1 (en) * 2009-03-19 2009-10-23 제이씨텍(주) Method of preparing carbon narrow fabric

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