KR20150134761A - Method of manufacturing polyacrylonitrile type precursor fiber for carbon fiber and polyacrylonitrile type precursor fiber manufactured thereby - Google Patents
Method of manufacturing polyacrylonitrile type precursor fiber for carbon fiber and polyacrylonitrile type precursor fiber manufactured thereby Download PDFInfo
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- KR20150134761A KR20150134761A KR1020140061970A KR20140061970A KR20150134761A KR 20150134761 A KR20150134761 A KR 20150134761A KR 1020140061970 A KR1020140061970 A KR 1020140061970A KR 20140061970 A KR20140061970 A KR 20140061970A KR 20150134761 A KR20150134761 A KR 20150134761A
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- Prior art keywords
- polyacrylonitrile
- carbon fiber
- fiber
- precursor fiber
- acrylonitrile
- Prior art date
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- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 69
- 239000000835 fiber Substances 0.000 title claims abstract description 58
- 239000002243 precursor Substances 0.000 title claims abstract description 47
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 34
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 34
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 43
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000005484 gravity Effects 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000004804 winding Methods 0.000 claims abstract description 3
- 230000005855 radiation Effects 0.000 claims description 10
- 238000010894 electron beam technology Methods 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 238000010884 ion-beam technique Methods 0.000 claims description 2
- 230000005251 gamma ray Effects 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 230000006641 stabilisation Effects 0.000 abstract description 9
- 238000011105 stabilization Methods 0.000 abstract description 9
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000007363 ring formation reaction Methods 0.000 abstract description 4
- 229920001577 copolymer Polymers 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000005660 chlorination reaction Methods 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 238000006298 dechlorination reaction Methods 0.000 description 4
- 238000009987 spinning Methods 0.000 description 3
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000194370 Cyclocephala pan Species 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 231100000987 absorbed dose Toxicity 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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
- 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
- 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
- D01D10/06—Washing or drying
-
- 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
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- 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
-
- 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
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/003—Treatment with radio-waves or microwaves
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/008—Treatment with radioactive elements or with neutrons, alpha, beta or gamma rays
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Inorganic Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
Description
The present invention relates to a process for producing polyacrylonitrile-based precursor fibers for carbon fibers and polyacrylonitrile-based precursor fibers for carbon fibers produced therefrom. More specifically, the present invention relates to a process for producing polyacrylonitrile- The present invention relates to a polyacrylonitrile precursor fiber for carbon fibers and a process for producing the same, which can treat the chlorination process at a low temperature only for a short time due to a low calorific value in a chlorination process for producing carbon fibers.
Generally, the carbon fiber is made of oxidized acrylonitrile fiber (Oxi), which is molecularly structured and thermally stabilized through an initial thermal stabilization process and an anti-chlorination process in which polyacrylonitrile precursor fibers are heat-treated at a temperature of about 200 to 300 ° C. -PAN fibers) and then heating them to a high temperature of about 800 ° C or higher to finally form a carbon hexagonal structure through a carbonization process.
Since polyacrylonitrile precursor fibers known so far have a very high calorific value of 1500 to 4000 J / g at the high temperature treatment, there is a problem that they are ignited by rapid oxidation due to a high calorific value when treated at a temperature close to 300 DEG C from the beginning, The time required for the chlorination process must be long enough for the chlorination process and the carbonization process to take about 80% or more of the total heat treatment time by gradually increasing the temperature from 3 to 6 stages at the initial temperature, This is a major cause of poor process efficiency.
That is, the conventional chlorination process is a process in which the polyacrylonitrile precursor fibers having a monofilament fineness of about 0.5 to 2.0 denier and a specific gravity of about 1.15 to less than 1.20 are subjected to initial heat stabilization treatment at a temperature of about 200 캜 for a predetermined time, It was necessary to proceed with chloride attack. Usually, the heat treatment is carried out at about 230 ° C for 4 hours, or between 200 ° C and 300 ° C depending on the treatment time. However, it is essential that the thermal stabilization treatment at the initial temperature of 200 ° C. between about 200 ° C. and 240 ° C. for about 15 minutes and for about 1 hour is required.
Therefore, the conventional chlorination process has to be performed for a long time at a high temperature of 200 to 300 ° C. for one to four hours, so that the energy consumption is increased and the manufacturing cost is increased, the process time is prolonged and the productivity is worse there was.
Disclosure of the Invention The object of the present invention is to provide a carbon fiber-reinforced polyolefin composition for carbon fiber which can reduce the heat stabilization process due to a low calorific value in the chlorination process for producing carbon fiber or can perform the chlorination process only at a relatively low temperature for a short time. Acrylonitrile-based precursor fibers and a method for producing the same.
Another object of the present invention is to provide a polyacrylonitrile precursor fiber for carbon fibers having a specific gravity of 1.2 to 1.4 and thermally stabilized by proceeding a cyclization reaction with a part of pyridine in a molecular structure and a process for producing the same.
In order to achieve the above object, in the present invention, an acrylonitrile-based polymer is subjected to water washing, hot water drawing, primary drying, hot steam drawing, secondary drying and winding to obtain a polyacrylonitrile- When preparing the precursor fibers, the secondarily dried polyacrylonitrile filaments are irradiated with radiation.
The polyacrylonitrile precursor fiber for carbon fiber produced by the present invention undergoes a cyclization reaction with a part of pyridine in the molecular structure by irradiation with radiation to have a specific gravity of 1.2 to 1.4 and to be thermally stabilized. As a result, the polyacrylonitrile-based precursor fibers for carbon fiber produced by the present invention can shorten the thermal stabilization time for producing carbon fibers and lower the calorific value in the chlorination step, It can be processed only at a relatively low temperature for a short time than in the prior art, thereby simplifying the manufacturing process of the carbon fiber and improving the productivity.
Hereinafter, the present invention will be described in detail.
The present invention relates to a method for producing a polyacrylonitrile-based precursor fiber for a carbon fiber by preparing an acrylonitrile-based polymer by washing the acrylonitrile-based filament with water, hot drawing, primary drying, hot steam drawing, And irradiating the dried polyacrylonitrile-based filament with radiation.
The radiation may be gamma rays, ion beams, ultraviolet rays, X-rays or electron beams, preferably using electron beams.
It is preferable that the radiation absorbing dose during irradiation be adjusted to 500 to 10,000 kGy to thermally stabilize the polyacrylonitrile-based filament.
The acrylonitrile-based filament may be coated with the silicone oil before the hot-steam-elongated acrylonitrile-based filament is secondarily dried.
In the present invention, an example of a method for producing polyacrylonitrile-based precursor fibers will be described. First, an acrylonitrile-based polymer is spun to produce an acrylonitrile-based filament.
Next, after spinning the irradiated polyacrylonitrile-based multifilament, the washed polyacrylonitrile-based multifilament is hot-water-stretched at 70 to 100 ° C in water, and then the thermally stretched polyacrylonitrile-based multifilament And then the dried polyacrylonitrile multifilament was hot-steam-stretched in a steam of 1 kg / cm 2 캜 to 5 kg / cm 2 캜, and then hot-steam-stretched polyacrylonitrile multifilament Secondary drying is carried out at a temperature of 120 to 220 ° C for 15 seconds to 15 minutes.
Next, the dried polyacrylonitrile multifilament is irradiated with an electron beam so as to have a radiation absorption dose of 500 to 10,000 kGy, and then taken up to produce a polyacrylonitrile-based precursor fiber for carbon fiber.
At this time, an emulsion coating process for coating the polyacrylonitrile-based multifilament with a silicone oil may be selectively performed before secondary drying the hot-steam-stretched polyacrylonitrile multifilament.
In the polyacrylonitrile-based precursor fiber for carbon fiber produced as described above, the cyclization reaction of a part of pyridine in the molecular structure is progressed by heat irradiation to be thermally stabilized, and the specific gravity becomes 1.20 to 1.40.
As a result, the calorific value is reduced to 1,000 to 3,000 J / g in the stabilization process (the chlorination treatment process) for producing the carbon fiber, and the stabilization process can be performed at a low temperature of 200 ° C or lower, And the time required for the stabilization treatment process is shortened to 1/2 or less compared with the conventional one for 30 minutes to 1 hour.
For reference, the polyacrylonitrile-based precursor fibers for carbon fibers not subjected to the radiation irradiation process are not thermally stabilized, so that the amount of heat generated in the chlorination treatment process is as high as 2,000 to 3,500 J / g, 6 hours, the temperature was increased to 1 ~ 4 hours for a long period of time.
Hereinafter, the present invention will be described in detail with reference to examples and comparative examples.
The following examples are only illustrative examples of the present invention and do not limit the scope of protection of the present invention.
Example One
A copolymer consisting of 95 mol% of acrylonitrile, 3 mol% of methacrylic acid and 2 mol% of itaconic acid was polymerized by a solution polymerization method using dimethylsulfoxide as a solvent, ammonia was added thereto in the same amount as itaconic acid And neutralized to prepare a polyacrylonitrile copolymer in the form of ammonium salt to obtain a spinning solution having a copolymer component content of 18% by weight. This spinning solution was spun through a spinneret (temperature: 45 ° C, diameter: 0.08 mm, two holes of 6,000 holes) and introduced into a coagulation bath to be an aqueous solution of 40% dimethyl sulfoxide controlled at 45 ° C., A polyacrylonitrile-based unstretched filament having a number of 12,000 was produced.
Next, the polyacrylonitrile-based unstretched filament was washed with water, stretched five times in hot water at 80 DEG C, and then a network-modified, silicone-based silicone emulsion was applied to obtain a polyacrylonitrile primary stretched filament .
Next, after passing through the above-mentioned polyacrylonitrile primary elongating (intermediate stretching) filament roll heating rollers, the film was first dried and then hot steam drawn to obtain a total draw ratio of 10 in 3 kg / cm < 2 > Followed by secondary drying at a temperature of 30 seconds to prepare a polyacrylonitrile-based drawn filament filament having a filament count of 12,000 with a single filament fineness of 1.5 denier.
Next, polyacrylonitrile-based precursor fibers were prepared by irradiating the polyacrylonitrile-based drawn filament with an electron beam irradiation apparatus at an electron beam absorbing dose of 2,000 / kGy for 30 seconds.
The prepared polyacrylonitrile precursor fibers had a specific gravity of 1.20 and a calorific value of 2,600 J / g was low when the temperature was raised from room temperature to 460 ° C.
Example 2
A polyacrylonitrile precursor fiber was prepared in the same manner as in Example 1, except that the amount of the electron beam absorbed dose was changed to 5,000 kGy when the polyacrylonitrile-based stretched filament of Example 1 was irradiated with an electron beam.
The prepared polyacrylonitrile precursor fibers had a specific gravity of 1.24 and a calorific value of 2,400 J / g when heated up to 460 ° C.
Comparative Example One
A polyacrylonitrile precursor fiber was produced in the same manner as in Example 1, except that the polyacrylonitrile-based stretched filament of Example 1 was directly used as the polyacrylonitrile-based precursor fiber without being irradiated with an electron beam.
The prepared polyacrylonitrile precursor fibers had a specific gravity as low as 1.15, and the calorific value was as high as 2,909J / g when the temperature was increased from room temperature to 460 ° C.
The polyacrylonitrile-based precursor fibers prepared in Example 1 and Comparative Example 1, respectively, were subjected to the chlorination treatment under the following four chlorination conditions. As a result, the density of the chlorinated polyacrylonitrile- The indexes were as shown in Table 1.
My chloride Process conditions
- Treatment condition 1: treatment at a temperature of 230 캜 for 40 minutes
- Treatment condition 2: treatment at a temperature of 230 캜 for 90 minutes
- Treatment condition 3: Treatment at 230 DEG C for 120 minutes
- Treatment condition 4: Treatment at 230 占 폚 for 15 minutes, 240 占 폚 for 15 minutes, 250 占 폚 for 15 minutes, and 260 占 폚 for 15 minutes (total 60 minutes)
My chloride Process execution method
And two para-type wholly aromatic polyamide fibers (aramid fiber, manufactured by Kolon Co., Ltd., product name: Heraclon) having a denier of 3,000 were twisted together as lead fibers. 100 turns / m in the S direction as the lower edge, and 70 turns / m in the Z direction as the upper edge.
The lead wire was connected to the automatic thread hooking device, and the thread hooking device was operated to set the lead fibers in each heat treating furnace. After the setting, the temperature of each heat treatment furnace was raised to the respective specified temperature.
The lead fiber and the polyacrylonitrile-based fiber bundle were connected during the temperature rise of the heat treatment furnace. Each of the heat treatment furnaces was raised to a specified temperature and then driven at a speed of 4 m / min to replace the lead fibers in the heat treatment with polyacrylonitrile-based fibers. Upon completion of the replacement, the target heat-treated polyacrylonitrile-based fibers were continuously wound and transferred to a subsequent process.
(%)
Example 1
Comparative Example 1
* The density was measured according to the ASTM standard.
The Aromatic Index is an index for evaluating the degree of chloride resistance, and is an index of resistance against the total calorific value of polyacrylonitrile-based precursor fibers in a state before the dechlorination process measured by a differential scanning calorimeter (DSC) Is 45 to 60% as a ratio of the calorific value of the polyacrylonitrile-based precursor fiber to the polyacrylonitrile-based precursor fiber.
In Table 1, the polyacrylonitrile-based precursor fibers prepared in Example 1 were subjected to the dechlorination step under the treatment condition 1 (treatment at 230 캜 for 40 minutes), and the polyacrylonitrile precursor fibers prepared in Comparative Example 1 The fiber had reached the same density and aramometry index as that subjected to the dechlorination process under treatment condition 3 (treatment at 230 DEG C for 120 minutes), and the initial dechlorination time was shortened to one third.
In Table 1, the polyacrylonitrile-based precursor fibers prepared in Example 1 and Comparative Example 1, respectively, were subjected to the chlorination treatment under the treating condition 4, and the polyacrylonitrile-based precursor fibers prepared in Example 1 were subjected to chlorination The aramometry index and density after the process were superior to the aromatics index and density after the chlorination process of the polyacrylonitrile precursor fibers prepared in Comparative Example 1.
Claims (6)
A method for producing a polyacrylonitrile precursor fiber for carbon fibers, which comprises irradiating a secondary dried polyacrylonitrile-based filament with radiation.
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| KR1020140061970A KR20150134761A (en) | 2014-05-23 | 2014-05-23 | Method of manufacturing polyacrylonitrile type precursor fiber for carbon fiber and polyacrylonitrile type precursor fiber manufactured thereby |
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| KR1020140061970A KR20150134761A (en) | 2014-05-23 | 2014-05-23 | Method of manufacturing polyacrylonitrile type precursor fiber for carbon fiber and polyacrylonitrile type precursor fiber manufactured thereby |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11286580B2 (en) | 2017-09-29 | 2022-03-29 | Lg Chem, Ltd. | Method for producing acrylonitrile-based fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11286580B2 (en) | 2017-09-29 | 2022-03-29 | Lg Chem, Ltd. | Method for producing acrylonitrile-based fiber |
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