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Method for preparing polyacrylonitrile-based carbon fiber precursor fiber

A polyacrylonitrile-based carbon fiber and carbon fiber technology, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, wet spinning method, etc., can solve the problem of low yield of polyacrylonitrile raw silk, easy gelation in the production process, Adjacent fibers are bonded to each other to prolong the swelling time of the slurry, which is beneficial to smoothness and stable flow direction

Active Publication Date: 2008-04-16
吉林碳谷碳纤维股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production of polyacrylonitrile precursors by this method is low, and the polymerization process is difficult to control, and gels are prone to occur during the production process, resulting in unstable properties of the precursors.
[0005] As the spinning method, dry-wet spinning is generally used, since the dry-wet spinning method includes extruding the spinning solution through a nozzle into the air, and then making it pass through a coagulation bath continuously to form nascent fibers, Therefore, it is easy to obtain dense fibers. On the other hand, reducing the pitch of nozzle holes will cause the problem of bonding adjacent fibers to each other and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The PAN powder prepared by the two-step method of inorganic oxidation-reduction aqueous phase suspension copolymerization is mixed with dimethylacetamide at -18°C to prepare a slurry with a solid content of 16wt%, and vacuumed to 40Kpa. When heated to 45°C, After dissolving for 1 hour, the spinning dope with 16% solid content (this solution can be stored for 24 hours) is obtained, and then the spinning dope is heated to 70°C, sent to the spinning metering pump, and extruded through a 3000-hole spinneret into the The concentration of dimethylacetamide is 50wt%, and the temperature is 50 DEG C in the spinning tube in the coagulation bath, and the negative draft is 0.2%, and the wet spinning is carried out.

[0020] The as-spun fibers are washed 6 times in hot water at 80-90°C and 4 times in water at 91-100°C. After rinsing and removing the solvent, they are stretched at the same time with a total draw ratio of 6.98 times of water washing and drafting. The fibers are immers...

Embodiment 2

[0022] The PAN powder prepared by the two-step method of inorganic oxidation-reduction aqueous phase suspension copolymerization is mixed with dimethylacetamide at -18°C to prepare a slurry with a solid content of 20wt%, and vacuumed to 65Kpa. When heated to 45°C, After dissolving for 1 hour, the spinning dope with 16% solid content (this solution can be stored for 24 hours) is obtained, and then the spinning dope is heated to 70°C, sent to the spinning metering pump, and extruded through a 3000-hole spinneret into the The concentration of dimethylacetamide is 60wt%, the temperature is 45°C in the spinning tube in the coagulation bath, and the negative draft is 0.2%, and the wet spinning is carried out.

[0023] The as-spun fibers are washed 6 times in hot water at 80-90°C and 4 times in water at 91-100°C. After rinsing and removing the solvent, they are stretched at the same time with a total draw ratio of 6.98 times of water washing and drafting. The fibers are immersed in I...

Embodiment 3

[0025] The PAN powder prepared by the two-step method of inorganic oxidation-reduction aqueous phase suspension copolymerization is mixed with dimethylacetamide at -9°C to prepare a slurry with a solid content of 16wt%, and vacuumed to 95Kpa. When heated to 55°C, After dissolving for 1 hour, the spinning dope with 16% solid content (this solution can be stored for 24 hours) is obtained, and then the spinning dope is heated to 80°C, sent to the spinning metering pump, and extruded through a 3000-hole spinneret into the The concentration of dimethylacetamide is 70wt%, the temperature is 40°C in the spinning tube in the coagulation bath, the negative draft is 0.4%, and the wet spinning is carried out.

[0026] The as-spun fibers are washed 6 times in hot water at 80-90°C and 4 times in water at 91-100°C. After rinsing and removing the solvent, they are stretched at the same time with a total draw ratio of 6.98 times of water washing and drafting. The fibers are immersed in In a b...

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Abstract

The invention provides a preparation method for polyacrylonitrile base carbon fiber protofilament. ammonium persulfate-ammonium sulfite or ammonium hydrogen sulfite is used as the aqueous phase suspension copolymerization of a initiation system for preparing polyacrylonitrile base carbon fiber protofilament which uses polymers as raw materials; polymers are made into 16-20Wt percent of slurry at -18-0 DEG C, vacuumized to 40-95 Kpa and dissolved for 1-2 hours at 40-55 DEG C; then spinning stock solution at 70-80 DEG C is extruded into a spinning pipe in coagulation bath via a spinneret to be shaped, and PAN nascent fiber is obtained through the minus elongation of the coagulation bath; the PAN nascent fiber has desolventize flushed away by hot water, and is simultaneously stretched, oiled, dried for densification, baked and elongated to obtain PAN base protofilament, and the tensile strength is no lower than 6.60N / dtex; the carbon fiberstrength is 3.30-4.01Gpa, and the elastic modulus is 210-262Gpa. The main technical indexes of the present invention are equivalent to the similar products in America, Japan and other countries.

Description

technical field [0001] The invention relates to a method for preparing synthetic fiber precursors, in particular to a method for preparing polyacrylonitrile-based carbon fiber precursors. technical background [0002] Carbon fiber is a reinforced and functional fiber material with high strength ratio and high specific modulus. It is a high-tech product developed rapidly in the 1960s. It has a series of comprehensive properties such as low density, heat resistance, chemical corrosion resistance, friction resistance, thermal shock resistance, electrical conductivity, heat conduction, radiation resistance, good damping, shock absorption, and noise reduction. At present, it is widely used in sports equipment, entertainment and leisure, tourist facilities, automobile components, train parts, aircraft manufacturing, electric power, petroleum, chemical industry, navigation, biomedicine, construction, strategic missiles, bulletproof armor and other fields. Therefore, improving the ...

Claims

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Application Information

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IPC IPC(8): D01F6/18D01F9/22D01D5/06
Inventor 王进军马俊庄海林刘明哲王继军周宝庆
Owner 吉林碳谷碳纤维股份有限公司
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