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Preparation method of binary polyacrylonitrile carbon fiber precursor

A polyacrylonitrile-based carbon fiber and acrylonitrile technology, which is applied in spinning solution preparation, fiber type, fiber treatment, etc., can solve the problems of high amount of comonomer and difficulty in controlling the regularity of polyacrylonitrile polymer structure. Improve the regularity of structure, small fineness, and reduce the effect of dosage

Inactive Publication Date: 2014-03-05
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ternary copolymerization disclosed in the patent to prepare polyacrylonitrile polymers for carbon fiber precursors has the following disadvantages: the amount of comonomer used is relatively large, and the structural regularity of the prepared polyacrylonitrile polymers is difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Vacuumize the polymerization reactor and circulate nitrogen for 3 times. Add 9.9kg of acrylonitrile, 60g of β-methyl itaconate amide, and 41.67kg of dimethyl sulfoxide into a 100L polymerization reactor. Azodiisobutyronitrile, gradually increase the temperature from 35°C to 60°C (taking 5 hours), and gradually add the remaining 40g of the second monomer β-methyl itaconate amide dropwise (continuing 12 hours), while maintaining the reaction at 60°C After 24 hours, the molecular weight of the prepared polyacrylonitrile was 3.9×10 5 g / mol, and the molecular weight distribution is 2.44. The above-mentioned polymer solution is filtered through a pressure-sensitive automatic scraper cylindrical filter, and then singled and defoamed to obtain a spinning stock solution.

[0033] (2) The spinning stock solution obtained in step (1) is subjected to dry-jet wet spinning, the positive draft of the spinneret is 2.2 times, the content of dimethyl sulfoxide in the primary coagula...

Embodiment 2

[0035] (1) Vacuumize the polymerization reactor and circulate nitrogen for 3 times. Add 9.9kg of acrylonitrile, 60g of β-methyl itaconate amide, and 38.46kg of dimethyl sulfoxide into a 100L polymerization reactor. Azodiisobutyronitrile, gradually increase the temperature from 35°C to 60°C (taking 5 hours), and gradually add the remaining 40g of the second monomer β-methyl itaconate amide dropwise (continuing 12 hours), while maintaining the reaction at 60°C After 24 hours, the molecular weight of the prepared polyacrylonitrile was 4.6×10 5 g / mol, molecular weight distribution is 2.56. The above-mentioned polymer solution is filtered through a pressure-sensitive automatic scraper cylindrical filter, and then singled and defoamed to obtain a spinning stock solution.

[0036] (2) The spinning stock solution obtained in step (1) is subjected to dry-jet wet spinning, the positive draft of the spinneret is 2.2 times, the content of dimethyl sulfoxide in the primary coagulation bat...

Embodiment 3

[0038] (1) Vacuumize the polymerization reactor and circulate nitrogen for 3 times. Add 9.9kg of acrylonitrile, 60g of β-methyl itaconate amide, and 41.67kg of dimethyl sulfoxide into a 100L polymerization reactor. Azodiisobutyronitrile, gradually increase the temperature from 35°C to 60°C (taking 5 hours), and gradually add the remaining 40g of the second monomer β-methyl itaconate amide dropwise (continuing 12 hours), while maintaining the reaction at 60°C After 24 hours, the molecular weight of the prepared polyacrylonitrile was 3.6×10 5 g / mol, the molecular weight distribution is 2.42. The above-mentioned polymer solution is filtered through a pressure-sensitive automatic scraper cylindrical filter, and then singled and defoamed to obtain a spinning stock solution.

[0039] (2) The spinning stock solution obtained in step (1) is subjected to dry-jet wet spinning, the positive draft of the spinneret is 2.2 times, the content of dimethyl sulfoxide in the primary coagulation...

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Abstract

The invention relates to a preparation method of a binary polyacrylonitrile carbon fiber precursor. The method comprises the following steps: mixing acrylonitrile, a second comonomer beta-itaconic acid ester amide and a solvent in the presence of nitrogen, and adding an initiator; reacting for 22-38 hours under the condition of 35-75 DEG C, so as to obtain an acrylonitrile polymer; then filtering, taking off and defoaming, so as to prepare a spinning solution; spinning the spinning solution by virtue of a dry-jet wet process, stretching, oiling, drying, densifying, drawing by hot steam, and thermoforming, so as to obtain the binary polyacrylonitrile carbon fiber precursor. By adopting the preparation method, double functional group beta-itaconic acid ester amide is adopted as a comonomer, and a polyacrylonitrile macromolecule for the carbon fiber precursor is prepared by binary copolymerization and substituted ternary copolymerization. Thus, the dosage of the comonomer is reduced, meanwhile, the structural regularity of the polyacrylonitrile macromolecule is improved, and the prepared carbon fiber precursor is even in structure, small in fineness and high in strength.

Description

technical field [0001] The invention belongs to the field of preparation of carbon fiber precursors, in particular to a method for preparing binary polyacrylonitrile-based carbon fiber precursors. Background technique [0002] Carbon fiber has the characteristics of high specific strength, high specific modulus, high temperature resistance, corrosion resistance, fatigue resistance, and creep resistance. and other fields have been widely used. [0003] Polyacrylonitrile-based carbon fiber has always been a hot spot in carbon fiber research and industrialization due to its simple production process and excellent comprehensive performance. The research and development and production of polyacrylonitrile-based carbon fiber started in the 1960s. After being stable in the 1970s and 1980s, it developed rapidly in the 1990s. By the beginning of the 21st century, its preparation technology and process have basically matured. Now it has developed into two types of large tow carbon f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/38D01F9/22D01D1/02D01D5/04D01D5/06D01D5/14D01D10/02D06M15/643C08F220/44C08F222/38C08F4/04D06M101/28
Inventor 徐洪耀巨安奇光善仪
Owner DONGHUA UNIV
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