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Ternary copolymerization highly hydrophilic polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof

A technology of polyacrylonitrile-based carbon fiber and spinning solution, which is applied in the field of ternary copolymerization of high-hydrophilic polyacrylonitrile-based carbon fiber spinning solution and preparation, can solve the problem of large difference in polymerization rate, high preparation cost and hydrophilicity. It can reduce the surface tension and contact angle, improve the uniformity and density, and avoid severe heat release.

Active Publication Date: 2013-08-14
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in China, acrylonitrile-itaconic acid binary copolymerization or acrylonitrile-itaconic acid-methyl acrylate ternary copolymerization polyacrylonitrile resin is mostly used as the precursor of polyacrylonitrile-based carbon fibers. This system is gradually exposed during use. These defects are not conducive to spinning high-performance polyacrylonitrile precursors and obtaining homogenized pre-oxidized yarns, which limit the strength of the obtained carbon fibers. Further improve
In recent years, people have been studying ways to improve and increase the hydrophilicity of polyacrylonitrile resins, such as Chemical Science and Technology, 2003, 11(4): 1-3 and Polymer Materials Science and Engineering, 2005, 21(2): 132 -134, ammonium itaconate and acrylamide were used as comonomers to improve the hydrophilic properties of the polymer, but the segregation ratios of these two monomers and acrylonitrile are quite different, and it is not suitable to prepare acrylonitrile copolymers with uniform chain structure Chinese patent CN101148489A discloses a highly hydrophilic polyacrylonitrile-based spinning stock solution containing vinylimidazolium salt structural units, but vinylimidazolium salt belongs to ionic liquid, and the preparation cost is relatively high, so it is not suitable for large-scale industrial production
Chinese patents CN1164811C and CN1231616C use polymerization to carry out ammoniation to convert carboxyl groups into ammonia salts. Although the hydrophilicity of polyacrylonitrile resins can be effectively improved, the reaction between ammonia gas and polyacrylonitrile viscous liquid is a complex multiphase reaction , mass transfer is difficult, the reaction is not easy to control, and the reproducibility is poor
The present invention is based on the premise of binary copolymerization of acrylonitrile-itaconic acid, adding a third component to prepare a method for spinning solution of ternary copolymerization highly hydrophilic polyacrylonitrile-based carbon fiber, which has not yet been reported in the literature

Method used

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  • Ternary copolymerization highly hydrophilic polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof
  • Ternary copolymerization highly hydrophilic polyacrylonitrile-based carbon fiber spinning solution and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0020] Add the main monomer (acrylonitrile) / comonomer 1 (itaconic acid) / comonomer 2 (AMPS) into the reactor according to the ratio of 99.50 / 0.45 / 0.05, and the mass concentration of the total monomer is 10%. The amount of nitrogen bisisobutyronitrile is 0.3% of the total weight of monomers, and dimethyl sulfoxide is used as a solvent for copolymerization. Introduce high-purity nitrogen into the reactor for 10 minutes to replace the air in the reaction system, start stirring and raise the temperature to 50°C, and polymerize for 15 hours under the protection of nitrogen to obtain a ternary copolymerization highly hydrophilic acrylonitrile-based carbon fiber spinning solution. The contact angle of PAN resin is 54.5°, and the surface tension is 38.9dyn / cm.

Embodiment 2

[0022] The main monomer (acrylonitrile) / comonomer 1 (itaconic anhydride) / comonomer 2 (AMPS) is added in the reactor according to the ratio of 96.90 / 2.00 / 0.10, and the mass concentration of the total monomer is 12%. The amount of nitrogen bisisobutyronitrile is 0.5% of the total weight of monomers, and dimethyl sulfoxide is used as a solvent for copolymerization. Introduce high-purity nitrogen into the reactor for 20 minutes to replace the air in the reaction system, start stirring and raise the temperature to 60°C, and polymerize for 20 hours under the protection of nitrogen to obtain a ternary copolymerization highly hydrophilic acrylonitrile-based carbon fiber spinning solution. The contact angle of PAN resin is 54.1°, and the surface tension is 37.1dyn / cm.

Embodiment 3

[0024] The main monomer (acrylonitrile) / comonomer 1 (itaconic acid) / comonomer 2 (AMPS) is added in the reactor according to the ratio of 98.88 / 2.00 / 0.12, and the mass concentration of the total monomer is 14%. The amount of nitrogen bisisobutyronitrile is 0.7% of the total weight of monomers, and dimethyl sulfoxide is used as a solvent for copolymerization. Introduce high-purity nitrogen into the reactor for 25 minutes to replace the air in the reaction system, start stirring and raise the temperature to 60°C, and polymerize under the protection of nitrogen for 18 hours to obtain a ternary copolymerization highly hydrophilic acrylonitrile-based carbon fiber spinning solution . The contact angle of PAN resin is 53.9°, and the surface tension is 36.3dyn / cm.

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Abstract

The invention relates to ternary copolymerization highly hydrophilic polyacrylonitrile-based carbon fiber spinning solution, which consists of the following raw materials: acrylonitrile serving as a main monomer, a comonomer 1, a comonomer 2, azodiisobutyronitrile serving as an initiator, and an organic solvent, wherein the weight ratio of the main monomer to the comonomer 1 to the comonomer 2 is(90.0-99.5):(0.45-5.0):(0.05-5.0); the using amount of the azodiisobutyronitrile serving as the initiator is 0.3 to 2.0 percent based on the total weight of the monomers; and the monomers account for10 to 25 mass percent of the solution. The invention has the advantages that: the spinning solution has low cost and high hydrophilicity, and the reaction is easy to control.

Description

technical field [0001] The invention relates to a carbon fiber spinning solution and a preparation method, in particular to a ternary copolymerization highly hydrophilic polyacrylonitrile-based carbon fiber spinning solution and a preparation method. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber has low density, high specific strength, high specific modulus, fatigue resistance, high temperature resistance, wear resistance, creep resistance, electrical conductivity, thermal conductivity, small thermal expansion coefficient, electromagnetic shielding, vibration attenuation Therefore, it can be used not only as structural material, but also as ablation material and functional material to meet the needs of different fields such as aerospace, national defense construction, sports and leisure products, medical equipment and construction. application requirements. The key step in the preparation of high-performance polyacrylonitrile carbon fiber is the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F9/22D01D1/02C08F220/44C08F222/02C08F222/04C08F220/06C08F220/58
Inventor 吕春祥李永红王鹏卢慧斌段晋星袁淑霞
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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