Method for preparing polyacrylonitrile spinning solution

A technology of polyacrylonitrile spinning and acrylonitrile, which is applied in the direction of spinning solution preparation, textile and papermaking, fiber chemical characteristics, etc. It can solve the problems such as difficult temperature control, achieve high controllability, less residual monomer, The effect of simple process

Active Publication Date: 2013-06-12
WEIHAI TUOZHAN FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The feed concentration directly affects the heat release of the reaction. The higher the feed concentration, the greater the heat release, and the more difficult it is to control the temperature.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Mix the dimethyl sulfoxide solution of acrylonitrile, itaconic acid, methyl acrylate, and the dimethyl sulfoxide solution of azobisisoheptanonitrile, according to the molar ratio of acrylonitrile, itaconic acid, and methyl acrylate: The ratio of 96:2:2, the mass concentration of comonomer is 19%, and the mass concentration of azobisisoheptanonitrile is 0.2%. Heat up the reaction at 52°C, raise the temperature to 70°C after 8 hours, and increase the vacuum in the kettle to -80kPa, and then increase the vacuum in the kettle to -98kPa after 1h, and continue the extraction for 4h.

[0012] The polymer solution after vacuum extraction is sent to the defoaming tank for continuous defoaming treatment at -80kPa and 70°C. The polymer after defoaming treatment is then filtered through three stages: first stage filtration, filter material It is a 316L stainless steel filter with a filtration accuracy of 5um and a filtration temperature of 70°C, mainly filtering large particles of ...

Embodiment 2

[0019] Mix the dimethyl sulfoxide solution of acrylonitrile, itaconic acid, methyl acrylate, and the dimethyl sulfoxide solution of azobisisoheptanonitrile, according to the molar ratio of acrylonitrile, itaconic acid, and methyl acrylate: The ratio of 96:2.5:1.5, the mass concentration of comonomer is 16%, the mass concentration of azobisisoheptanonitrile is 0.15%, and the solution is filtered through a 0.1um filter cloth before mixing. Heat up the reaction at 54°C, raise the temperature to 80°C after 7 hours, and increase the vacuum in the kettle to -80kPa, and then increase the vacuum in the kettle to -98kPa after 1h, and continue the extraction for 6h.

[0020] The polymer solution after vacuum extraction is sent to the defoaming tank for continuous defoaming treatment at -80kPa and 60°C. The polymer after defoaming treatment is then filtered through three stages: first stage filtration, filter material It is a 316L stainless steel filter with a filtration accuracy of 5um ...

Embodiment 3

[0027] Mix the dimethyl sulfoxide solution of acrylonitrile, itaconic acid, methyl acrylate, and the dimethyl sulfoxide solution of azobisisoheptanonitrile, according to the molar ratio of acrylonitrile, itaconic acid, and methyl acrylate: The ratio of 98:1:1, the mass concentration of comonomer is 20%, and the mass concentration of azobisisoheptanonitrile is 0.2%. Heat up the reaction at 56°C, raise the temperature to 80°C after 7 hours, and increase the vacuum in the kettle to -80kPa, and then increase the vacuum in the kettle to -98kPa after 1h, and continue the extraction for 3h.

[0028] The polymer solution after vacuum extraction is sent to the defoaming tank for continuous defoaming treatment at -80kPa and 80°C. The polymer after defoaming treatment is then filtered through three stages: first stage filtration, filter material It is a 316L stainless steel filter with a filtration accuracy of 5um and a filtration temperature of 80°C, mainly for filtering large particles...

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PUM

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Abstract

The invention belongs to the field of organic polymers and particularly relates to a method for preparing polyacrylonitrile spinning solution. The method comprises the following steps of: mixing the dimethyl sulfoxide solution of acrylonitrile, itaconic acid and methyl acrylate which serve as comonomers with the dimethyl sulfoxide solution of azo-bis-iso-heptonitrile, wherein the concentrations of the comonomers are12-20%, the concentration of the azo-bis-iso-heptonitrile is 0.1-1%, and the molar ratio of the acrylonitrile, the itaconic acid and the methyl acrylate is (96-99):(0.5-3):(0.5-3); carrying out polymerization reaction at the temperature of 50-80 DEG C; controlling the temperature at 60-80 DEG C 5-10 hours later; continuing to stir and extracting a polymer solution in a polymerizing kettle in vacuum until the vacuum degree in the polymerizing kettle is -80kPa; increasing the vacuum degree in the polymerizing kettle to -98kPa after extracting for 1 hour; continuing to extract; feeding the polymer solution extracted in vacuum into a defoaming kettle; continuously defoaming under the condition of -80kPa and 60-80 DEG C; and carrying out tertiary filtering on a defoamed polymer. The method is simple in process and high in controllability, and the content of solid in the prepared spinning solution is large, and the content of residual monomers is low.

Description

technical field [0001] The invention relates to the field of organic polymer materials, in particular to a method for preparing polyacrylonitrile spinning solution with low feeding concentration, high solid content and low residual monomer. Background technique [0002] We know that due to its high specific strength, high specific modulus, and no rust, carbon fiber has a large development space in industries such as automobiles, electric power, construction, electronics, and chemicals, and has become an important component of aircraft, missiles, launch vehicles, and artificial Indispensable basic materials for structures such as satellites. [0003] For carbon fiber production, the quality of the raw silk plays a decisive role, and the performance of the raw silk also affects the cost and output of carbon fiber production. Only high-quality precursors can produce high-quality carbon fibers, and a large part of the quality of precursors depends on the performance of the spin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/46C08F222/02C08F6/06D01D1/02D01F9/22
Inventor 黄大明张大勇张洪池刘艳艳周式桂邱伟峰
Owner WEIHAI TUOZHAN FIBER
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