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Method for preparing binary polyacrylonitrile-based carbon fiber protofilament

A polyacrylonitrile-based carbon fiber and acrylonitrile technology, applied in dry spinning, wet spinning, stretch spinning, etc., can solve the problems of high amount of comonomer and difficulty in controlling the regularity of polyacrylonitrile polymer structure. , to achieve the effect of improving structural regularity, small fineness, and reducing production costs

Inactive Publication Date: 2012-07-25
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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  • Method for preparing binary polyacrylonitrile-based carbon fiber protofilament
  • Method for preparing binary polyacrylonitrile-based carbon fiber protofilament

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Acrylonitrile and β-ammonium itaconate are mixed evenly in a mass ratio of 99:1 and then added to the reactor (the total concentration of mixed monomers is 25%), then dimethyl sulfoxide is added, and finally azobis Isobutyronitrile (accounting for 0.4% of the total mass of mixed monomers), reacted for 24 hours at 60 ° C, and the prepared polyacrylonitrile molecular weight was 1.8 × 10 5 g / mol, the molecular weight distribution is 2.64. The above-mentioned polymer solution is filtered through a filter material of 1 μm, singled out, and defoamed to obtain a spinning dope.

[0027] (2) step (1) is obtained spinning dope through dry jet wet spinning, the distance of air section is 10cm, and the temperature of air section is 10 ℃, and relative humidity is 65%, and coagulation bath is dimethyl sulfoxide and Water, wherein the content of dimethyl sulfoxide is 60wt%, the temperature of the coagulation bath is 0 ℃, and the coagulation time is 1min; 2.5 times; oiling; 150°C...

Embodiment 2

[0029] (1) Acrylonitrile and β-ammonium itaconate are mixed evenly in a mass ratio of 99:1 and then added to the reactor (the total concentration of mixed monomers is 25%), then dimethyl sulfoxide is added, and finally azobis Isobutyronitrile (accounting for 0.2% of the total mass of mixed monomers), reacted for 24 hours at 60°C, and the prepared polyacrylonitrile molecular weight was 2.1×10 5 g / mol, the molecular weight distribution is 2.78. Filter the above-mentioned polymer solution through a 0.5 μm filter material, remove the single, and defoam to obtain the spinning stock solution.

[0030] (2) step (1) is obtained spinning dope through dry jet wet spinning, the distance of air section is 5cm, and the temperature of air section is 30 ℃, and relative humidity is 50%, and coagulation bath is dimethyl sulfoxide and Water, wherein the content of dimethyl sulfoxide is 45wt%, the temperature of the coagulation bath is 15 ℃, and the coagulation time is 0.5min; Stretching 2 tim...

Embodiment 3

[0032] (1) Acrylonitrile and β-ammonium itaconate are mixed evenly in a mass ratio of 98:2 and then added to the reactor (the total concentration of mixed monomers is 25%), then dimethyl sulfoxide is added, and finally azobis Isobutyronitrile (accounting for 0.2% of the total mass of mixed monomers), reacted for 24 hours at 55°C, and the prepared polyacrylonitrile molecular weight was 1.7×105 g / mol, the molecular weight distribution is 2.84. The above-mentioned polymer solution is filtered through a filter material of 2 μm, singled out, and defoamed to obtain a spinning dope.

[0033] (2) step (1) is obtained spinning dope through dry jet wet spinning, the distance of air section is 15cm, and the temperature of air section is 20 ℃, and relative humidity is 75%, and coagulation bath is dimethyl sulfoxide and Water, wherein the content of dimethyl sulfoxide is 60wt%, the temperature of the coagulation bath is 0 ℃, and the coagulation time is 1min; Stretching 4 times; oiling; dr...

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Abstract

The invention relates to a method for preparing a binary polyacrylonitrile-based carbon fiber protofilament. The method comprises the following steps of: (1) performing copolymerization reaction on acrylonitrile and beta-ammonium itaconate for 10 to 30 hours at the temperature of between 50 and 70 DEG C by using dimethyl sulfoxide as a solvent and using azodiisobutyronitrile as an initiator, filtering, removing residual monomers, and defoaming to obtain a spinning solution; and (2) sequentially performing dry-spray wet spinning, drawing, oiling, drying densification, hot steam drawing and heat setting on the spinning solution, and thus obtaining the carbon fiber protofilament. By the method, the consumption of copolymerization monomers is reduced, and the structural regularity of polyacrylonitrile macromolecules is improved; and the prepared carbon fiber protofilament is uniform in structure, low in fineness and high in strength, and is suitable for preparing high-performance carbon fibers.

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): D01F9/22C08F220/44C08F222/22D01D5/04D01D5/06D01D5/14D01D10/06D01D10/02
Inventor 徐洪耀巨安奇光善仪
Owner DONGHUA UNIV
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