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Method suitable for carrying out consolidation forming on polyacrylonitrile carbon fiber precursor by dry-wet method

A polyacrylonitrile carbon fiber, coagulation molding technology, applied in the chemical characteristics of fibers, chemical post-processing of rayon, textiles and papermaking, etc. The effect of strong generality and strong applicability

Active Publication Date: 2015-01-07
ZHONGFU SHENYING CARBON FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This forming method will form very serious structural defects, which will be inherited during the operation of the tow, thus greatly reducing the overall performance of the original silk and even carbon filaments

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, a kind of method that is applicable to dry-wet method polyacrylonitrile carbon fiber precursor coagulation molding, its preparation step is as follows:

[0020] The coagulation bath uses dimethyl sulfoxide as the coagulation bath solute, water as the solvent, the mass concentration is 25%, and the coagulation bath temperature is 0°C. The spinning dope with a pH of 9.5, a dope solid content of 23%, and a temperature of 15°C after ammoniation treatment was passed through a spinneret with 12,000 holes and a hole diameter of 0.12mm at a spinning speed of 20m / min. , enter the coagulation bath after a 10cm air layer, the pre-drawing is controlled at 3.0 times, the residence time of the stock solution in the coagulation bath is 3s, the surface of the stock solution is rapidly quenched to form a hard film, and the double diffusion rate is slowed down by the hard film and conditions such as low temperature and low concentration , and improve the orientation deg...

Embodiment 2

[0021] Embodiment 2, a kind of method that is applicable to dry and wet method polyacrylonitrile carbon fiber precursor coagulation molding, its preparation step is as follows:

[0022] The coagulation bath uses dimethylformamide as the coagulation bath solute, acetone as the solvent, the mass concentration is 30%, and the coagulation bath temperature is 2°C. The spinning dope with a pH of 9.0, a dope solid content of 20%, and a temperature of 20°C after ammoniation treatment was passed through a spinneret with 6,000 holes and a hole diameter of 0.15mm at a spinning speed of 25m / min. , enter the coagulation bath after passing through a 12cm air layer, the pre-drawing is controlled at 3.3 times, the residence time of the stock solution in the coagulation bath is 4s, the surface of the stock solution is rapidly quenched to form a hard film, and the double diffusion rate is slowed down by the hard film and conditions such as low temperature and low concentration , and improve the...

Embodiment 3

[0023] Embodiment 3, a kind of method that is applicable to dry-wet method polyacrylonitrile carbon fiber precursor coagulation molding, its preparation step is as follows:

[0024] The coagulation bath uses dimethyl sulfoxide as the coagulation bath solute, water as the solvent, the mass concentration is 30%, and the coagulation bath temperature is 5°C. The spinning dope with a pH of 9.2, a dope solid content of 20%, and a temperature of 20°C after ammoniation treatment was passed through a spinneret with 6,000 holes and a hole diameter of 0.2mm at a spinning speed of 35m / min. , enter the coagulation bath after passing through a 12cm air layer, the pre-drawing is controlled at 3.3 times, the residence time of the stock solution in the coagulation bath is 5s, the surface of the stock solution is rapidly quenched to form a hard film, and the double diffusion rate is slowed down by the hard film and conditions such as low temperature and low concentration , and improve the orien...

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Abstract

The invention relates to a method suitable for carrying out consolidation forming on a polyacrylonitrile carbon fiber precursor by a dry-wet method. The method comprises the following preparation steps: in a low-temperature low-concentration coagulating bath with a consolidation temperature of 20 DEG C below zero to 25 DEG C and mass concentration of 5 to 40 percent, enabling spinning solution to pass through a spinneret plate and jetting the spinning solution by an air layer so as to enable the spinning solution to enter the coagulating bath, wherein residence time in the coagulating bath is 2 to 10s; rapidly quenching the surface of stock solution to generate a hard film; by the hard film and the conditions of low temperature, low concentration and the like, slowing down a double diffusion rate, improving the orientation degree of nascent fibers by the hard film to realize homogenizing of consolidation forming and avoid a skin-core structure so as to obtain the nascent fibers with pre-draft times of 2.3 to 4.0 times, wherein the nascent fibers have orientation degree of 65 to 70 percent. The protofilament prepared by the method disclosed by the invention has high homogeneity; high-quality protofilaments and carbon filaments can be obtained; moreover, in the dry-wet technology, the method has strong universality and can be popularized and used in the dry-wet production.

Description

technical field [0001] The invention relates to the technical field of preparation of polyacrylonitrile carbon fiber precursors, in particular to a method suitable for low-temperature and low-concentration homogeneous coagulation molding of dry-wet method polyacrylonitrile carbon fiber precursors. Background technique [0002] Polyacrylonitrile-based carbon fiber is the most promising precursor for the production of high-performance carbon fiber. The carbon fiber obtained through the pre-oxidation and carbonization process using polyacrylonitrile precursor fiber as the starting material has the best comprehensive performance. In the process of preparing polyacrylonitrile precursor fiber, coagulation molding is the key link of production, so the molding quality of the primary fiber directly affects the comprehensive performance of the precursor fiber and carbon fiber. In wet spinning, coagulation and forming mainly rely on double diffusion as the forming power, so that the sp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01F11/12
Inventor 张国良李怀京刘芳金亮陈秋飞
Owner ZHONGFU SHENYING CARBON FIBER
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