Rapid dissolving method for ultrahigh molecular weight polyacrylonitrile

An ultra-high molecular weight, polyacrylonitrile technology, applied in the direction of spinning solution preparation, etc., can solve the problems of unable to prepare polymer solution, difficult to control the dissolution process, unstable factors, etc., to achieve shortened swelling time, low dissolution temperature, The effect of reducing production costs

Inactive Publication Date: 2014-01-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, international research on high-strength and high-modulus polyacrylonitrile fibers mainly focuses on the spinning process of fibers, but in practice, it is found that polyacrylonitrile or its copolymers (usually acrylic raw materials) with a weight average molecular weight of about 70,000 In comparison, due to the high molecular weight, a uniform polymer solution cannot be obtained by conventional dissolution methods, so the preparation of uniform ultra-high molecular weight polymer slurry has become a very important link in the entire manufacturing process of fibers
At present, there are few reports on the dissolution process of polyacrylonitrile, especially ultra-high molecular weight polyacrylonitrile. Zhang Bin (Journal of Donghua University, 2002, 28 (1): 111-114) studied The dissolution process in the sodium cyanate aqueous solution is carried out by heating up in stages, and finally a polyacrylonitrile spinning solution with a solid content of 5% is obtained. However, this swelling and dissolving technology often takes a long time and is likely to cause instability. Occurs, making the dissolution process difficult to control
Mitsubishi Corporation of Japan (JP 2008-214816) studied the dissolution process of polyacrylonitrile with a molecular weight between 1 million and 3 million. This method also has the problem of time-consuming and long-term

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 7L solvent DMSO into the 10L dissolving kettle first, stir at 600-650 rpm, and control the temperature at 18-20℃; add a certain amount of ultra-high molecular weight polyacrylonitrile powder (M w = 1.57 million, M w / M η =1.82) Milling, 200 mesh sieving;

[0024] While stirring, slowly put the ultra-high molecular weight polyacrylonitrile powder into the dissolving kettle; then keep stirring and slowly raise the temperature to 60°C for 6 hours; through observation, it is found that there is no gel mass and the material is discharged, which may be intercepted by the filter The resulting gel mass contains 1% solids.

Embodiment 2

[0026] Add 7L solvent DMSO into the 10L dissolving kettle first, stir at 600-650 rpm, and control the temperature at 18-20℃; add a certain amount of ultra-high molecular weight polyacrylonitrile powder (M w = 1.57 million, M w / M η =1.82) Milling, 200 mesh sieving;

[0027] While stirring, slowly put the ultra-high molecular weight polyacrylonitrile powder into the dissolving kettle; then keep stirring and slowly raise the temperature to 75°C for 7 hours; through observation, it is found that there is no gel mass and the material is discharged, which may be intercepted by the filter The resulting gel mass contains 2% solids.

Embodiment 3

[0029] Add 5L solvent DMSO into the 10L dissolving kettle first, stir at 650-700 revolutions / min, and control the temperature at 18-20℃; add a certain amount of ultra-high molecular weight polyacrylonitrile powder (M w = 2.98 million, M w / M η =1.93) Milling, 200 mesh screen;

[0030] While stirring, slowly put the ultra-high molecular weight polyacrylonitrile powder into the dissolving kettle; then keep stirring, slowly increase the temperature to 80°C, and continue for 10 hours; through observation, it is found that there is no gel mass and the material is discharged, which may be intercepted by the filter The resulting gel mass contains 5% solid content.

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Abstract

The invention relates to a rapid dissolving method for ultrahigh molecular weight polyacrylonitrile. The method comprises the following steps: (1) grinding ultrahigh molecular weight polyacrylonitrile solid particles, sieving with a 50-300 mesh sieve so as to obtain ultrahigh molecular weight polyacrylonitrile powder; (2) slowly adding the ultrahigh molecular weight polyacrylonitrile powder in a solvent with a temperature of 0 to 25 DEG C under mechanical stirring with a rotation speed of 200-1000 revolution per minute, after adding ultrahigh molecular weight polyacrylonitrile powder, heating the solvent to a temperature of 60 to 120 DEG C under mechanical stirring with a rotation speed of 200-1000 revolution per minute, maintaining the temperature for 6 to 12 hours so as to obtain a ultrahigh molecular weight polyacrylonitrile solution, and finally filtering. The rapid dissolving method for ultrahigh molecular weight polyacrylonitrile has the advantages that the dissolving temperature is low, the energy consumption is saved, and the swelling time is greatly reduced so as to quickly finish the dissolution; furthermore, the dissolution operation is convenient, the equipment is simple, and the method is easy to carry out in engineering.

Description

Technical field [0001] The invention belongs to the field of preparation of high-performance carbon fiber precursors, and particularly relates to a method for quickly dissolving ultra-high molecular weight polyacrylonitrile (UHMW-PAN). Background technique [0002] Carbon Fiber (Carbon Fiber) has a series of excellent properties such as high specific strength, high specific modulus, high temperature resistance, corrosion resistance, fatigue resistance, radiation resistance, electrical conductivity, heat transfer, shock absorption, noise reduction and low specific gravity. It is a typical high Performance fiber. It is precisely because of the outstanding performance of carbon fiber that it is used in many fields and products such as aircraft, missiles, oilfield equipment, textile machinery, anti-corrosion chemical equipment, auto parts, precision instruments, anti-static products, building materials, sports equipment, and entertainment products. It is widely used. Compared with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/11C08J3/05C08L33/20D01D1/02D01F9/22
Inventor 姜会钰周美华潘鼎徐东陈力陈惠芳
Owner DONGHUA UNIV
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