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A homogeneous coagulation molding method for polyacrylonitrile precursor

A technology of polyacrylonitrile spinning and polyacrylonitrile, applied in the direction of wet spinning, etc., can solve the problems of slowing down the double diffusion speed, it is difficult to achieve homogenization of coagulation molding, and it is difficult to obtain high-performance PAN precursors and carbon fibers. , to achieve the effect of slowing down the diffusion speed and achieving homogenization

Inactive Publication Date: 2011-11-30
ZHEJIANG TAIXIAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It can be seen that the existing coagulation molding method has great limitations in slowing down the double diffusion speed, and it is difficult to achieve homogenization of coagulation molding, so it is difficult to obtain high-performance PAN precursors and carbon fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Using DMSO as a solvent, azobisisobutyronitrile as an initiator, and acrylonitrile and itaconic acid as comonomers, react in a polymerization tank for 20 hours, wherein the mass percentage of itaconic acid in the total monomers is 1%; After vacuum stripping and standing defoaming, the PAN spinning solution with a solid mass percentage content of 20% is obtained;

[0018] Adopt the way of continuous dropping, add ammonium dihydrogen phosphate aqueous solution to the circulation system of coagulation bath, make the concentration of ammonium dihydrogen phosphate in the coagulation bath be stably controlled at 8×10 -4 mol / L; using a spinneret with 6000 holes (ie 6k) and a diameter of 55 μm in DMSO / H with a concentration of 60wt% and a temperature of 50°C 2 Wet spinning is carried out in a coagulation bath; and then after drawing, washing, oiling, drying, steam drawing and heat setting, the PAN precursor with a fineness of 0.75dtex is obtained.

[0019] Put the above-mentio...

Embodiment 2

[0024] Using the same polymerization and spinning process as in Example 1, the only difference is that the concentration of ammonium dihydrogen phosphate in the control coagulation bath is 1 × 10 -5 mol / L, the PAN precursor with a fineness of 0.75dtex was also prepared.

[0025] The above-mentioned PAN precursor was subjected to the same pre-oxidation, carbonization, and surface treatment processes as in Example 1 to obtain a high-performance PAN-based carbon fiber with a tensile strength of 5.29GPa and a tensile modulus of 286GPa.

Embodiment 3

[0027] Using the same polymerization and spinning process as in Example 1, the only difference is that the ammonia-containing compound added to the coagulation bath circulation system is an aqueous solution of ammonium borate, so that the concentration of ammonium borate in the coagulation bath is stably controlled at 3 × 10 -5 mol / L, the PAN precursor with a fineness of 0.75dtex was also prepared.

[0028] The above-mentioned PAN precursor was subjected to the same pre-oxidation, carbonization, and surface treatment processes as in Example 1 to obtain a high-performance PAN-based carbon fiber with a tensile strength of 5.51 GPa and a tensile modulus of 295 GPa.

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Abstract

The invention discloses a method for homogenizing, solidifying and forming polyacrylonitrile precursor. By adopting a wet spinning technology, a polyacrylonitrile spinning solution trickles in a coagulating bath to be subjected to double diffusions through solvent and precipitator and then solidified and separated so that the polyacrylonitrile precursor is formed. According to the method disclosed by the invention, an ammonia-containing compound is added in the a coagulating bath; the ammonia-containing compound is served as a third component and can be used for retarding the double-diffusion speed in the solidification process of the polyacrylonitrile spinning solution; therefore, the solidifying and forming homogenization is realized; and the high-performance polyacrylonitrile precursor and carbon fibre can be obtained.

Description

technical field [0001] The invention relates to the technical field of preparation of polyacrylonitrile precursors, in particular to a method for homogenizing and solidifying polyacrylonitrile precursors. Background technique [0002] Carbon fiber has many excellent properties such as low density, high specific strength, high specific modulus, high temperature resistance and corrosion resistance, and has been widely used in various fields of aerospace, national defense and civilian industries. According to the raw material route, carbon fiber can be divided into three types: polyacrylonitrile (PAN)-based, pitch-based and viscose-based. Among them, PAN-based carbon fiber has become a carbon fiber with the fastest development, the highest output, the most varieties and the widest application due to its simple production process, low production cost and excellent mechanical properties. [0003] It is well known that high-performance PAN precursors are the prerequisite for the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D5/06
Inventor 欧阳琴陈友汜姜亚平黄显雯莫高明严庆
Owner ZHEJIANG TAIXIAN NEW MATERIAL
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