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Preparation method for polyacrylonitrile-based carbon fiber

A polyacrylonitrile-based carbon fiber and polyacrylonitrile resin technology, which is applied in the fields of fiber chemical characteristics, stretch spinning, single-component synthetic polymer rayon, etc., can solve the problems of raw silk purification and mechanical performance deterioration, etc. Achieve good purification effect and improve mechanical properties

Active Publication Date: 2013-03-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the existing technology has not effectively solved the above-mentioned contradiction between the purification of the raw silk and the deterioration of the mechanical properties

Method used

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  • Preparation method for polyacrylonitrile-based carbon fiber
  • Preparation method for polyacrylonitrile-based carbon fiber
  • Preparation method for polyacrylonitrile-based carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0040] 1) The polyacrylonitrile resin is prepared into a spinning solution by using DMSO as a solvent, and the content of the polyacrylonitrile resin in the spinning solution is 18-25 wt%. Using 30-50wt% DMSO aqueous solution as a coagulation bath to prepare nascent fibers through spinning and coagulation forming by a solution spinning process;

[0041] 2) The as-spun fiber is drawn in a water bath in 20-30 wt% DMSO aqueous solution, and the water bath temperature and the draw ratio of each embodiment are shown in Table 1, and this step is defined as pre-drawing in the table;

[0042] 3) The as-spun fibers are rinsed with deionized water, the water temperature is controlled at 45-60°C, and the rinse time is controlled at 2-20 minutes;

[0043] 4) The as-spun fiber is immersed in a buffer solution containing acid A and salt B. The control data of the buffer solution composition and pH value, the temperature of the buffer solution, the bath ratio and the immersion time of each e...

Embodiment 11～12

[0049] 1) The polyacrylonitrile resin is formulated into a spinning solution by using DMAc as a solvent, and the content of the polyacrylonitrile resin in the spinning solution is 18-25 wt%. Using 30-50wt% DMAc aqueous solution as a coagulation bath to prepare nascent fibers through spinning and coagulation forming by a solution spinning process;

[0050] 2) to 8) are the same as in Examples 1 to 10.

Embodiment 13～20、 comparative example 5～6

[0071] Part of the precursors obtained in the above-mentioned Examples 1-12 and Comparative Examples 1-4 were selected to further prepare carbon fibers. The selected precursors are listed in Table 6.

[0072] The raw silk is first pre-oxidized to obtain pre-oxidized silk. The pre-oxidation is carried out in air and is completed in three stages. The oxidation temperature of the first stage is 210-222°C, the oxidation time is 20-24min, and the draw ratio is 0-5; the oxidation temperature of the second stage is 235-245°C. The time is 20~24min, the draw ratio is -1~1; the third oxidation temperature is 255~265℃, the oxidation time is 20~24min, and the draft ratio is -1~1;

[0073] The pre-oxidized silk is further carbonized in nitrogen, and the carbonization is completed in two stages. The carbonization temperature of the first stage is 350-700°C, the carbonization time is 1-2min, and the drafting ratio is 3-5 times; the carbonization temperature of the second stage is 800 ~1350℃...

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Abstract

The invention provides a preparation method for a polyacrylonitrile-based carbon fiber. The third monomer of a protofilament spinning raw material, i.e., polyacrylonitrile resin, is itaconic acid; a spinning solution is prepared from the resin by using DMSO or DMAc, and spinning and solidification are carried out so as to prepare a nascent fiber. The nascent fiber successively undergoes the following procedures: water bath drafting in an aqueous solution of a spinning solvent; drip washing with deionized water; dipping in a buffer solution containing acid A and salt B, wherein A is sulfuric acid, hydrochloric acid or nitric acid, and B is a sodium salt or a sylvite of A; water bath drafting in pure water; dipping in an acidic aqueous solution; and hot bath rinsing with deionized water until rinsing liquid is neutral. A carbon fiber protofilament is prepared by subjecting the nascent fiber to post-processing procedures like oiling and dry densification. The protofilament undergoes pre-oxidation in an aerobic atmosphere under the condition of drafting and then undergoes carbonization in an anoxic atmosphere under the condition of drafting so as to obtain a finished product of the polyacrylonitrile-based carbon fiber.

Description

technical field [0001] The invention relates to a method for manufacturing polyacrylonitrile-based carbon fibers. The polyacrylonitrile resin used as the raw material for the preparation of carbon fiber precursors uses itacrylic acid as the third comonomer, and the precursors are prepared through a solution spinning process. Background technique [0002] Carbon fiber has excellent mechanical properties, and its extremely high specific strength and specific modulus are incomparable to other materials. As a reinforcing material, it is widely used in the fields of aerospace, aircraft and sports equipment manufacturing. Carbon fibers are usually made from pre-oxidized and carbonized precursors made of carbonizable substances. Because polyacrylonitrile resins have a high carbonization yield, polyacrylonitrile fibers are very ideal carbon fiber precursors. The prepared carbon fibers It is called polyacrylonitrile-based carbon fiber. [0003] In order to obtain polyacrylonitrile-b...

Claims

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Application Information

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IPC IPC(8): D01F9/22D01F6/38D01F11/06D01D5/14D01D10/06C08F220/44C08F220/14C08F220/18C08F218/08C08F222/02
Inventor 顾文兰陆正鸣王平黄翔宇张捷吴嵩义冯林明袁玉红郑鹏
Owner CHINA PETROLEUM & CHEM CORP
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