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Manufacturing 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, wet spinning, textiles and papermaking, can solve the problems of raw silk purification and poor mechanical properties, and achieve good purification effect and mechanical The effect of performance improvement

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～12

[0040] 1) Polyacrylonitrile resin is prepared by using 45-58wt% NaSCN aqueous solution as a solvent to prepare a spinning solution, and the content of polyacrylonitrile resin in the spinning solution is 10-14wt%. Using 8-16wt% NaSCN aqueous solution as a coagulation bath, adopting a wet spinning process, spinning and coagulating to form primary fibers;

[0041] 2) The nascent fibers are drawn in a water bath in an aqueous NaSCN solution of 1 to 5 wt %, and the water bath temperature and drawing ratio of each embodiment are shown in Table 1, and this step is defined as front drawing in the table;

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

[0043] 4) the primary fibers are placed in the acidic aqueous solution and dipped, and the control data such as the acid and pH value, the temperature of the acidic aqueous solution, the bath ratio and the dipping time...

Embodiment 13～20、 comparative example 5～6

[0068] Part of the precursor fibers obtained in the above Examples 1 to 12 and Comparative Examples 1 to 4 were selected to further prepare carbon fibers. The selected precursor fibers are listed in Table 6.

[0069] The raw silk is pre-oxidized to obtain pre-oxidized silk. The pre-oxidation is carried out in the 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 drawing ratio is 0-5; the oxidation temperature of the second stage is 235-245°C, and the oxidation The time is 20~24min, the drafting ratio is -1~1; the oxidation temperature of the third stage is 255~265℃, the oxidation time is 20~24min, and the drafting ratio is -1~1;

[0070] The pre-oxidized wire 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...

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Abstract

The invention provides a manufacturing method for a polyacrylonitrile-based carbon fiber. The third monomer of a protofilament spinning raw material polyacrylonitrile resin is itaconic acid, a spinning solution is prepared from the resin by using an aqueous solution of NaSCN, 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 the aqueous solution of NaSCN; drip washing with deionized water; dipping in an acidic aqueous solution; dipping in a sodium hydroxide or potassium hydroxide aqueous solution; water bath drafting in pure water; and rinsing with deionized water until rinsing liquid is neutral and sodium or potassium ions cannot be measured, and continued rinsing for 5 to 15 min. 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 producing polyacrylonitrile-based carbon fibers. The raw material for carbon fiber preparation is polyacrylonitrile resin, which uses itafuroic acid as the third comonomer, and the raw fibers are prepared by a wet spinning process. Background technique [0002] Carbon fiber has excellent mechanical properties, and its extremely high specific strength and specific modulus are incomparable with other materials. As a reinforcing material, it is widely used in aerospace, aircraft and sports equipment manufacturing and other fields. Carbon fiber is usually obtained by pre-oxidation and carbonization of precursors made of carbonizable substances. Because polyacrylonitrile resin has a high carbonization yield, polyacrylonitrile fibers are very ideal carbon fiber precursors. It is called polyacrylonitrile-based carbon fiber. [0003] In order to obtain polyacrylonitrile-based carbon fibers with excellent performance, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01D1/02D01D5/06D06B1/00C08F220/46C08F222/02
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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