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Manufacturing method for polyacrylonitrile-based carbon fiber protofilament

A technology of polyacrylonitrile-based carbon fiber and a manufacturing method, which is applied in the field of producing polyacrylonitrile-based carbon fiber precursor by solution spinning process, can solve the problems of purification of precursor and deterioration of mechanical properties, etc., and achieves good purification effect and obvious invention effect. Effect

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0035] Carry out the preparation of carbon fiber precursor according to the following steps:

[0036] 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;

[0037] 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;

[0038] 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;

[0039] 4) The as-spun fiber is placed in the acidic aqueous solution for immersion, the control data of the acid and pH value, the temperature of th...

Embodiment 11～12

[0045] Carry out the preparation of carbon fiber precursor according to the following steps:

[0046] 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;

[0047] 2) to 8) are the same as in Examples 1 to 10.

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Abstract

The invention provides a manufacturing method for a polyacrylonitrile-based carbon fiber protofilament. The third monomer of a protofilament spinning raw material polyacrylonitrile resin is itaconic acid. The preparation method comprises the following successive steps: preparing a spinning solution from the resin by using DMSO or DMAc and carrying out spinning and solidification so as to prepare a nascent fiber; placing the nascent fiber in an aqueous solution of the spinning solvent for water bath drafting and carrying out drip washing with deionized water; dipping the nascent fiber in an acidic aqueous solution for 2 to 10 min; then dipping the nascent fiber in a sodium hydroxide or potassium hydroxide aqueous solution for 1 to 5 min; placing the nascent fiber in pure water for water bath drafting; rinsing the nascent fiber with deionized water until rinsing liquid is neutral and sodium or potassium ions cannot be measured, and then continuing rinsing for 5 to 15 min; and carrying out post-processing procedures like oiling and dry densification so as to obtain a product of the polyacrylonitrile-based carbon fiber protofilament. According to the invention, purification of the protofilament is realized through rinsing, and breaking strength of fibers is not affected, so the defects of the prior art are overcome.

Description

technical field [0001] The invention relates to a method for manufacturing polyacrylonitrile-based carbon fiber precursors, in particular to using itaconic acid as a third comonomer of polyacrylonitrile resin as a spinning raw material to produce polyacrylonitrile-based carbon fiber precursors through a solution spinning process Methods. 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 polya...

Claims

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Application Information

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IPC IPC(8): D01F6/18D01D1/02D01D5/06D06B1/00D01F9/22C08F220/46C08F222/02
Inventor 顾文兰陆正鸣黄翔宇冯林明袁玉红吴嵩义张捷
Owner CHINA PETROLEUM & CHEM CORP
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