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Preparation method for polyacrylonitrile-based carbon fiber protofilament

A technology of polyacrylonitrile-based carbon fiber and polyacrylonitrile resin is applied in the field of preparing polyacrylonitrile-based carbon fiber precursor by solution spinning process, which can solve the problems of purification of precursor and deterioration of mechanical properties, and achieves good purification effect. obvious effect

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

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0034] Carry out the preparation of carbon fiber precursor according to the following steps:

[0035] 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;

[0036] 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;

[0037] 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;

[0038] 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 p...

Embodiment 11～12

[0043] Carry out the preparation of carbon fiber precursor according to the following steps:

[0044] 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;

[0045] 2) to 7) are the same as in Examples 1 to 10.

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Abstract

The invention provides a preparation method for a polyacrylonitrile-based carbon fiber protofilament. The third monomer of a 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 as a spinning solvent 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 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, and dipping time is controlled to be 2 to 10 min; placing the nascent fiber in pure water for water bath drafting; subjecting the nascent fiber to hot bath rinsing 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.

Description

technical field [0001] The invention relates to a method for preparing polyacrylonitrile-based carbon fiber precursors, in particular to the preparation of polyacrylonitrile-based carbon fiber precursors through a solution spinning process using polyacrylonitrile resins using itaconic acid as the third comonomer as spinning raw materials 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 obt...

Claims

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Application Information

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IPC IPC(8): D01F6/38D01F11/06D01F9/22D01D5/14D01D10/06C08F220/44C08F220/14C08F220/18C08F218/08C08F222/02
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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