Method for preparing polyacrylonitrile-based carbon fiber protofilament

A technology of polyacrylonitrile-based carbon fiber and polyacrylonitrile resin, which is applied in the field of producing polyacrylonitrile-based carbon fiber precursors by solution spinning process, and can solve problems such as shortage

Active Publication Date: 2008-04-23
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the process is concerned, the two-step method is obviously more suitable for the manufacture of polyacrylonitrile-based carbon fiber precursors, but at present there is still a lack of effective and industrialized methods for the removal of impurities from the polymerization initiation system in the polyacrylonitrile resin of the spinning raw material. means

Method used

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  • Method for preparing polyacrylonitrile-based carbon fiber protofilament
  • Method for preparing polyacrylonitrile-based carbon fiber protofilament
  • Method for preparing polyacrylonitrile-based carbon fiber protofilament

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0040] The polyacrylonitrile resin, which is the raw material for spinning, is soaked and swelled in deionized water, the water temperature is controlled in the required temperature range, soaked and swelled to the required time, and then taken out to remove excess water. See Table 1 for the process conditions of soaking and swelling;

[0041] The soaked and swollen polyacrylonitrile resin is placed in an aqueous acid solution and stirred for pickling. Embodiment 1~8 adopts nitric acid, and embodiment 9~10 adopts hydrochloric acid, and other pickling process conditions are shown in Table 1;

[0042] Then the polyacrylonitrile resin is rinsed to neutrality with deionized water, and the rinse water temperature is shown in Table 1;

[0043] Finally, the polyacrylonitrile resin is dehydrated by vacuum filtration, and dried at a temperature of 80-100°C until the moisture content of the resin is lower than 3%.

[0044] The ash content and Na ion content of the polyacrylonitrile re...

Embodiment 11～17

[0052] The polyacrylonitrile resin of embodiment 1~10 washing treatment adopts conventional technology to carry out solution spinning, and the steps are as follows:

[0053] Mix the washed resins of Examples 1-10, dissolve them in a solvent to make a spinning stock solution, the solvent is 35-58 wt% NaSCN aqueous solution, and the content of polyacrylonitrile resin in the spinning stock solution is 8-16 wt%;

[0054] The spinning stock solution is spun after removing air bubbles, and is coagulated by a coagulation bath to form nascent fibers. The coagulation bath is 8 to 16 wt% NaSCN aqueous solution, and the temperature of the coagulation bath is controlled between -5 and 16 °C;

[0055] The as-spun fibers were rinsed with deionized water, and the water temperature and rinse time were shown in Table 3;

[0056] The nascent fibers are pickled in an acidic water bath, and the acid is nitric acid or hydrochloric acid, wherein Examples 11-14 and 16-18 are nitric acid, and Example...

Embodiment 18

[0061] The as-spun fibers are directly drawn after pickling, and the drawing is heated by a hot water bath, and the rinsing process is carried out simultaneously with the heating and drawing process in the drawing hot water bath. The drawing hot water bath is deionized water, the temperature of the drawing hot water bath is the same as that of the rinsing hot water bath, and the residence time of the as-spun fibers in the drawing hot water bath is the same as the rinsing time.

[0062] Except above-mentioned, all the other are with embodiment 11~15. Determination of the ash and Na ion content of the raw silk product, the results are shown in Table 4.

[0063] table 3.

[0064]

[0065] Table 4.

[0066] Raw silk ash

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Abstract

The process of preparing polyacrylonitrile fiber for carbon fiber includes the following steps: soaking resin in deionized water at 20-50 deg.c to swell for 1-2.5 hr; pickling in water solution of nitric acid or hydrochloric acid in pH 0.1-3.0 at 25-60 deg.c for 0.5-1.5 hr; rinsing with deionized water to neutral; dewatering and drying to water content lower than 3 %; dissolving in 35-58 wt% concentration NaSCN aqua to form spinning fluid in resin content of 8-16 wt%; debubbling and spinning to form initial fiber; washing with deionized water, acid aqua and hot water successively; drafting, oiling, drying, densifying, etc to produce polyacrylonitrile fiber for carbon fiber. The polyacrylonitrile fiber product has ash content not higher than 0.01% and alkali metal ion content not higher than 0.005%.

Description

technical field [0001] The invention relates to a method for manufacturing polyacrylonitrile-based carbon fiber precursors, in particular to a method for manufacturing polyacrylonitrile-based carbon fiber precursors through a solution spinning process using polyacrylonitrile resin prepared by an aqueous phase suspension polymerization process as a spinning raw material. 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 fiber is usually made of precursors made of carbonizable substances after pre-oxidation and carbonization. Since polyacrylonitrile resin has a high carbonization yield, polyacrylonitrile fiber is a very ideal carbon fiber precursor. The carbon fiber is called polyacrylonitrile-based carbon fiber. To obtain car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01F6/18D01D1/02D01D5/06D01D10/06C08F120/44C08F4/40
Inventor 顾文兰黄翔宇袁玉红关晓凤
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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