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Preparation method of polyacrylonitrile-based precursor

A polyacrylonitrile-based, precursor technology, applied in the direction of spinning solution preparation, single-component synthetic polymer rayon, wet spinning, etc., can solve the problem of low strength of carbon fiber precursor, unstable performance, high filament breakage rate, etc. problems, to achieve the effect of maintaining stability, ensuring stability, and controlling the broken wire rate

Active Publication Date: 2016-06-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention mainly solves the problems existing in the prior art that the spinning dope sprayed out through the filter has poor spinnability, high filament breakage rate, and the carbon fiber precursor obtained by spinning has low strength and unstable performance.

Method used

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  • Preparation method of polyacrylonitrile-based precursor

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Experimental program
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Embodiment 1

[0018] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, and azobisisobutyronitrile (AIBN) accounts for 0.4wt% of the comonomer, Add dimethyl sulfoxide (DMSO) as a solvent into the reactor, and react at a constant temperature of 38° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles, and then filtered through a 5 μm filter material. The filter assembly used first wets the filter, and the dimethyl sulfoxide solvent accounts for 40% of the volume of the filter. The temperature is controlled at 60°C, the vacuum degree of the filter vacuum is at -45KPa (gauge pressure), the speed of the metering pump is controlled so that the rising speed of the stock solution is 25mm / min, the discharge time of the bottom valve is controlled at 15min, and the discharge t...

Embodiment 2

[0026] 1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, and azobisisobutyronitrile (AIBN) accounts for 0.4wt% of the comonomer, Add dimethyl sulfoxide (DMSO) as a solvent into the reactor, and react at a constant temperature of 38° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles, and then filtered through a 5 μm filter material. The filter assembly used first wets the filter, and the dimethyl sulfoxide solvent accounts for 40% of the volume of the filter. The temperature is controlled at 60°C, the vacuum degree of the filter is evacuated at -45KPa (gauge pressure), the speed of the metering pump is controlled so that the rising speed of the stock solution is 30mm / min, the discharge time of the bottom valve is controlled at 20min, and the discharg...

Embodiment 3

[0029] 1.1. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, and azobisisobutyronitrile (AIBN) accounts for 0.4wt of the comonomer %, put dimethyl sulfoxide (DMSO) into the reactor as a solvent, and react at a constant temperature of 38° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution. Then the spinning solution is decompressed to remove residual monomers and air bubbles, and then filtered through a 5 μm filter material. The filter assembly used first wets the filter, and the dimethyl sulfoxide solvent accounts for 40% of the volume of the filter. The temperature is controlled at 60°C, the vacuum degree of the filter vacuum is at -45KPa (gauge pressure), the speed of the metering pump is controlled so that the rising speed of the stock solution is 22mm / min, the discharge time of the bottom valve is controlled at 12min, and the discharge ...

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Abstract

The present invention relates to a preparation method of a polyacrylonitrile-based precursor, and mainly solves the problems that in the prior art bubbles in a material sprayed out by a filter cannot be completely eliminated, spinnability is poor, wire broken rate is high, and a carbon fiber precursor obtained by spinning is low in strength and unstable in performance. The preparation method well solves the problems, and the preparation method includes the following steps: 1) solvent dimethyl sulfoxide, first monomer acrylonitrile, a second monomer itaconic acid and initiator azodiisobutyronitrile are polymerized to obtain a spinning stock solution, and a high performance polyacrylonitrile copolymer spinning stock solution is obtained by filtering after demonomerisation and defoaming of the spinning stock solution; nascent fiber is obtained by jet extrusion and consolidation forming; and a high-performance polyacrylonitrile carbon fiber precursor is obtained by drawing, water washing, oiling, compacting by drying, steam stretching, heat-setting and collection of the nascent fiber; and the method can be used for the industrial production of the carbon fiber precursor.

Description

technical field [0001] The invention relates to a method for preparing polyacrylonitrile-based precursors. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, thermal conductivity, etc. It is widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] Precursor is the prerequisite for producing high-performance carbon fiber, and in the spinning process, the filtering effect of the filter often determines the broken f...

Claims

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Application Information

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IPC IPC(8): D01F6/38D01F9/22D01D1/02D01D5/06C08F220/46
Inventor 张静沈志刚屠晓萍肖士洁
Owner CHINA PETROLEUM & CHEM CORP
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