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Preparation method of high-quality polyacrylonitrile spinning dope

A technology of polyacrylonitrile spinning and stock solution, which is applied in the direction of spinning solution preparation, single-component synthetic polymer rayon, textiles and papermaking, and can solve the problem of low single removal efficiency of carbon fiber spinning stock solution and CV of carbon fiber stock performance Large value and other problems, to achieve the effect of improving the efficiency of single removal, reducing the residual amount, and counteracting the volatilization of sulfoxide

Active Publication Date: 2019-04-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the carbon fiber spinning stock solution prepared in the prior art has a low single removal efficiency, and the CV value of the carbon fiber precursor obtained by spinning is relatively large, and a method for preparing a high-quality spinning stock solution is provided. , the preparation method has the advantages of high single removal efficiency and high solid content, so that high density and high strength carbon fiber precursors can be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] a. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 98:2, with a solid content of 20%, azobisisobutyronitrile (AIBN) accounting for 0.5wt% of comonomers, Add dimethyl sulfoxide (DMSO) into the reactor as a solvent, and react at a constant temperature of 60° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution;

[0020] b. Raise the temperature of the single removal kettle to 60°C, evacuate the pressure of the single removal kettle to a vacuum degree of 30mbar, then slowly pour the prepared polymerization stock solution into the single removal kettle, and flow from the bottom of the single removal kettle to the A mixed gas of dimethyl sulfoxide and nitrogen is introduced into the kettle, the temperature of the mixed gas is 80°C, and the content of dimethyl sulfoxide is 40%. Single quantity is less than 0.3%;

[0021] c. After degassing for 48 hours at a temperature o...

Embodiment 2

[0024] a. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 97:3, with a solid content of 20%, azobisisobutyronitrile (AIBN) accounting for 0.4wt% of the comonomer, Add dimethyl sulfoxide (DMSO) into the reactor as a solvent, and react at a constant temperature of 60° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution;

[0025] b. Raise the temperature of the single removal kettle to 50°C, then place the prepared polymerization stock solution in the single removal kettle, and evacuate the pressure of the single removal kettle to a vacuum degree of 50mbar; The mixed gas of dimethyl sulfoxide and inert gas is introduced inside, the temperature of the mixed gas is 100°C, and the content of dimethyl sulfoxide is 80%. Single quantity is less than 0.3%;

[0026] c. After degassing for 48 hours at a temperature of 60°C and a vacuum of 20 mbar, a high-performance polyacrylonitril...

Embodiment 3

[0029] a. Preparation of stock solution: Distilled acrylonitrile (AN) and itaconic acid (IA) in a ratio of 98:2, with a solid content of 22%, azobisisobutyronitrile (AIBN) accounting for 0.5wt% of the comonomer, Add dimethyl sulfoxide (DMSO) into the reactor as a solvent, and react at a constant temperature of 60° C. for 20 hours under the protection of nitrogen to obtain a binary acrylonitrile copolymer spinning solution;

[0030] b. Raise the temperature of the single removal kettle to 65°C, then place the prepared polymerization stock solution in the single removal kettle, and evacuate the pressure of the single removal kettle to a vacuum degree of 40mbar; The mixed gas of dimethyl sulfoxide and inert gas is introduced inside, the temperature of the mixed gas is 110°C, and the content of dimethyl sulfoxide is 10%. Single quantity is less than 0.3%;

[0031] c. After degassing for 56 hours at a temperature of 50° C. and a vacuum degree of 20 mbar, a high-performance polyacr...

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Abstract

The invention relates to a high-quality polyacrylonitrile spinning raw solution preparation method. A purpose of the present invention is mainly to solve the problems of low monomer removing efficiency and high CV value of the carbon fiber precursor obtained through spinning in the prior art. The technical scheme of the present invention comprises: a, polymerizing a solvent dimethyl sulfoxide, a first monomer acrylonitrile, a second monomer itaconic acid, an initiator azobisisobutyronitrile and an adjustment agent to obtain a polymerization raw solution; and b, vacuumizing the pressure of a monomer removing kettle to achieve a vacuum degree of 10-1000 mbar, and introducing the mixed gas of dimethyl sulfoxide and an inert gas into the kettle from the bottom portion of the monomer removing kettle when the polymerization solution is beaten into the monomer removing kettle so as to obtain the polyacrylonitrile spinning raw solution with characteristics of residual monomer content of less than 0.3% and uniform and stable solid content, wherein the temperature of the mixed gas is 50-150 DEG C, and the dimethyl sulfoxide content in the mixed gas is 0.1-100% (wt). With the technical scheme, the problems in the prior art are well solved. The preparation method of the present invention can be used for the industrial production of the carbon fiber precursor.

Description

technical field [0001] The invention relates to a method for preparing high-quality polyacrylonitrile spinning stock solution. 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. In addition to the moderate molecular weight and good hydrophilicity of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01D1/02D01D1/10C08F220/46C08F222/02C08F6/10D01F9/22
Inventor 史纪友沈志刚缪金根李磊
Owner CHINA PETROLEUM & CHEM CORP
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