High-quality polyacrylonitrile spinning raw solution preparation method

A polyacrylonitrile spinning, high-quality technology, applied in the direction of spinning solution preparation, single-component synthetic polymer rayon, filament molding treatment, etc., can solve the problem of large CV value of carbon fiber precursor performance, carbon fiber spinning stock solution Solve the problems of low single removal efficiency and achieve the effect of improving the single removal efficiency, offsetting the volatilization of sulfoxide, and reducing the residual amount

Active Publication Date: 2017-04-26
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 proportion of 98:2, solid content 20%, azobisisobutyronitrile (AIBN) accounted for 0.5wt% of the comonomer, Add dimethyl sulfoxide (DMSO) as a solvent to the reactor, and react under the protection of nitrogen at a constant temperature of 60°C for 20 hours to obtain a binary acrylonitrile copolymer spinning solution;

[0020] b. Raise the temperature of the single reactor to 60°C, evacuate the pressure of the single reactor to a vacuum of 30 mbar, and then slowly pump the prepared polymerization stock solution into the single reactor, and move from the bottom of the single reactor to The mixed gas of dimethyl sulfoxide and nitrogen is introduced into the kettle, the temperature of the mixed gas is 80℃, and the content of dimethyl sulfoxide is 40%. After the feeding is finished, the vacuum is maintained and the mixer gas is passed through until the residue is obtained. The unit amount...

Embodiment 2

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

[0025] b. Raise the temperature of the single-removing reactor to 50°C, then place the prepared polymerization stock solution in the single-removing reactor, and evacuate the pressure of the single-removing reactor to a vacuum degree of 50 mbar; The mixed gas of dimethyl sulfoxide and inert gas is passed into the mixture, the temperature of the mixed gas is 100 ℃, and the content of dimethyl sulfoxide is 80%. After the feeding is completed, the vacuum is maintained and the mixer gas is passed through until the residue is obtained. The unit amount is less than 0.3%;

[0026] ...

Embodiment 3

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

[0030] b. Raise the temperature of the single reactor to 65°C, then place the prepared polymerization stock solution in the single reactor, and evacuate the pressure of the single reactor to a vacuum of 40mbar; and move from the bottom of the single reactor to the reactor The mixed gas of dimethyl sulfoxide and inert gas is introduced into the mixture. The temperature of the mixed gas is 110°C, and the content of dimethyl sulfoxide is 10%. After the feeding is completed, the vacuum is maintained and the mixer gas is introduced until the residue is obtained. The unit amoun...

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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 dope. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material that 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, heat conduction, etc. Performance, 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] The raw silk is the prerequisite for the production of high-performance carbon fiber. The preparation of high-performance raw silk requires a moderate mol...

Claims

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Application Information

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Patent Type & Authority Applications(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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