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A kind of method for preparing polyacrylonitrile solution by continuous polymerization of dimethyl sulfoxide method

A dimethyl sulfoxide method, dimethyl sulfoxide technology, is applied in the direction of single-component synthetic polymer rayon, textile and papermaking, fiber chemical characteristics, etc. It can improve the thermal performance and hydrophilicity, slow down the exothermic reaction, and achieve the effect of high polymer regularity.

Active Publication Date: 2018-11-09
ZHONG AN XIN TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Batch polymerization has the characteristics of flexible process adjustment, but the concentrated heat release requires high heat exchange capacity of the polymerization tank, which makes the structure of the tank complex, the operation is cumbersome, and the tank is easy to hang glue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Dissolve acrylonitrile: itaconic acid: acrylamide comonomer with a mass ratio of 98:1:1 and chain transfer agent isopropanol in dimethyl sulfoxide solvent at room temperature, stir evenly, and prepare a mixture Feed liquid, the chain transfer agent isopropanol accounted for 0.05% of the monomer mass fraction, and the total feed concentration of the comonomer was 22%.

[0024] (2) Continuously pump the prepared feed liquid into the polymerization kettle, and drop the AIBN solution accounting for 0.4% of the monomer mass fraction into the polymerization kettle at the same time;

[0025] (3) Control the temperature of the reactor to gradually rise from 25° C. to 60° C. When the monomer conversion rate is 63% after the reaction is carried out for 5 hours, feed ammonia gas into the polymerization kettle and discharge to terminate the polymerization reaction to obtain a polymerization liquid;

[0026] (4) The polymerization solution is transferred from the polymerization ...

Embodiment 2

[0028] (1) Dissolve acrylonitrile: itaconic acid: acrylamide comonomer with a mass ratio of 98:1:1 and chain transfer agent isopropanol in dimethyl sulfoxide solvent at room temperature, stir evenly, and prepare a mixture liquid, the chain transfer agent isopropanol accounted for 0.06% of the mass fraction of monomers, and the total feed concentration of comonomers was 23%.

[0029] (2) Continuously pump the prepared feed liquid into the polymerization kettle, and drop the AIBN solution accounting for 0.6% of the monomer mass fraction into the polymerization kettle at the same time;

[0030] (3) Control the temperature of the reactor to gradually rise from 25°C to 62°C. When the monomer conversion rate is 67% after the reaction is carried out for 5 hours, feed ammonia gas into the polymerization kettle and discharge to terminate the polymerization reaction to obtain a polymerization liquid;

[0031] (4) The polymerization solution is transferred from the polymerization kettle ...

Embodiment 3

[0033] (1) Dissolve acrylonitrile: itaconic acid: acrylamide mass ratio comonomer of 95:4:1 and chain transfer agent isopropanol in dimethyl sulfoxide solvent at room temperature, stir evenly, and prepare a mixture Feed liquid, the chain transfer agent isopropanol accounted for 0.01% of monomer mass fraction, and the total feed concentration of comonomer was 20.5%.

[0034] (2) Continuously pump the prepared feed liquid into the polymerization kettle, and drop the AIBN solution accounting for 0.1% of the monomer mass fraction into the polymerization kettle at the same time;

[0035] (3) Control the temperature of the reaction kettle to gradually rise from 25°C to 50°C. When the monomer conversion rate is 70% after 5.5 hours of reaction, feed ammonia gas into the polymerization kettle and discharge to terminate the polymerization reaction to obtain a polymerization solution;

[0036] (4) The polymerization solution is transferred from the polymerization kettle to the single-rem...

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Abstract

The application discloses a method for preparing a polyacrylonitrile solution by continuous polymerization of a dimethyl sulfoxide method and a polyacrylonitrile solution obtained by the method. The method for preparing the polyacrylonitrile solution comprises the following steps: (1) preparing first-third comonomers and dimethyl sulfoxide into mixed feed liquid according to a certain proportion;(2) continuously pumping the mixed feed liquid into a polymerization kettle, and simultaneously dropwise adding the dimethyl sulfoxide solution containing an initiator into the polymerization kettle;(3) controlling the temperature of the reaction kettle to be increased from 25 DEG C to 50-70 DEG C gradually, and when the conversion rate of the comonomer is 60-70%, discharging polymeric liquid toend the reaction; and (4) transferring the polymeric liquid to a demonomerization device to carry out demonomerization and defoaming treatment, thereby obtaining a finished product. According to the method disclosed by the invention, the method for polymerizing the polyacrylonitrile solution by a medium conversion rate is proposed for the first time, and macromolecules are prevented from crosslinking to avoid generating gel; for the polyacrylonitrile solution prepared by the method, the molecular-weight distribution index D is 1.2-2.0 and the isotactic content is 30-34.5%.

Description

technical field [0001] This application generally relates to the technical field of chemical fiber manufacturing, specifically to the technical field of polyacrylonitrile spinning stock solution preparation, and in particular to a method for preparing polyacrylonitrile solution by continuous polymerization of dimethyl sulfoxide and the polyacrylonitrile solution obtained by the method . Background technique [0002] Carbon fiber has excellent performance and is widely used in national defense technology, aerospace and industrial production, among which polyacrylonitrile-based carbon fiber is the fastest growing one. The first step in the preparation of polyacrylonitrile-based carbon fibers is to polymerize polyacrylonitrile, and the quality of the obtained polyacrylonitrile is directly related to the quality of the original silk, which in turn affects the comprehensive performance of carbon fibers. Therefore, it is particularly important to prepare spinning solutions with n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/48C08F222/02C08F220/56C08F2/38C08F2/06D01F6/38D01F9/22
Inventor 王永生张永明方静廉信淑李大伟张平张兆坤刘永华金琥任春生李德生霍照明杨丽云金鹏魏艳军吕长波何旌旗马艳
Owner ZHONG AN XIN TECH CO LTD