Method for removing acrylonitrile monomer in spinning solution

A technology for spinning dope and acrylonitrile, applied in the field of acrylonitrile monomer removal, can solve problems such as skinning of spinning dope, and achieve the effects of reducing residual amount, alleviating the phenomenon of skinning, and avoiding a large amount of extraction

Active Publication Date: 2011-09-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is that in the prior art, when the acrylonitrile monomer in the spinning stock solution is removed, there is a problem that the solvent is easily carried out together, and skinning is easily formed on the surface of the spinning stock solution. A new The removal method of acrylonitrile monomer in the spinning dope

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Through solution polymerization, in the stock solution obtained by the copolymerization of acrylonitrile and itaconic acid, the ratio of acrylonitrile monomer / copolymer / DMSO is 3% / 17% / 80%, and the initiator used in the polymerization process is azobisiso Butyronitrile, the polymerization reaction temperature is 60°C, and the polymerization tank is 5L. After the reaction is finished, vacuumize and remove the sheets. The vacuum degree is 50mbar. After 15 minutes of vacuuming, nitrogen gas is introduced to normal pressure. The nitrogen gas first passes through the preheating device, and the preheating temperature is 55°C. Stir during nitrogen flow, the stirring rate is 50 rpm, and continue to vacuumize after 10 minutes. After repeating this 4 times, the residual single content in the measured mixture is 800ppm.

Embodiment 2

[0027] Through solution polymerization, in the stock solution obtained by copolymerization of acrylonitrile and methyl acrylate, the ratio of acrylonitrile monomer / copolymer / DMSO is 10% / 20% / 70%, and the initiator used in the polymerization process is azodiiso Butyronitrile, the polymerization reaction temperature is 58°C, and the polymerization tank is 5L. After the reaction is finished, vacuumize and remove the sheets. The vacuum degree is 120mbar. After 18 minutes of vacuuming, nitrogen gas is introduced to normal pressure. The nitrogen gas first passes through the preheating device, and the preheating temperature is 55°C. Stir during nitrogen flow, the stirring rate is 180 rpm, and continue to vacuumize after 15 minutes. After repeating this for 3 times, the residual single content in the measured mixture is 600ppm.

Embodiment 3

[0031]Through solution polymerization, in the stock solution obtained by copolymerization of acrylonitrile, itaconic acid and methyl acrylate, the ratio of acrylonitrile monomer / copolymer / DMSO is 8% / 18% / 74%, and the initiator used in the polymerization process is Azobisisoheptanonitrile, the polymerization reaction temperature is 45°C, and the polymerization tank is 5L. After the reaction is finished, vacuumize and remove singletons. The vacuum degree is 80mbar. After evacuating for 18 minutes, nitrogen gas is introduced to normal pressure. The nitrogen gas first passes through the preheating device, and the preheating temperature is 40°C. Stir during nitrogen flow, the stirring rate is 15 rev / min, and continue to vacuumize after 8 minutes. After repeating this 6 times, the residual single content in the measured mixture is 400ppm.

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Abstract

The invention relates to a method for removing an acrylonitrile monomer in a spinning solution, which mainly solves the problem that in the prior art, a solvent is easy to take out together and the surface of the spinning solution is easy to crust in a process of striping the acrylonitrile monomer in the spinning solution. The method comprises the following steps of: placing a copolymer and the spinning solution of an initiator in a container, wherein the copolymer is obtained through the copolymerization between one solvent acrylonitrile monomer containing at least one of dimethylsulfoxide, dimethylformamide and dimethylacetamide and an acrylonitrile monomer, and the initiator initiates the copolymerization of the monomers; vacuumizing the container to a vacuum degree of 5 to 500mbar; b. in the mixing state, injecting gas into the container so as to lead the pressure of the container to restore to the constant pressure, wherein the gas is inert relative to the spinning solution; and c. repeating the steps from a to b so as to ensure that the residual amount of the acrylonitrile monomer in the spinning solution is less than 0.1%. The technical scheme better solves the problem and can be applied to the industrial production of removing the acrylonitrile monomer in a solution spinning process.

Description

technical field [0001] The invention relates to a method for removing acrylonitrile monomers in spinning dope. Background technique [0002] The carbon fiber obtained by ablation of polyacrylonitrile (PAN) fiber has the best comprehensive performance, simple production process, and its output accounts for more than 90% of the total carbon fiber output. It is currently the leading and most promising precursor for the production of high-performance carbon fiber. At present, the one-step spinning process using dimethylsulfoxide (DMSO), dimethylformamide (DMF), and dimethylacetamide (DMAC) as solvents produces the largest amount of raw silk, and the performance of carbon fibers is the most stable after carbonization . Therefore, the preparation of a spinning solution with excellent performance is the prerequisite for obtaining high-performance carbon fibers, and single removal has also become a very critical step in the preparation of the spinning solution. [0003] PAN polyme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D1/02
Inventor 崔晶赵微微沈志刚周文乐王坚
Owner CHINA PETROLEUM & CHEM CORP
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