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Preparation method of acrylonitrile copolymer spinning solution

A technology for spinning dope and acrylonitrile, which is applied in the field of preparing acrylonitrile copolymer spinning dope, can solve the problems of limited solubility, easy generation of gel, unfavorable continuous spinning, etc., and achieves good technical effect and gel content. less effect

Inactive Publication Date: 2012-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can synthesize polyacrylonitrile with a large molecular weight, due to the limited solubility of dimethyl sulfoxide, the viscosity of the spinning stock solution is relatively high, which is prone to gel and clogging the spinneret and many other disadvantages, which is not conducive to continuous production. spinning

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 61.75 g of distilled acrylonitrile (AN), 0.75 g of itaconic acid (IA), 0.31 g of azobisisoheptanonitrile (ABVN) and 187.50 g of N,N-dimethylformamide (DMF) were added to In the reactor, the magnetic sub-stirring makes the mixing uniform, and the reactor is sealed. Under the protection of a gas inert with the reaction substance, react at a constant temperature of 40° C. for 50 hours to obtain an acrylonitrile copolymer spinning solution. After the spinning solution is decompressed to remove residual monomers and air bubbles, a novel acrylonitrile copolymer spinning stock solution is obtained. When the reaction was recorded for 24 hours, the solid content of the spinning solution recorded was 14.3%, and the weight-average molecular weight recorded by GPC was 52700, and the molecular weight distribution was 2.7. In 48 hours, the solid content of the spinning solution recorded was 20.0%, and the GPC The measured weight-average molecular weight is 46200, the molecular weigh...

Embodiment 2

[0016] 49.40 g of distilled acrylonitrile (AN), 0.60 g of itaconic acid (IA), 0.10 g of azobisisoheptanonitrile (ABVN) and 200 g of N,N-dimethylformamide (DMF) were added to the reaction In the reactor, the magnetic sub-stirring makes the mixing uniform, and the reactor is sealed. Under the protection of a gas inert with the reaction substance, the reaction was carried out at a constant temperature of 38° C. for 50 hours to obtain an acrylonitrile copolymer spinning solution. After the spinning solution is decompressed to remove residual monomers and air bubbles, a novel acrylonitrile copolymer spinning stock solution is obtained. When the reaction was recorded for 24 hours, the solid content of the spinning solution recorded was 11.0%, and the weight average molecular weight recorded by GPC was 86800, and the molecular weight distribution was 2.2. In 48 hours, the solid content of the spinning solution recorded was 15.0%, and the GPC The measured weight-average molecular wei...

Embodiment 3

[0018] 81.51 g of distilled acrylonitrile (AN), 0.99 g of itaconic acid (IA), 0.83 g of azobisisoheptanonitrile (ABVN) and 167.50 g of N,N-dimethylformamide (DMF) were added to In the reactor, the magnetic sub-stirring makes the mixing uniform, and the reactor is sealed. Under the protection of an inert gas with the reaction substance, the reaction was carried out at a constant temperature of 33° C. for 50 hours to obtain an acrylonitrile copolymer spinning solution. After the spinning solution is decompressed to remove residual monomers and air bubbles, a novel acrylonitrile copolymer spinning stock solution is obtained. When the reaction was recorded for 24 hours, the solid content of the spinning solution recorded was 19.8%, and the weight-average molecular weight recorded by GPC was 80700, and the molecular weight distribution was 2.6. In 48 hours, the solid content of the spinning solution recorded was 23.8%, and the GPC The measured weight-average molecular weight is 75...

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Abstract

The invention relates to a preparation method of an acrylonitrile copolymer spinning solution to mainly solve a problem of easy gel generation of solutions in the prior art. The preparation method comprises the following steps: 1, adding a solvent, acrylonitrile, itaconic acid and an initiator azo-bis-iso-heptonitrile to a reactor, and reacting at 30-45DEG C for 24-50h under the protection of a gas inert to the reacting substances to obtain an acrylonitrile copolymer spinning solution I; and 2, carrying out pressure reduction on the spinning solution I to remove residual monomers and bubbles to obtain the novel acrylonitrile copolymer spinning solution. The method well solves the problem through above technical scheme, and can be applied to the industrial production of carbon fiber precursors.

Description

technical field [0001] The invention relates to a preparation method of an acrylonitrile copolymer spinning dope. Background technique [0002] The premise of producing high-performance carbon fiber is to use high-quality polyacrylonitrile precursor, and the preparation of high-performance spinning dope is the premise of high-quality polyacrylonitrile precursor. As a high-performance spinning dope, in addition to the characteristics of moderate viscosity, regular polyacrylonitrile molecular chain structure, no branching and cross-linking, and uniform distribution of comonomers on the main chain, the spinning dope must also have high High solid content and narrow molecular weight distribution. [0003] On the premise of ensuring spinnability, the spinning dope must have a high solid content. After pre-oxidation and carbonization, the polyacrylonitrile precursor spun from high solid content spinning dope can easily form a large-area graphite sheet structure. In this way, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/38D01F9/22C08F220/46C08F222/02D01D1/10
Inventor 王贺团沈志刚吴粮华屠晓萍
Owner CHINA PETROLEUM & CHEM CORP
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