Binary acrylonitrile copolymer spinning fluid and preparation method thereof

A technology of acrylonitrile and carbon fiber is applied in the field of spinning solution and preparation of binary acrylonitrile copolymer, which can solve the problems of poor controllability and the like

Inactive Publication Date: 2009-09-30
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ternary radical copolymerization is a very complicated process, especially in the case of a large difference in the reactivity ratio between monomers and a high conversion rate, and the controllability is even worse.
Using a bifunctional monomer with a reactivity rate close to that of acrylonitrile and having both the functions of unsaturated carboxylic acid and unsaturated carboxylic ester as a comonomer to carry out binary copolymerization with acrylonitrile to prepare carbon fiber spinning solution has not yet been see literature report

Method used

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  • Binary acrylonitrile copolymer spinning fluid and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer β-MMI, and the free radical initiator azobisisobutyronitrile were added to the reactor with a condenser tube and a mechanical stirring device. The weight percentage ratio of the added raw materials is: the main monomer acrylonitrile is 98% of the total monomer weight, the comonomer β-MMI is 2% of the total monomer weight, and the amount of azobisisobutyronitrile is the monomer. 0.5% of the total weight, the total monomer concentration (weight percent) is 20%. The mixture was stirred and mixed at room temperature, and after nitrogen bubbling for 20 minutes, under nitrogen protection, the reaction was carried out at a constant temperature of 60 °C for 24 hours, and then residual monomers and air bubbles were removed to obtain a carbon fiber with a uniform chain structure. material spinning solution. The weight average molecular weight of the copolymer is 263,000, and the molecular weight distri...

Embodiment 2

[0022] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer β-MEI, and the free radical initiator azobisisobutyronitrile were added to the reactor with a condenser tube and a mechanical stirring device. The weight percentage ratio of the added raw materials is: the main monomer acrylonitrile is 90% of the total weight of the monomer, the comonomer β-MEI is 10% of the total weight of the monomer, and the amount of azobisisobutyronitrile is the monomer. 0.5% of the total weight, the total monomer concentration (weight percent) is 20%. The mixture was stirred and mixed at room temperature, and after nitrogen bubbling for 20 minutes, under nitrogen protection, the reaction was carried out at a constant temperature of 60 °C for 24 hours, and then residual monomers and air bubbles were removed to obtain a carbon fiber with a uniform chain structure. material spinning solution. The weight-average molecular weight of the copolymer is 92,000, and the molecular...

Embodiment 3

[0024] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer β-MPI, and the free radical initiator azobisisobutyronitrile were added into the reactor with a condenser tube and a mechanical stirring device. The weight percentage ratio of the added raw materials is: the main monomer acrylonitrile is 97% of the total monomer weight, the comonomer β-MPI is 3% of the total monomer weight, and the amount of azobisisobutyronitrile is the monomer. 0.5% of the total weight, the total monomer concentration (weight percent) is 25%. The mixture was stirred and mixed at room temperature, and after nitrogen bubbling for 20 minutes, under nitrogen protection, the reaction was carried out at a constant temperature of 65 ° C for 24 hours, and then the residual monomers and air bubbles were removed to obtain a carbon fiber with a uniform chain structure. material spinning solution. The weight average molecular weight of the copolymer is 298,000, and the molecular weight...

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Abstract

The invention relates to a binary acrylonitrile copolymer spinning solution for carbon fibers with uniform chain structure. The composition of this spinning solution is the dimethyl sulfoxide solution of the copolymer of main monomer acrylonitrile and itaconic acid β-monoester; the main monomer is 90~99.5% of the monomer weight, and the comonomer weight is 0.5-10% of the weight of the monomer, the monomer is the main monomer and comonomer, and the weight percentage concentration of the monomer is 15-25%. Add the solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer, and free radical initiator azobisisobutyronitrile according to the proportioning ratio into the reactor, stir and mix at room temperature, and after bubbling nitrogen for 20 minutes, Under nitrogen protection, react at a constant temperature of 50-70°C for 6-36 hours, remove residual monomers and bubbles, and obtain the product. Its chain structure is uniform, and itaconate β-monoester contains both carboxyl and ester functional groups, which can not only improve the spinnability of polyacrylonitrile resin but also regulate the oxidation-carbonization process of carbon fiber precursors; due to the bifunctional monomer The introduction of itaconate β-monoester greatly reduces the amount of comonomer with acrylonitrile, leading to the improvement of carbon fiber performance.

Description

technical field [0001] The invention relates to a spinning solution of a binary acrylonitrile copolymer for carbon fibers with a uniform chain structure and a preparation method. Background technique [0002] Carbon fiber has the characteristics of high specific strength, high specific modulus, heat resistance, corrosion resistance, fatigue resistance, creep resistance, etc. It is a high-performance fiber material and has been widely used in aerospace, national defense construction, sports and leisure products, medical equipment and construction industries. Polyacrylonitrile-based carbon fibers have outstanding mechanical properties and are a hot spot in carbon fiber research in recent years. Some people think that high-quality polyacrylonitrile precursor is one of the keys to the preparation of high-performance polyacrylonitrile-based carbon fiber, and to obtain high-quality polyacrylonitrile precursor must be synthesized from high-quality acrylonitrile copolymer spinning ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38C08F220/44C08F4/04
Inventor 李悦生张贵宝李百祥白云刚刘晓辉杨正华
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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