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Binary acrylonitrile copolymer spinning fluid and preparation method thereof

A technology of binary acrylonitrile and copolymer, which is applied in the direction of single-component synthetic polymer rayon, textiles and papermaking, and fiber chemical characteristics, which can solve the problems of poor controllability and other problems

Inactive Publication Date: 2008-04-09
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
  • Binary acrylonitrile copolymer spinning fluid and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0021] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer β-MMI, and the free radical initiator azobisisobutyronitrile are added to a 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 weight of the monomers, the comonomer β-MMI is 2% of the total weight of the monomers, and the amount of azobisisobutyronitrile is 98% of the total weight of the monomers. 0.5% of the total weight, the total monomer concentration (weight percent) is 20%. The mixture was stirred and mixed at room temperature. After bubbling nitrogen gas for 20 minutes, it was reacted at a constant temperature of 60° C. for 24 hours under the protection of nitrogen gas, and then residual monomers and bubbles were removed to obtain a binary acrylonitrile copolymer spinning solution. The weight average molecular weight of the copolymer is 263,000, and the molecular wei...

Embodiment 2

[0023] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer β-MEI, and the free radical initiator azobisisobutyronitrile are added to a 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 monomers, the comonomer β-MEI is 10% of the total weight of the monomers, and the amount of azobisisobutyronitrile is 90% of the total weight of the monomers. 0.5% of the total weight, the total monomer concentration (weight percent) is 20%. The mixture was stirred and mixed at room temperature. After bubbling nitrogen gas for 20 minutes, it was reacted at a constant temperature of 60° C. for 24 hours under the protection of nitrogen gas, and then residual monomers and bubbles were removed to obtain a binary acrylonitrile copolymer spinning solution. The weight-average molecular weight of the copolymer is 92,000, and the molecular wei...

Embodiment 3

[0025] The solvent dimethyl sulfoxide, the main monomer acrylonitrile, the comonomer β-MPI, and the free radical initiator azobisisobutyronitrile are 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 97% of the total weight of the monomers, the comonomer β-MPI is 3% of the total weight of the monomers, and the amount of azobisisobutyronitrile is 97% of the total weight of the monomers. 0.5% of the total weight, the total monomer concentration (weight percent) is 25%. The mixture was stirred and mixed at room temperature. After bubbling nitrogen for 20 minutes, under the protection of nitrogen, it was reacted at a constant temperature of 65°C for 24 hours, and then residual monomers and bubbles were removed to obtain a binary acrylonitrile copolymer spinning solution. The weight-average molecular weight of the copolymer is 298,000, and the molecular weight dis...

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Abstract

The invention relates to binary acrylonitrile copolymer spinning solution and a corresponding production method. The spinning solution comprises main monomer acrylonitrile and dimethyl sulfoxide solution with copolymer of itaconic acid Beta- monoester; the weight of the main monomer accounts for 90% to 99.5% of that of monomer, while the weight of the comonomer accounts for 0.5% to 10% thereof. The monomer is composed of the main monomer and the comonomer and the weight percentage concentration of the monomer is from15% to 25%. The dimethyl sulfoxide solution, the main monomer acrylonitrile, the comonomer, free radical initiator of azobisisobutyronitrile are added to a reactor by proportion and then mixed at room temperature and reacted for six to thirty six hours at a constant temperature of 50 DEG C to 70 DEG C to remove bubble of residual monomer and obtain the solution with protection from nitrogen which has bubbled for twenty minutes. The solution has a uniform chain structure and itaconic acid Beta-monoester contains two functional groups of carboxy and ester, thus being able to improve spinnability of polyacrylonitrile resin as well as regulate an oxidation-carbonization process of carbon fiber precursor. Due to introduction of a bifunctional group of monomer itaconic acid Beta-monoester, the amount of acrylonitrile comonomer is greatly reduced to improve performance of carbon fiber.

Description

technical field [0001] The invention relates to a binary acrylonitrile copolymer spinning liquid and a preparation method thereof, in particular to a polyacrylonitrile-based carbon fiber spinning liquid containing itaconic acid β-monoester structural units and a preparation method thereof. Background technique [0002] Carbon fiber has the characteristics of high specific strength, high specific modulus, heat resistance, corrosion resistance, fatigue resistance, and creep resistance. It is a high-performance fiber material and has been widely used in aerospace, national defense construction, sports and leisure products, and medical equipment. and construction industries. Polyacrylonitrile-based carbon fiber has outstanding mechanical properties and is a hot spot in carbon fiber research in recent years. Some people think that high-quality polyacrylonitrile precursor is one of the keys to prepare high-performance polyacrylonitrile-based carbon fibers, and to obtain high-qual...

Claims

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Application Information

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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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