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Polyacryl-nitrile spinning fluid containing glyoxaline salt and method of producing the same

A technology for spinning polyacrylonitrile and containing imidazolium salt is applied in the field of polyacrylonitrile-based carbon fiber spinning solution and its preparation to achieve the effects of improving spinnability, improving hydrophilicity and promoting spinnability

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

AI Technical Summary

Problems solved by technology

[0007] A bifunctional monomer with a reactivity rate close to that of acrylonitrile and a comonomer of unsaturated carboxylic acid and unsaturated carboxylic acid ester and a polymerizable ionic liquid with high hydrophilicity are used as comonomers and propylene The preparation of high-performance polyacrylonitrile-based carbon fiber spinning solution by ternary free radical copolymerization of nitrile has not been reported in the literature so far.

Method used

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  • Polyacryl-nitrile spinning fluid containing glyoxaline salt and method of producing the same
  • Polyacryl-nitrile spinning fluid containing glyoxaline salt and method of producing the same
  • Polyacryl-nitrile spinning fluid containing glyoxaline salt and method of producing the same

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Experimental program
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Effect test

Embodiment 1

[0029] Solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer VinBuIm + Br - And β-MMI, azobisisobutyronitrile, a free radical initiator, is added to the reactor with a condenser and a mechanical stirring device. The weight percentage proportioning of added raw material is: main monomer acrylonitrile is 98% of monomer gross weight, comonomer VinBuIm + Br - 1% of the total monomer weight, comonomer β-MMI is 1% of the total monomer weight, and the consumption of azobisisobutyronitrile is 0.5% of the total monomer weight, and the total monomer concentration (percentage by weight) is 20%. 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 60° C. for 24 hours, and then residual monomers and bubbles were removed to obtain a polyacrylonitrile spinning solution containing imidazolium salt. The weight-average molecular weight of the copolymer is 242,0...

Embodiment 2

[0031] Solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer ViEtIm + Br - And β-MEI, the free radical initiator azobisisobutyronitrile, was added to the reactor with a condenser and a mechanical stirring device. The weight percentage proportioning of added raw material is: main monomer acrylonitrile is 90% of monomer gross weight, comonomer ViEtIm + Br - Be 5% of monomer gross weight, comonomer β-MEI is 5% of monomer gross weight, the consumption of azobisisobutyronitrile is 0.5% of monomer gross weight, monomer gross concentration (percentage by weight) is 20%. 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 60° C. for 24 hours, and then residual monomers and bubbles were removed to obtain a polyacrylonitrile spinning solution containing imidazolium salt. The weight-average molecular weight of the copolymer is 109,000, the molecular wei...

Embodiment 3

[0033] Solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer ViMeIm + Cl - And β-MPI, a free radical initiator azobisisobutyronitrile, is added to the reactor with a condenser and a mechanical stirring device. The weight percent proportioning of added raw material is: main monomer acrylonitrile is 97% of monomer gross weight, comonomer ViMeIm + Cl - 1% of the total weight of the monomers, comonomer β-MPI is 2% of the total weight of the monomers, and the consumption of azobisisobutyronitrile is 0.5% of the total weight of the monomers, and the total concentration of the monomers (percentage by weight) 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 polyacrylonitrile spinning solution containing imidazolium salt. The weight-average molecular weight...

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Abstract

The invention relates to a polyacrylonitrile spinning liquid containing imidazolium salt and a preparation method thereof. The described spinning solution is a dimethyl sulfoxide solution of the main monomer acrylonitrile and comonomer 1 itaconate β-monoester and comonomer 2 vinylimidazolium salt copolymer; the main monomer is monomer total 90-99.5% of the weight, the total weight of the comonomer is 0.5-10% of the total weight of the monomer; wherein the comonomer 1 accounts for 10-90% of the total weight of the comonomer, and the total monomer concentration (percentage by weight) is 15% ~25%. Add solvent dimethyl sulfoxide, main monomer acrylonitrile, comonomer 1 and comonomer 2, free radical initiator azobisisobutyronitrile into the reactor with condenser tube and mechanical stirring device according to the ratio Stir and mix at room temperature. After bubbling nitrogen for 20 minutes, under the protection of nitrogen, react at a constant temperature of 50-70°C for 6-36 hours, and then remove residual monomers and bubbles to obtain a polypropylene containing imidazolium salt. Nitrile spinning solution. Its characteristics are: uniform chain structure, narrow distribution, and high hydrophilicity.

Description

technical field [0001] The invention relates to a polyacrylonitrile-based carbon fiber spinning solution containing a bifunctional monomer β-itaconate and a highly hydrophilic ionic monomer vinylimidazolium salt structural unit 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-quality polyacrylonitrile precurs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/38D01F9/22
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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