Acrylonitrile copolymer spinning solution with uniform chain structure and narrow molecular-weight distribution and preparation method thereof

A technology of acrylonitrile and copolymer, applied in the field of acrylonitrile copolymer spinning solution and its preparation, can solve the problems of poor uniformity in the microscopic physical structure and chemical reactivity of the precursor, adverse effects on the properties of carbon fibers, etc., and achieve excellent spinnability. Performance, high chain structure uniformity, high conversion effect

Active Publication Date: 2012-01-11
中科金绮新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the instantaneous composition of the polyacrylonitrile copolymer is constantly changing during the polymerization process, the final copolymerized product is actually composed of a "blend" of polyacrylonitrile copolymers containing different amounts of copolymerized segments, and raw materials spun from this copolymer The uniformity of silk in microscopic physical structure and chemical reactivity is poor, which will have an adverse effect on the performance of carbon fiber

Method used

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  • Acrylonitrile copolymer spinning solution with uniform chain structure and narrow molecular-weight distribution and preparation method thereof
  • Acrylonitrile copolymer spinning solution with uniform chain structure and narrow molecular-weight distribution and preparation method thereof
  • Acrylonitrile copolymer spinning solution with uniform chain structure and narrow molecular-weight distribution and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Accurately weigh 26.25Kg of solvent dimethyl sulfoxide and 13.5Kg of the first monomer acrylonitrile and join in the stainless steel reactor A with condenser and mechanical stirring device, stir and mix at room temperature, while nitrogen bubbling protection, Heat up to 60°C on one side;

[0033] (2) Accurately weigh 8.75Kg of the solvent dimethyl sulfoxide and 1.5Kg of the second comonomer itaconic acid and add it to a stainless steel dropping kettle B with a mechanical stirring device, stir and mix at room temperature, and bubble nitrogen for 60 minutes;

[0034] (3) Under nitrogen protection and stirring, 75g free radical initiator azobisisobutyronitrile is thrown into reaction kettle A at one time, and the solution prepared in step (2) is added dropwise to kettle B within 4 hours. Add it to reaction kettle A, stir and react at a constant temperature of 65°C for 6 hours, and then remove residual monomers and air bubbles to obtain an acrylonitrile copolymer spinni...

Embodiment 2

[0036](1) Accurately weigh 24Kg of solvent dimethyl sulfoxide and 9.75Kg of the first monomer acrylonitrile into a stainless steel reactor A with a condenser and a mechanical stirring device, stir and mix at room temperature, while nitrogen bubbling protection, while Heat up to 60°C;

[0037] (2) Accurately weigh 16Kg of the solvent dimethyl sulfoxide and 250g of the second comonomer itaconic acid and add it to a stainless steel dropping kettle B with a mechanical stirring device, stir and mix at room temperature, and bubble nitrogen for 30 minutes;

[0038] (3) Under nitrogen protection and stirring, 60g free radical initiator azobisisobutyronitrile is thrown into reaction kettle A at one time, and the solution prepared in step (2) is added dropwise to kettle B within 4 hours. Add it to the reaction kettle A, stir and react at a constant temperature of 60°C for 24 hours, and then remove residual monomers and air bubbles to obtain an acrylonitrile copolymer spinning solution w...

Embodiment 3

[0040] (1) Accurately take by weighing 31.2Kg solvent dimethyl sulfoxide, the first monomer acrylonitrile of 10.67Kg and the third comonomer methyl acrylate of 220g join in the stainless steel reactor A that has condenser and mechanical stirring device, Stir and mix at room temperature, and raise the temperature to 50°C while nitrogen bubbling is protected;

[0041] (2) Accurately weigh 7.8Kg of solvent dimethyl sulfoxide and 110g of second comonomer acrylic acid and join in the stainless steel dripping kettle B with a mechanical stirring device, stir and mix at room temperature, and bubble nitrogen for 30 minutes;

[0042] (3) Under nitrogen protection and stirring, 55g free radical initiator azobisisoheptanonitrile is thrown into reaction kettle A at one time, and the solution prepared in step (2) is added dropwise to kettle B within 3 hours. Add it to reactor A, stir and react at 50°C for 18 hours, then remove residual monomers and air bubbles to obtain an acrylonitrile cop...

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Abstract

The invention discloses an acrylonitrile copolymer spinning solution and a preparation method thereof. The spinning solution is a dimethyl sulfoxide solution of the acrylonitrile copolymer; the acrylonitrile copolymer is made from the polymerization of a first monomer acrylonitrile and comonomer, and the comonomer contains unsaturated carboxylic acid monomers; the mass of the first monomer acrylonitrile is 90-99.5% of the total mass of the monomers, and the mass of the comonomer is 0.5-10% of the total mass of the monomers; the percentage concentration by mass of the monomers in the spinning solution is 15-30%, and the percentage concentration by mass of the dimethyl sulfoxide in the spinning solution is 70-85%. In the acrylonitrile copolymerization process, by the way of continuously adding a second comonomer in drops during a certain period of the reaction, the invention effectively controls the range of the second comonomer content change in the reaction solution, which ensures that the content of the second comonomer is still in a specific range during a certain period of the reaction to stabilize the instantaneous composition of the acrylonitrile copolymer and produce the acrylonitrile copolymer spinning solution with uniform chain structure, high molecular weight and narrow molecular-weight distribution.

Description

technical field [0001] The invention relates to an acrylonitrile copolymer spinning liquid with uniform chain structure and narrow molecular weight distribution 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 and industrialization in recent years. The key to restricting the development of polyacrylonitrile-based carbon fibers is the quality of polyacrylonitrile precursors, and to obtain high-quality polyacrylonitrile precursors must start from the synthesis of high-quality polyacrylonitrile...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/46D01F6/38D01F9/22
Inventor 肖耀南李春成管国虎徐坚
Owner 中科金绮新材料科技有限公司
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