Acrylonitrile copolymer spinning solution with high molecular weight and narrow 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 adverse effects on carbon fiber properties, widening of copolymer molecular weight distribution, uneven chain structure, etc., and achieve excellent spinnability. , the effect of narrow molecular weight distribution and widening of the exothermic range

Inactive Publication Date: 2010-08-18
INST OF CHEM CHINESE ACAD OF SCI
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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 chain segments, resulting in a widening of the molecular weight distribution of the copolymer, chain Inhomogeneous structure will adversely affect the performance of carbon fiber

Method used

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  • Acrylonitrile copolymer spinning solution with high molecular weight and narrow distribution and preparation method thereof
  • Acrylonitrile copolymer spinning solution with high molecular weight and narrow distribution and preparation method thereof
  • Acrylonitrile copolymer spinning solution with high molecular weight and narrow distribution and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Stir and mix 34.65Kg dimethyl sulfoxide and 350g ethanol to obtain a mixed solvent for use;

[0042] (2) Accurately weigh 26.25Kg of the above-mentioned mixed solvent and 13.5Kg of the first monomer acrylonitrile and join in a stainless steel reaction kettle A with a condenser and a mechanical stirring device, stir and mix at room temperature, and heat up to 60°C;

[0043] (3) Add the remaining 8.75Kg mixed solvent and 1.5Kg second comonomer itaconic acid into the stainless steel dropping kettle B with a mechanical stirring device, stir and mix at room temperature, and bubble nitrogen for 60 minutes;

[0044] (4) 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 bubbl...

Embodiment 2

[0046] (1) Stir and mix 36kg dimethyl sulfoxide, 2Kg secondary water, and 2Kg methanol to obtain a mixed solvent for use;

[0047] (2) Accurately weigh 24Kg of the above-mentioned mixed solvent and 9.75Kg of the first monomer acrylonitrile and join it in a stainless steel reaction kettle A with a condenser and a mechanical stirring device, stir and mix at room temperature, and heat up to 60 °C while nitrogen bubbling is protected. ℃;

[0048] (3) Add the remaining 16Kg of mixed solvent and 250g of the second comonomer itaconic acid into the stainless steel dropping kettle B with a mechanical stirring device, stir and mix at room temperature, and bubble nitrogen for 30 minutes;

[0049] (4) 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 (3) is added dropwise to kettle B within 4 hours. Add it to reaction kettle A, stir and react at a constant temperature o...

Embodiment 3

[0051] (1) Stir and mix 36.27kg dimethyl sulfoxide and 2.73kg butanone to obtain a mixed solvent for use;

[0052] (2) Accurately weigh 31.2Kg of the above-mentioned mixed solvent, 10.67Kg of the first monomer acrylonitrile and 220g of the third comonomer methyl acrylate and join in the stainless steel reactor A with a condenser and a mechanical stirring device, stir and mix at room temperature , while nitrogen bubbling protection, while raising the temperature to 50 ° C;

[0053] (3) Add the remaining 7.8Kg mixed solvent dimethyl sulfoxide and 110g of the second comonomer acrylic acid into the stainless steel dripping kettle B with a mechanical stirring device, stir and mix at room temperature, and bubble nitrogen for 30 minutes;

[0054] (4) 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 (3) is added dropwise to kettle B within 3 hours. Add it to react...

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Abstract

The invention discloses an acrylonitrile copolymer spinning solution and a preparation method thereof. The spinning solution is a mixed solvent solution of an acrylonitrile copolymer; the acrylonitrile copolymer is formed by polymerization of a first acrylonitrile monomer and a comonomer, and the comonomer comprises unsaturated carboxylic acid monomers; the mass of the first acrylonitrile monomer is 90-99.5% of the total mass of monomers, and the mass of the comonomer is 0.5-10% of the total mass of monomers; the mixed solvent is a mixture comprising dimethyl sulfoxide and at least one of water, alcohol solvents and ketone solvents; and the mass percent concentration of the monomers in the spinning solution is 15-30%. In the invention, the mixed solvent of the dimethyl sulfoxide is adopted in the process of acrylonitrile copolymerization, and the proportion of each solvent is controlled to carry out copolymerization reaction in homogeneous phases; and meanwhile, the second comonomer is continuously replenished in a certain time of reaction to stabilize the instantaneous composition of the acrylonitrile copolymer to obtain the polyacrylonitrile copolymer spinning solution with high molecular weight, narrow molecular weight distribution and uniform chain structure.

Description

technical field [0001] The invention relates to a high-molecular-weight, narrow-distribution acrylonitrile copolymer spinning solution 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 copolymer spinning soluti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/38C08F220/46C08F222/02C08F220/14C08F220/06C08F220/56C08F222/14C08F2/06C08F2/10D01F9/22
Inventor 肖耀南李春成管国虎徐坚
Owner INST OF CHEM CHINESE ACAD OF SCI
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