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Preparation method of hydrophilic acrylonitrile copolymer spinning dope

A spinning dope, acrylonitrile technology, which is used in the preparation of spinning solutions, single-component synthetic polymer rayon, textiles and papermaking, etc., can solve the problems of difficult mass transfer, poor repeatability between batches, high viscosity, etc. achieve good technical results

Active Publication Date: 2020-09-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that in the prior art, because the viscosity of the polyacrylonitrile copolymer is relatively large, it is a complex multiphase reaction to make ammonia gas react with the high-viscosity stock solution, and the mass transfer is difficult and difficult to control. The poor repeatability between them is difficult to be applied to the problem of the preparation of polyacrylonitrile spinning dope in industry, and a method for preparing hydrophilic acrylonitrile copolymer spinning dope is provided.

Method used

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  • Preparation method of hydrophilic acrylonitrile copolymer spinning dope

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Acrylic acid is potassiumized before polymerization to form potassium acrylate, and 67.5g of acrylonitrile, 5.25g of acrylic acid, 2.25g of potassium acrylate, 0.075g of azobisisobutyronitrile (AIBN), and 425g of dimethylacetamide are added to the reactor In the process, under the protection of nitrogen, react at a constant temperature of 60°C for 20 hours, and then the spinning solution is decompressed to remove residual monomers and bubbles to obtain a polyacrylonitrile copolymer spinning solution. After testing, the contact angle between the copolymer film made from this stock solution and water is 42.5°.

Embodiment 2

[0026] Sodium itaconate monomethyl before polymerization to form sodium itaconate monomethyl, 85.5g distilled acrylonitrile (AN), 3.6g itaconic acid (IA), 0.9 sodium itaconate monomethyl Add methyl ester, 0.09g azobisisobutyronitrile (AIBN), and 410g N,N-dimethylformamide into the reactor, and react at a constant temperature of 55°C for 24 hours under the protection of helium, and then spin After the silk solution is decompressed to remove residual monomers and air bubbles, a polyacrylonitrile copolymer spinning stock solution is obtained. After testing, the contact angle between the copolymer film made from this stock solution and water is 52.5°.

Embodiment 3

[0028] Ammonium methacrylic acid was hydrogenated before polymerization to form ammonium methacrylate, 102.9 g distilled acrylonitrile (AN), 1.68 g methacrylic acid, 0.42 g ammonium methacrylate, 0.21 g azobisisobutyronitrile (AIBN) and 410g N,N-dimethylacetamide were added to the reactor, and under the protection of argon, they were reacted at a constant temperature of 65°C for 26 hours, and then the spinning solution was decompressed to remove residual monomers and bubbles Finally, the polyacrylonitrile copolymer spinning dope is obtained. After testing, the contact angle between the copolymer film made from this stock solution and water is 45.6°.

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Abstract

The present invention relates to a hydrophilic acrylonitrile copolymer spinning raw liquid preparation method. In the prior art, the method for improving the hydrophilicity of the raw liquid by introducing ammonia gas into the raw liquid has the following problems that the viscosity of the original raw liquid is high, the mass transfer is difficult and is not easily controlled, and the prepared polyacrylonitrile spinning raw liquid is not uniform. A purpose of the present invention is mainly to solve the problems in the prior art. The technical scheme of the present invention comprises that acrylonitrile, a first copolymerization monomer, a second copolymerization monomer and azobisisobutyronitrile adopted as an initiator are mixed in a solvent, the obtained mixture is added to a reactor, a reaction is performed for 12-24 h at a temperature of 50-80 DEG C, and the residual monomer and the bubbles are removed through pressure reducing to obtain the hydrophilic acrylonitrile copolymer spinning raw liquid, wherein the first copolymerization monomer is subjected to ionization before the polymerization to obtain the second copolymerization monomer. With the technical scheme, the problems in the prior art are well solved. The preparation method of the present invention can be used in the industrial production of the carbon fiber raw fiber.

Description

technical field [0001] The invention relates to a method for preparing a hydrophilic acrylonitrile copolymer spinning dope. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, thermal conductivity, etc. It is widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] The initial copolymer structure and properties determine the final carbon fiber structure and properties. Therefore, starting from the synthesis of po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/46C08F220/06C08F222/02C08F222/16C08F6/10D01F6/38D01F9/22D01D1/10D01D1/02
Inventor 沈志刚屠晓萍缪金根赵微微
Owner CHINA PETROLEUM & CHEM CORP