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Nylon 6 and two-stage polymerization preparation method thereof

A technique of nylon and polymerization reaction, which is applied in the manufacture of rayon, single-component polyamide rayon, and fiber chemical characteristics. It can solve the problems of difficult product quality, operation economy, and complicated preparation process. The concentration of the catalyst can be achieved. Recycling, high reaction efficiency, good anti-aging performance

Pending Publication Date: 2022-01-21
湖南岳化化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production of nylon 6 in my country has problems of product quality and operation economy of large-scale equipment; at the same time, the light stabilizer used in the synthesis of nylon 6 also has the problem of complex preparation process

Method used

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  • Nylon 6 and two-stage polymerization preparation method thereof
  • Nylon 6 and two-stage polymerization preparation method thereof
  • Nylon 6 and two-stage polymerization preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 10mol caprolactam, 1mol iron oxide, 0.1mol N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-naphthalene dicarboxamide into the reactor, React at 121kPa, 260°C for 10h; then transfer the material to the second reactor, and then react at 101kPa, 180°C for 2h. After the reaction, nylon 6 with a relative viscosity of 4.2 is obtained.

[0022] Among them, the preparation method of N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-naphthalene dicarboxamide is as follows: 0.2mol 2,2,6, Add 6-tetramethyl-4-piperidone and 0.1mol 2,7-naphthalene dicarboxylic acid into 20mL of chloroform, then transfer to the reactor, heat and reflux at 61°C for 10h; after the heating and reflux reaction, add 20mL of toluene and 5g of sodium hydroxide were stirred evenly, the organic phase was separated, and after the organic phase was washed and filtered, the stabilizer was obtained, and its structural formula was as follows:

[0023]

Embodiment 2

[0025] Add 15mol caprolactam, 0.5mol iron oxide, 0.3mol N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-naphthalene dicarboxamide into the reactor , react at 121kPa, 260°C for 10h; then transfer the material to the second reactor, and then react at 101kPa, 180°C for 2h. After the reaction, nylon 6 with a relative viscosity of 4.4 is obtained.

[0026] Among them, the preparation method of N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-naphthalene dicarboxamide is as follows: 0.2mol 2,2,6, Add 6-tetramethyl-4-piperidone and 0.1mol 2,7-naphthalene dicarboxylic acid into 20mL of chloroform, then transfer to the reactor, heat and reflux at 61°C for 10h; after the heating and reflux reaction, add Stir 20mL of toluene and 5g of sodium hydroxide evenly, separate the organic phase, wash and filter the organic phase to obtain the stabilizer.

Embodiment 3

[0028] Add 20mol caprolactam, 0.7mol iron oxide, 0.2mol N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-naphthalene dicarboxamide into the reactor , react at 121kPa, 260°C for 10h; then transfer the material to the second reactor, then react at 101kPa, 180°C for 2h, after the reaction, nylon 6 with a relative viscosity of 4.5 is obtained.

[0029] Among them, the preparation method of N,N'-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,3-naphthalene dicarboxamide is as follows: 0.2mol 2,2,6, Add 6-tetramethyl-4-piperidone and 0.1mol 2,7-naphthalene dicarboxylic acid into 20mL of chloroform, then transfer to the reactor, heat and reflux at 61°C for 10h; after the heating and reflux reaction, add Stir 20mL of toluene and 5g of sodium hydroxide evenly, separate the organic phase, wash and filter the organic phase to obtain the stabilizer.

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Abstract

The invention discloses a nylon 6 and a two-stage polymerization preparation method thereof. The preparation method comprises the following steps: adding caprolactam, a catalyst and a stabilizer into a reactor, and carrying out two-stage polymerization reaction to obtain the nylon 6. The two-stage polymerization production method provided by the invention has the advantages of large production capacity, high reaction efficiency, good controllability, less generated waste, low catalyst concentration, recoverability, compatibility with most synthesis methods and the like, and is suitable for large-scale industrial application; meanwhile, the obtained product is relatively good in various properties, good in anti-aging performance and wide in application prospect.

Description

technical field [0001] The invention relates to the technical field of polymer material preparation, in particular to a nylon 6 and a two-stage polymerization preparation method thereof. Background technique [0002] Caprolactam is one of the important organic chemical raw materials. Except for a very small number of hot melt adhesives, fine chemicals and pharmaceuticals, more than 98% of them are polymerized to form polyamide chips (commonly known as nylon-6 chips, or nylon-6 chips) ), and then further processed into nylon fibers, engineering plastics, plastic films. Among them, in the consumption of nylon 6 fiber, the consumption of nylon yarn (including sportswear, casual clothes, socks, etc.) accounts for 47%, the consumption of carpets accounts for 30%, and the consumption of industrial yarn (including cord fabrics, fishing wire nets, etc.) 23%. Domestic nylon 6 fibers used in civilian silk textiles, industrial silk textiles, engineering plastics, film packaging and o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/16D01F6/90D01F1/10
CPCC08G69/16D01F6/90D01F1/106Y02P20/584
Inventor 李兆鹏李伟聪欧文元潘春田丁德贤邬俊杨泰良易恒杰袁学林童明
Owner 湖南岳化化工股份有限公司