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Preparation technology of caprolactam composite sodium salt

A technology for the preparation of caprolactam, which is applied in the field of preparation of caprolactam composite sodium salt, can solve the problems of easy moisture absorption and deterioration, unsuitable for long-term preparation of large-sized products, poor stability, etc.

Inactive Publication Date: 2018-08-10
XIAN YUANTONG KNIGHT AUTOMOTIVE SAFETY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional casting nylon production process uses sodium caprolactam as a catalyst, which not only has poor stability and is easy to absorb moisture and deteriorate, but also cannot eliminate a large number of hydrogen bonds between MC nylon molecular chains during the casting process, which has little effect on performance improvement , Sodium caprolactam is easy to decompose in the casting high temperature environment, resulting in a short adaptation period, not suitable for long-term preparation of large-scale products

Method used

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  • Preparation technology of caprolactam composite sodium salt
  • Preparation technology of caprolactam composite sodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 10kg of solid caprolactam, heat it up to 100°C in a sealed 50-liter stainless steel tank and melt it for 2 hours, then vacuumize and remove water for 30 minutes until the liquid level is calm, and keep the vacuum at 1000pa;

[0019] Add 333g of powdered NaOH and stir evenly, then slowly raise the temperature to 130°C and continue vacuuming to below 100pa until the water is completely removed and the liquid level is calm;

[0020] Slowly cool down the obtained mixture to 70°C, add 100 g of hexahydro-2H-azepine-2-one, and stir slowly while adding;

[0021] The mixed solution obtained by stirring evenly was cooled to 40°C at a cooling rate of 5°C / min, then removed from the reactor, slowly cooled to room temperature, sealed and isolated from the air, and condensed to a white solid at 25°C, which was the lactam complex sodium salt. After casting experiments, it was found that the product has the characteristics of good stability and long adaptation period (attached fig...

Embodiment 2

[0023] Take 5kg of solid caprolactam, heat it up to 100°C in a sealed 50-liter stainless steel tank and melt it for 2 hours, vacuumize and remove water for 30 minutes until the liquid level is calm, and keep the vacuum at 720pa;

[0024] Add 100g of powdered NaOH and stir evenly, then slowly heat up to 130°C and continue vacuuming to below 100pa until the water is completely removed and the liquid level is calm;

[0025] Slowly cool down the obtained mixture to 70°C, add 50 g of hexahydro-2H-azepine-2-one, and stir slowly while adding;

[0026] The mixed solution obtained by stirring evenly was cooled to 40°C at a cooling rate of 3°C / min, then removed from the reactor, slowly cooled to room temperature, sealed and isolated from the air, and condensed to a white solid at 25°C, which was the lactam complex sodium salt. After casting experiments, it was found that the product has the characteristics of good stability and long adaptation period (attached figure 1 Infrared test an...

Embodiment 3

[0028] Take 15kg of solid caprolactam, heat it up to 100°C in a sealed 50-liter stainless steel tank and melt it for 2 hours, vacuumize and remove water for 30 minutes until the liquid level is calm, and keep the vacuum at 1000pa;

[0029] Add 500g of powdered NaOH and stir evenly, then slowly heat up to 130°C and continue vacuuming to below 100pa until the water is completely removed and the liquid level is calm;

[0030] Slowly cool down the obtained mixture to 70°C, add 75g of hexahydro-2H-azepine-2-one, and stir slowly while adding;

[0031] The mixed solution obtained by stirring evenly was cooled to 40°C at a cooling rate of 2°C / min, then removed from the reactor, slowly cooled to room temperature, sealed and isolated from the air, and condensed to a white solid at 25°C, which was the lactam complex sodium salt. After casting experiments, it was found that the product has the characteristics of good stability and long adaptation period (attached figure 1 Infrared test a...

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Abstract

The invention discloses a preparation technology of caprolactam composite sodium salt and belongs to the technical field of chemical engineering materials. The preparation technology comprises the following steps: 1) after melting a caprolactam main material at 100 DEG C, vacuumizing and removing water for 30min; 2) after adding NaOH and uniformly stirring, raising the temperature to 130 DEG C andcontinually vacuumizing until the pressure is less than 100pa and until water is removed; 3) slowly cooling to 70 DEG C; adding hexahydro-2H-azepine-2-one and slowly stirring; 4) after uniformly stirring, slowly cooling to room temperature; sealing to be isolated from air and condensing at 25 DEG C to obtain a white solid, i.e., the caprolactam composite sodium salt. The preparation technology disclosed by the invention has the advantages of simple synthesis method and technology, wide lactam source, low cost and environment-friendly preparation process; the invention explores a new concept for developing a novel and long-adaptation-period casting nylon composite catalyst.

Description

technical field [0001] The invention relates to a preparation process of caprolactam composite sodium salt, belonging to the technical field of chemical materials. Background technique [0002] Cast nylon is a new type of synthetic material. It heats caprolactam in a container. After it is completely melted, it adds a basic catalyst and vacuumizes it at a certain temperature. After the moisture is exhausted, add a co-catalyst, quickly make it uniform and cast it in a preheated mold, and polymerize it under normal pressure. The material produced by this process is called monomer cast nylon or cast nylon (abbreviated as MC nylon). Because MC nylon has higher molecular weight and crystallinity than ordinary nylon, it has higher tensile strength, modulus, heat distortion temperature and chemical resistance, and has good wear resistance and low moisture absorption. At present, MC nylon is widely used in various fields such as transportation, aerospace, and mechanical preparatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/20
CPCC08G69/20
Inventor 李忠先薛旭东张文博李亚男段振龙王岁祥冯涛赵靓
Owner XIAN YUANTONG KNIGHT AUTOMOTIVE SAFETY TECH
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