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A kind of production method of laurolactam

A technology of laurolactam and its production method, which is applied in the production field of laurolactam to achieve the effect of simple control and operation

Active Publication Date: 2020-08-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to provide a production method of laurolactam, which solves the separation problem of the intermediate product oxime and the problem of mass transfer and heat transfer in the rearrangement reaction under the premise of ensuring the efficiency of the oximation reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 79g of Raschig solution was neutralized with ammonia water to pH=5 to obtain aqueous hydroxylamine solution. Add 20 g of cyclododecanone and 120 g of isopropanol to the nitrogen-substituted round-bottom bottle, heat to 80° C., and maintain the temperature, and drop the aforementioned hydroxylamine solution into the round-bottom bottle while stirring. The dropping time is about 30 minutes, and the reaction is continued for 5 hours after the dropping, and the conversion rate of cyclododecanone reaches 99.5%. After the reaction was completed, let it stand for 5 minutes to separate the liquid. The oil phase obtained after liquid separation contained 16.20% of water, no inorganic salt was detected, the content of IPA in the water phase was 0.05%, and the content of cyclododecanone oxime was 11 ppm.

[0054] The oil phase is subjected to pressurized flash evaporation. Under the conditions of pressure 0.6MPa and temperature 135°C, the separation time is controlled at 30 minut...

Embodiment 2

[0058] 79g of Raschig solution was neutralized with ammonia water to pH = 8 to obtain aqueous hydroxylamine solution. Add 20 g of cyclododecanone and 80 g of tert-butanol into the nitrogen-substituted round-bottom bottle, heat to 90° C., and maintain the temperature, and drop the aforementioned hydroxylamine solution into the round-bottom bottle while stirring. The dropwise addition time is about 30 minutes, and the reaction is continued for 2 hours after the dropwise addition is completed, and the conversion rate of cyclododecanone reaches 99.4%. After the reaction was completed, let it stand for 30 minutes to separate the liquid. The oil phase obtained after liquid separation contained 16.15% water, no inorganic salt was detected, the content of tert-butanol in the water phase was 0.04%, and the content of cyclododecanone oxime was 10 ppm.

[0059] The oil phase is subjected to pressurized flash evaporation. Under the conditions of pressure 1.1MPa and temperature 160°C, the...

Embodiment 3

[0063] 79g of Raschig solution was neutralized with aqueous ammonia to pH = 6 to obtain an aqueous solution of hydroxylamine. Add 20 g of cyclododecanone and 100 g of isopropanol to the nitrogen-substituted round-bottom flask, heat to 85° C., and maintain the temperature, and dropwise add the aforementioned hydroxylamine solution into the round-bottom flask while stirring. The dropwise addition time is about 30 minutes, and the reaction is continued for 4 hours after the dropwise addition is completed, and the conversion rate of cyclododecanone reaches 99.4%. After the reaction was completed, it was left to stand for 10 min, and the reaction solution was phase-separated. The oil phase obtained after liquid separation contained 16.3% water, no inorganic salt was detected, the content of isopropanol in the water phase was 0.02%, and the content of cyclododecanone oxime was 7 ppm.

[0064] The oil phase is subjected to pressurized flash evaporation. Under the conditions of press...

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Abstract

A production method of laurolactam, in the presence of a solvent a, the oximation reaction is carried out with cyclododecanone and Raschig liquid as raw materials; the oil phase obtained by liquid separation is removed by pressure distillation and the solvent is recovered, and the obtained Molten cyclododecanone oxime is dissolved in solvent b, and undergoes Beckmann rearrangement reaction under the catalysis of rare earth metal-modified magnetic solid superacid catalyst c, and the laurolactam product is obtained after refining.

Description

technical field [0001] The invention relates to a production method of laurolactam, in particular to a method for efficiently producing laurolactam from cyclododecanone oxime, which belongs to the field of organic chemical synthesis. Background technique [0002] Lauryl lactam is an important chemical raw material for the production of high-performance nylon material - nylon 12. [0003] In industry, laurolactam is obtained from cyclododecanone as raw material through oximation reaction and Beckmann rearrangement reaction. Although from the chemical reaction form, the preparation of laurolactam from cyclododecanone is similar to the preparation of caprolactam from cyclohexanone. However, since the physical and chemical properties of cyclododecanone and its corresponding derivatives are significantly different from those of cyclohexanone and its corresponding derivatives, there is a large difference in the production process. Compared with the production process of preparing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D201/06C07D225/02B01J27/188B01J27/02B01J37/02B01J37/08B01J37/34
CPCB01J27/02B01J27/188B01J37/0201B01J37/031B01J37/082B01J37/342C07D201/06C07D225/02Y02P20/52
Inventor 赵晶李俊平张彦雨杜旺明牟通王漭付松王锐边新建陈海波黎源
Owner WANHUA CHEM GRP CO LTD
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