Method for producing dodecanoic lactam

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

Active Publication Date: 2019-03-26
WANHUA CHEM GRP
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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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0052] Example 1

[0053] 79 g of Lassi solution was added with ammonia water and neutralized to pH=5 to obtain an aqueous solution of hydroxylamine. In a round-bottomed flask replaced with nitrogen, 20 g of cyclododecanone and 120 g of isopropanol were added, heated to 80° C. and maintained at this temperature, and the aforementioned hydroxylamine solution was added dropwise to the round-bottomed flask with stirring. The dropwise addition time was about 30min, and the reaction was continued for 5h after the dropwise addition, and the conversion rate of cyclododecanone reached 99.5%. After the reaction was completed, it was left to stand for 5 min to separate the liquids. The oil phase obtained after liquid separation contained 16.20% 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 flashed under pressure, and the separation time is controlled at 30 min under...

Example Embodiment

[0057] Example 2

[0058] 79 g of Lassi solution was added to ammonia water and neutralized to pH=8 to obtain an aqueous solution of hydroxylamine. In a round-bottomed flask replaced with nitrogen, 20 g of cyclododecanone and 80 g of tert-butanol were added, heated to 90° C. and maintained at this temperature, and the aforementioned hydroxylamine solution was added dropwise to the round-bottomed flask with stirring. The dropwise addition time was about 30min, and the reaction was continued for 2h after the dropwise addition, and the conversion rate of cyclododecanone reached 99.4%. After the reaction was completed, it was left to stand for 30 min to separate the liquids. 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 flashed under pressure, and the separation time is controlled at 1 mi...

Example Embodiment

[0062] Example 3

[0063] 79 g of Lassi solution was added with ammonia water and neutralized to pH=6 to obtain an aqueous solution of hydroxylamine. In a round-bottomed flask replaced with nitrogen, 20 g of cyclododecanone and 100 g of isopropanol were added, heated to 85° C. and maintained at this temperature, and the aforementioned hydroxylamine solution was added dropwise to the round-bottomed flask with stirring. The dropwise addition time was about 30min, and the reaction was continued for 4h after the dropwise addition, and the conversion rate of cyclododecanone reached 99.4%. After the completion of the reaction, it was allowed to stand for 10 min, and the reaction solution was subjected to phase separation treatment. 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 flashed under pr...

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PUM

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Abstract

The invention discloses a method for producing dodecanoic lactam. The method comprises the following steps: carrying out an oximation reaction in the presence of a solvent a by taking cyclododecanoneand Raschig liquid as raw materials; performing pressure distillation on an oil phase obtained by liquid separation to remove and recover the solvent, dissolving the obtained cyclododecone oxime in amolten state with a solvent b, carrying out a Beckmann rearrangement reaction under catalysis of a rare-earth metal modified magnetic solid super-acid catalyst c, and refining, thereby obtaining the product dodecanoic lactam.

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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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
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