Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF9 Cites 4 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com