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

Method for preparing oxime

A technology of catalyst and mixture, which is applied in oxime preparation, organic chemistry, etc., can solve the problems of unfriendly environment, environmental pollution, large amount of hydroxylamine salt, etc., and achieve the effect of simple post-processing, expanding application fields, and high selectivity

Inactive Publication Date: 2018-08-10
EAST CHINA NORMAL UNIV
View PDF4 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, oxime is mainly synthesized by reacting hydroxylamine salt with ketone or aldehyde. This preparation method not only consumes a large amount of hydroxylamine salt, but also produces a large amount of inorganic salt by-products. This process is an environmentally unfriendly process and is likely to cause environmental pollution.

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

[0019] The first step: sequentially add cyclohexanone and Ti-MSE molecular sieves, tert-butanol and ammonia water with a mass concentration of 25% into the reactor, and stir evenly to obtain a reaction system. In the reaction system, cyclohexanone and Ti-MSE molecules and The weight ratio of tert-butanol is 1:0.05:5, and the mol ratio of cyclohexanone and ammoniacal liquor is 1:2.

[0020] The second step: when the reaction temperature of the reaction system in the first step rises to 70°C, dropwise add hydrogen peroxide with a mass concentration of 30% in the reaction system, and the dropwise addition time is 1 hour, and continue the reaction after the dropwise addition is completed 1 Hour, the mol ratio of described hydrogen peroxide and cyclohexanone is 1.5: 1.

[0021] The third step: After the reaction is completed, the Ti-MSE molecular sieve catalyst is separated according to the conventional filtration method, and then according to the conventional distillation operatio...

Embodiment 2

[0023] The first step: sequentially add cyclohexanone and Ti-MSE molecular sieve, water and mass concentration of 25% ammonia water to the reactor, stir to obtain a reaction system, in which cyclohexanone and Ti-MSE molecules and water The weight ratio is 1: 0.1: 5, and the mol ratio of cyclohexanone and ammonia is 1: 2.

[0024] The second step: when the reaction temperature of the reaction system in the first step rises to 70°C, add dropwise the hydrogen peroxide with a mass concentration of 30% in the reaction system, and the dropwise addition time is 1 hour, and continue the reaction for 2 hours after the dropwise addition is completed Hour, the mol ratio of described hydrogen peroxide and cyclohexanone is 1.75: 1.

[0025] The third step: after the reaction is completed, the Ti-MSE molecular sieve catalyst is separated according to the conventional filtration method, and then according to the conventional distillation operation, the separated product is cyclohexanone oxim...

Embodiment 3

[0027] The first step: sequentially add cyclohexanone and Ti-MSE molecular sieves, tert-butanol and ammonia water with a mass concentration of 25% into the reactor, and stir evenly to obtain a reaction system. In the reaction system, cyclohexanone and Ti-MSE molecules and The weight ratio of tert-butanol is 1:0.05:5, and the mol ratio of cyclohexanone and ammoniacal liquor is 1:1.75.

[0028] The second step: when the reaction temperature of the reaction system of the first step rose to 75°C, the hydrogen peroxide whose mass concentration was 30% was added dropwise to the reaction system for 1.5 hours, and the reaction was continued for 1.5 hours after the addition was completed. Hour, the mol ratio of described hydrogen peroxide and cyclohexanone is 1.75: 1.

[0029] The third step: After the reaction is completed, the Ti-MSE molecular sieve catalyst is separated according to the conventional filtration method, and then according to the conventional distillation operation, th...

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 preparing oxime. The method is characterized in that catalytic reaction for oxime synthesis is performed by using a titanium silicate molecular sieve of a MSE topological structure as a catalyst and using ketone or aldehyde, ammonia and hydrogen peroxide as a reaction system, wherein in the reaction system, the weight ratio of ketone or aldehyde to the catalystto a solvent is 1:(0.03 to 0.15):(1 to 15); the molar ratio of the ketone or aldehyde to the ammonia is 1:(1 to 4); the catalyst is Ti-MSE or a combination body of Ti-MSE and silicon dioxide or a titanium-containing molecular sieve. Compared with the prior art, the method has the advantages that the selectivity is high; the catalytic activity is high; the aftertreatment is simple and convenient;the conversion rate of reactants of ketone or aldehyde reaches up to 99 percent; the product oxime selectivity reaches up to 99 percent, so that the molecular sieve shows excellent catalytic activityin the specific catalysis field; the application field of the molecular sieve is expanded; a novel and environment-friendly ammoxidation oxime preparation path is provided; certain industrial popularization and application prospects and prominent economic values are realized.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing oxime by using titanium-silicon molecular sieve as a catalyst and using ketone or aldehyde, ammonia and hydrogen peroxide as a reaction system. Background technique [0002] Oxime is a fine chemical with a wide range of uses, such as cyclohexanone oxime, which is used as a chemical intermediate for the synthesis of nylon-6 and nylon-66 and other basic raw materials for engineering plastics-caprolactam; butanone oxime, as an antioxidant for paint And anti-skinning agent is used for skinning treatment of polyurethane paint and various alkyd resin paints during storage; acetone oxime is used as an oxygen scavenger for deoxidation of thermal boiler water; acetaldehyde oxime is an important pharmaceutical and pesticide intermediate. [0003] At present, oxime is mainly synthesized by reacting hydroxylamine salt with ketone or aldehyde. This pr...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/44C07C251/38C07D307/52
CPCC07C249/04C07C251/44C07C2601/14C07D307/52C07C251/38
Inventor 吴鹏卢信清徐浩颜佳颖殷剑雍何鸣元
Owner EAST CHINA NORMAL UNIV
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