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

Method for synthesizing ketoxime

A technology for synthesizing ketoxime and materials, applied in oxime preparation, organic chemistry, etc., can solve the problems of gas-liquid-solid heterogeneous mass transfer and heat transfer, many side reactions in a series, poor product selectivity, etc., to avoid pollution and separation problems, improved reaction efficiency, and short residence time

Inactive Publication Date: 2019-12-20
CHEM TECH ACAD OF SHANDONG PROVINCE
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] To sum up, the ammoximation process currently has the following problems: (1) There is a problem of difficult gas-liquid-solid heterogeneous mass transfer and heat transfer in the solvent-free oximation reaction; (2) There is further deep oxidation of the oxime during the oximation process, A series of side reactions are many, there are nitroalkane by-products, and the product selectivity is poor

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for synthesizing ketoxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] First, raise the temperature of the temperature control system to 50°C, then feed material A butanone and catalyst, material B ammonia, and material C hydrogen peroxide into the tubular reactor. The feed is 1% of the amount of ketone, the feed rate of ammonia and hydrogen peroxide is controlled by pH 9, the pressure of the back pressure valve is adjusted to 0.1MPa, the residence time of the feed is 2min, after the feed is stable for 30min, the reaction is quenched by sampling, and the organic phase is analyzed and water content. Based on 100 g of ketone feed, the weight of the organic phase is 125.3 g, the conversion of ketone is 98.57%, and the selectivity is 99.9%.

Embodiment 2

[0025] First, raise the temperature of the temperature control system to 80°C, then feed three strands of material A, acetone and catalyst, material B ammonia, and material C hydrogen peroxide into the tubular reactor. 10% of the amount of ketone, the feed rate of ammonia and hydrogen peroxide is controlled by pH 10, the pressure of the back pressure valve is adjusted to 0.6MPa, the residence time of the material is 15min, after the feed is stable for 30min, the reaction is quenched by sampling, and the organic phase and Aqueous phase product content. Based on 100 g of ketone feed, the weight of the organic phase is 127.8 g, the conversion of ketone is 96.91%, and the selectivity is 99.7%.

Embodiment 3

[0027] First, raise the temperature of the temperature control system to 70°C, then feed three strands of material A butanone and catalyst, material B ammonia, and material C hydrogen peroxide into the tubular reactor. The feed is 10% of the amount of ketone, the feed rate of ammonia and hydrogen peroxide is controlled by pH 12, the pressure of the back pressure valve is adjusted to 0.1MPa, the residence time of the feed is 10min, after the feed is stable for 30min, the reaction is quenched by sampling, and the organic phase is analyzed and aqueous product content. Based on 100 g of ketone feed, the weight of the organic phase is 126.4 g, the conversion of ketone is 99%, and the selectivity is 99.2%.

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 relates to the field of organic synthesis processes, particularly to a method for synthesizing ketoxime, wherein ketoxime is prepared by using ketone, ammonia and hydrogen peroxide as raw materials in an internal spiral tubular reactor under the catalysis of a titanium-silicon molecular sieve. Compared with the traditional method for preparing ketoxime, the method of the present invention has the following advantages that the mass and heat transfer of materials is easily achieved so as to improve the reaction efficiency, the plug flow and the full mixed flow are combined to effectively reduce the generation of side reactions and improve the product selectivity, and the water-phase reaction system is adopted so as to avoid the problems of pollution and separation of traditional amidoxime chemical industry organic solvents.

Description

technical field [0001] The invention relates to the field of organic synthesis technology, in particular to a method for synthesizing ketoxime. Background technique [0002] The traditional ketoxime is prepared by reacting hydroxylamine salt with the corresponding ketone, which has problems such as low utilization rate of raw materials, large discharge of three wastes, and serious environmental pollution. After TS-1 titanium silicon molecular sieve was synthesized in the laboratory, cyclohexanone oxime was directly synthesized from titanium silicon molecular sieve using cyclohexanone, ammonia and hydrogen peroxide as raw materials. In 2004, Sinopec Petrochemical Research Institute and Baling Branch jointly carried out the project of "Complete New Technology for Synthesis of Cyclohexanone Oxime in Single Tank Continuous Slurry Bed". The new process of cyclohexanone ammoximation simplifies the production process, reduces the production cost, and has mild reaction conditions a...

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): C07C249/04C07C251/38C07C251/44
CPCC07C249/04C07C2601/14C07C251/38C07C251/44
Inventor 刘启奎岳涛杨旭卢福军陈贵军冯维春
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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