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

Preparation method of hexachloroacetone

A technology of hexachloroacetone and acetone, which is applied in the field of organic chemical gas preparation, and can solve problems such as difficult to obtain high-purity hexachloroacetone and difficult to recycle

Active Publication Date: 2019-06-28
中国船舶集团有限公司第七一八研究所
View PDF7 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopt pyridine, triphenylphosphine as catalyst, catalyst and its chloride are dissolved in the hexachloroacetone product, so it is difficult to recycle and reuse catalyst and its chloride When compound, trace catalyst and its chloride also remain in hexachloroacetone, so it is difficult to obtain high-purity hexachloroacetone

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

[0026] In the 1L glass reactor with stirrer, thermometer, gas inlet tube and condenser, add acetone (moisture content below 0.1%wt) 295g (5mol), stir, then chlorine gas is passed in the acetone with the flow rate of 4g / min, The reactor is kept at 30°C to 40°C with cooling water, and after about 710g (10mol) of chlorine gas is introduced, the cooling water is removed, 20.3g (0.25mol) of pyrimidine is added, and the temperature is automatically raised to 110°C to 120°C by reaction heat. ℃, to about 1775g (25mol) of chlorine gas, then heated up to 140°C to 150°C, to about 2343g (33mol) of chlorine gas, after adding nitrogen gas, purging to remove reaction residual chlorine and hydrogen chloride, the catalyst and the product were separated Finally, the product was isolated, washed three times with water, dried with calcium chloride, and distilled under reduced pressure at 0.1KPa to obtain the final product with a yield of 94.5%.

[0027] The final product was detected by gas chrom...

Embodiment 2

[0029] In the 1L glass reactor with stirrer, thermometer, gas inlet tube and condenser, add acetone (moisture content below 0.1%wt) 295g (5mol), stir, then chlorine gas is passed in the acetone with the flow rate of 4g / min, The reactor is kept at 30°C to 40°C with cooling water, and after about 710g (10mol) of chlorine gas is introduced, the cooling water is removed, 57.3g (0.50mol) of 2-chloropyrimidine is added, and the temperature is automatically raised to 110°C by reaction heat, to After about 1775g (25mol) of chlorine gas is introduced, heat up to 140°C to 150°C, and after about 2812g (39.6mol) of chlorine gas is added, nitrogen gas is introduced to purge to remove residual chlorine and hydrogen chloride, and the catalyst and product are separated and separated The product was washed three times with water, dried with calcium chloride, and distilled under reduced pressure at 0.1KPa to obtain the final product with a yield of 94.1%.

[0030] The final product was detected...

Embodiment 3

[0032] In the 1L glass reactor with stirrer, thermometer, gas inlet tube and condenser, add acetone (moisture content below 0.1%wt) 295g (5mol), stir, then chlorine gas is passed in the acetone with the flow rate of 4g / min, The reactor is kept at 30°C to 40°C with cooling water, and after about 710g (10mol) of chlorine gas is introduced, the cooling water is removed, and 36.8g (0.35mol) of 2-nitrile pyridine is added, and the temperature is raised to 110°C by relying on the heat of reaction. 120°C, to about 1775g (25mol) of chlorine gas, then heat up to 140°C to 150°C, to about 2450g (34.5mol) of chlorine gas, then pass in nitrogen gas to purge residual chlorine and hydrogen chloride, and wait for the catalyst and product to separate Finally, the product was isolated, washed with water three times, dried with calcium chloride, and distilled under reduced pressure at 0.1KPa to obtain the final product with a yield of 93.8%.

[0033] The final product was detected by gas chromat...

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 a preparation method of hexachloroacetone, belonging to the technical field of the preparation of organic chemical gas. The preparation method comprises the following steps: mixing a compound A with a chlorine molecule B, and reacting at 30-150 DEG C under the effect of a catalyst, wherein a reaction product is a mixture containing hexachloroacetone and the catalyst; and separating the catalyst from the mixture, so as to obtain a crude product; purifying the crude product, so as to obtain hexachloroacetone, wherein the compound A is at least one of acetone and chloroacetone with the chlorine atomic number of 1-5, the chlorine molecule B is chlorine or a mixture of chlorine and diluent gas, the diluent gas is inert gas or nitrogen, and the catalyst is pyrimidine, 2-chloropyrimidine or symtriazine. The method has the beneficial effects that the catalyst is easily recycled, and hexachloroacetone with extremely low impurity content can be obtained in a high-yield manner.

Description

technical field [0001] The invention relates to a preparation method of hexachloroacetone, which belongs to the technical field of organic chemical gas preparation. Background technique [0002] At present, the preparation method of hexachloroacetone is known in patents US2199934, US2635117, US3265740, JP2015556795, CN2013103226 and CN201580003850. Among them, US2199934, US3265740 and JP2015556795 use pyridine as a catalyst to make acetone react with chlorine molecule B; CN2013103226 uses triphenylphosphine as a catalyst to make acetone react with chlorine molecule B; US2635117 and CN201580003850 use activated carbon as Catalyst, the method that makes acetone and chlorine molecule B react; Said chlorine molecule B is the mixture of chlorine or chlorine and diluent gas, and diluent gas is the gas that does not participate in reaction such as inert gas or nitrogen. Adopt pyridine, triphenylphosphine as catalyst, catalyst and its chloride are dissolved in the hexachloroacetone...

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): C07C49/16C07C45/63
CPCY02P20/584
Inventor 许东海代伟娜刘晓林陈欢董云峰郭大伟王双超柴小丽
Owner 中国船舶集团有限公司第七一八研究所
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