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A kind of preparation method of hexachloroacetone

A technology of hexachloroacetone and acetone, applied in the field of organic chemical gas preparation, can solve problems such as difficulty in recovery and difficulty in obtaining high-purity hexachloroacetone, and achieve the effects of easy recovery and high yield

Active Publication Date: 2022-01-21
派瑞科技有限公司
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  • 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

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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...

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PUM

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Abstract

The invention relates to a preparation method of hexachloroacetone, which belongs to the technical field of organic chemical gas preparation. Compound A and chlorine molecule B are mixed and reacted at 30°C to 150°C under the action of a catalyst, and the reaction product is a mixture containing hexachloroacetone and the catalyst; the catalyst is separated from the mixture to obtain a crude product; the crude product is purified to obtain Hexachloroacetone; compound A is at least one of acetone and chloroacetone with chlorine atoms of 1 to 5; chlorine molecule B is a mixture of chlorine or chlorine and a diluent gas, and the diluent gas is an inert gas or nitrogen; the catalyst is pyrimidine, 2-chloropyrimidine, 2-cyanopyrimidine or s-triazine. The method is easy to recover the catalyst, and can obtain the hexachloroacetone with extremely low impurity content in high yield.

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

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Application Information

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Patent Type & Authority Patents(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 派瑞科技有限公司
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