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A kind of purification method of hexachloroacetone

A technology of hexachloroacetone and purification method, which is applied in the field of purification of hexachloroacetone, can solve the problems of low purity of hexachloroacetone, high content of pentachloroacetone, and difficulty in separation, and achieve low heating temperature, simple operation and low impurity content low effect

Active Publication Date: 2022-01-21
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Hexachloroacetone is a commonly used chemical raw material, which is mainly used in pesticide intermediates and pharmaceutical industries. Hexachloroacetone is mainly obtained by direct chlorination of acetone. The production principle is simple, but non-ideal low-boiling products will be produced during the production process. It is tetrachloroacetone and pentachloroacetone, especially pentachloroacetone has a large content and is difficult to separate
In the prior art, distillation and rectification under reduced pressure are used as purification means to purify, but the purity of hexachloroacetone after purification is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A method for purifying hexachloroacetone, the method steps are as follows:

[0021] At 8.7KPa, the crude hexachloroacetone solution is heated to 50°C by a heater, passed into the top of the purification tower, and sprayed to the bottom of the tower in a mist form from the top of the purification tower through the atomizer; the nitrogen is heated by the heater to 40°C, from the lower part of the purification tower into the purification tower; the atomized crude hexachloroacetone solution sprayed from top to bottom and the nitrogen flowing from bottom to top carry out convective interactive contact purification and heat exchange, nitrogen will bring low boiling point impurities out.

[0022] Nitrogen with low boiling point impurities is collected from the outlet of the purification tower and passed through the condenser, cooled to 20°C, and then passed into the gas-liquid separator. The low boiling point impurities are separated from the gas and passed into the low boilin...

Embodiment 2

[0025] A method for purifying hexachloroacetone, the method steps are as follows:

[0026] At 9.0KPa, the crude hexachloroacetone solution is heated to 50°C by a heater, passed into the top of the purification tower, passed through the atomizer from the top of the purification tower, and sprayed to the bottom of the tower in mist; the nitrogen is heated to 55°C, from the lower part of the purification tower into the purification tower; the atomized crude hexachloroacetone solution sprayed from top to bottom and the nitrogen flowing from bottom to top carry out convective interactive contact purification and heat exchange, nitrogen will bring low boiling point impurities out.

[0027] Nitrogen with low boiling point impurities is collected from the outlet of the purification tower through the condenser, cooled to 23°C, and then passed into the gas-liquid separator. The low boiling point impurities are separated from the gas and passed into the low boiling point collection tank ...

Embodiment 3

[0030] A method for purifying hexachloroacetone, the method steps are as follows:

[0031] At 8.5KPa, the crude hexachloroacetone solution is heated to 60°C by a heater, passed into the top of the purification tower, and sprayed to the bottom of the tower in a mist form from the top of the purification tower through the atomizer; the nitrogen is heated to 40°C, from the lower part of the purification tower into the purification tower; the atomized crude hexachloroacetone solution sprayed from top to bottom and the nitrogen flowing from bottom to top carry out convective interactive contact purification and heat exchange, nitrogen will bring low boiling point impurities out.

[0032] Nitrogen with low boiling point impurities is collected from the outlet of the purification tower through the condenser, cooled to 25°C, and then passed into the gas-liquid separator. The low boiling point impurities are separated from the gas and passed into the low boiling point collection tank f...

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Abstract

The invention relates to a method for purifying hexachloroacetone, belonging to the technical field of organic chemical purification. At 8.0KPa ~ 20KPa, after heating the crude hexachloroacetone solution to 45°C ~ 75°C, spray from top to bottom with the purification gas flowing from bottom to top heated to 35°C ~ 75°C for convective interactive contact purification, The low-boiling impurities are separated from the crude hexachloroacetone solution by purifying gas to obtain hexachloroacetone solution; the purifying gas is inert gas or nitrogen; and the low-boiling impurities are mainly pentachloroacetone and tetrachloroacetone. The method has a low material heating temperature, the purified gas can be recycled, the processing capacity can be enlarged, the operation is simple, and hexachloroacetone with extremely low impurity content can be obtained.

Description

technical field [0001] The invention relates to a method for purifying hexachloroacetone, belonging to the technical field of organic chemical purification. Background technique [0002] Hexachloroacetone is a commonly used chemical raw material, which is mainly used in pesticide intermediates and pharmaceutical industries. Hexachloroacetone is mainly obtained by direct chlorination of acetone. The production principle is simple, but non-ideal low-boiling products will be produced during the production process. It is tetrachloroacetone and pentachloroacetone, especially the content of pentachloroacetone is relatively large and difficult to separate. In the prior art, distillation and vacuum distillation are mostly used as purification means to purify, but the purity of hexachloroacetone after purification is not high. Contents of the invention [0003] For overcoming the defective that prior art exists, the object of the present invention is to provide a kind of purificat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/16C07C45/78
Inventor 代伟娜许东海刘晓林陈欢董云峰贾珂苏玲燕
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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