Purification method of hexachloroacetone

A technology of hexachloroacetone and purification method, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve the problems of easy decomposition, high difficulty and high boiling point, and achieve the effects of low operating temperature, long service life and simple operation

Active Publication Date: 2020-08-11
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

Due to the high boiling point of hexachloroacetone, it is easy to decompose and has strong corrosion, so it is very difficult to adopt rectification method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) After drying the spherical 5A molecular sieve with a diameter of 3mm at 200°C for 10h, fill it into an adsorption column with an inner diameter of 60mm and a volume of 1L, and the porosity of the 5A molecular sieve is 40%;

[0019] (2) Keep the temperature of the adsorption column at 0°C, and use a plunger pump to inject crude hexachloroacetone (pentachloroacetone impurity content of 0.5wt%) with a temperature of 0°C into the adsorption column from bottom to top at a flow rate of 5.5mL / min. Column, the flow velocity of hexachloroacetone crude product through adsorption column is 5mm / min, according to 5A molecular sieve to pentachloroacetone and hexachloroacetone adsorption selectivity is different, removes most of pentachloroacetone in hexachloroacetone crude product, obtains high-purity hexachloroacetone Chloroacetone.

[0020] Analysis by gas chromatography shows that the content of pentachloroacetone in the high-purity hexachloroacetone is 0.13wt%.

Embodiment 2

[0022] (1) After drying spherical β-activated alumina with a diameter of 3mm at 200°C for 10h, fill it into an adsorption column with an inner diameter of 60mm and a volume of 1L, and the porosity of β-activated alumina is 40%;

[0023] (2) Keep the temperature of the adsorption column at 0°C, and use a plunger pump to inject crude hexachloroacetone (pentachloroacetone impurity content of 0.5wt%) with a temperature of 0°C into the adsorption column from bottom to top at a flow rate of 5.5mL / min. column, the hexachloroacetone crude product is passed through the flow velocity of the adsorption column as 5mm / min, and according to the different adsorption selectivity of β-activated alumina to pentachloroacetone and hexachloroacetone, most of the pentachloroacetone in the hexachloroacetone crude product is removed to obtain high Pure hexachloroacetone.

[0024] Analysis by gas chromatography shows that the content of pentachloroacetone in the high-purity hexachloroacetone is 0.18wt...

Embodiment 3

[0026] (1) After drying spherical modified silica gel with a diameter of 3 mm (prepared by equal volume impregnation method, magnesium sulfate load of 5 wt%, drying temperature and time at 150 °C and 10 h) at 200 °C for 10 h, fill it into In a 60mm adsorption column with a volume of 1L, the porosity of the modified silica gel is 40%;

[0027] (2) Keep the temperature of the adsorption column at 0°C, and use a plunger pump to inject crude hexachloroacetone (pentachloroacetone impurity content of 0.5wt%) with a temperature of 0°C into the adsorption column from bottom to top at a flow rate of 5.5mL / min. column, the flow rate of hexachloroacetone crude product through the adsorption column is 5mm / min, according to the different adsorption selectivity of modified silica gel to pentachloroacetone and hexachloroacetone, most of the pentachloroacetone in the crude product of hexachloroacetone is removed to obtain high-purity Hexachloroacetone.

[0028] Analysis by gas chromatography...

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Abstract

The invention relates to a purification method of hexachloroacetone, and belongs to the technical field of organic chemical purification. According to the method, pentachloroacetone impurities in crude hexachloroacetone are removed according to different adsorption selectivity of an adsorbent to pentachloroacetone and hexachloroacetone, so as to obtain hexachloroacetone with the pentachloroacetonecontent being 0.2wt% or below. The method is easy to operate, low in operation temperature, long in service life of the adsorbent and easy to amplify.

Description

technical field [0001] The invention relates to a method for purifying hexachloroacetone, which belongs to the technical field of organic chemical purification. Background technique [0002] Hexachloroacetone is a commonly used fine chemical intermediate, mainly used in medicine, pesticides and organic chemicals. Hexachloroacetone is obtained by direct chlorination of acetone, and many by-products will be generated during the synthesis process, mainly including pentachloroacetone and acetone polycondensation chloride. Among them, the boiling point of acetone polycondensation chloride is close to 300°C, which is quite different from the boiling point of hexachloroacetone at 203°C, and can be removed by vacuum distillation; while pentachloroacetone and hexachloroacetone have similar structures, similar physical and chemical properties, and are difficult to remove . Due to the small difference between the boiling point of pentachloroacetone (192°C) and hexachloroacetone, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/16C07C45/79
CPCC07C45/79C07C49/16
Inventor 许东海刘晓林代伟娜王双超董云峰陈欢王雪鹏郭敬维贾珂耿超
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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