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Method for efficient hydrodechlorination purification of trichlorobenzene

A technology for hydrodechlorination and trichlorobenzene, which is applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry and other directions, can solve the problems of difficult control of isomer impurities and difficult to obtain high-purity products, and achieves high selectivity, high The effect of reducing equipment investment, simple and efficient process

Inactive Publication Date: 2019-09-06
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to solve the disadvantages that high-purity products are not easy to obtain and isomer impurities are difficult to control in the refined 1,2,4-trichlorobenzene in the prior art, and a method for purifying 1,2,4-trichlorobenzene is provided. The method has the characteristics of simple and efficient process, easy operation, good atom economy, high product purity, etc., which is beneficial to remove the isomers in 1,2,4-trichlorobenzene, thereby improving 1,2,4-trichlorobenzene Benzene purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 400g of 1,2,4-trichlorobenzene containing isomers (isomer content of 1%, 1,2,4-trichlorobenzene content of 99%) into a 1 liter autoclave, and add 5% by weight 35.3g of sodium hydroxide aqueous solution and palladium-carbon catalyst. After nitrogen replacement, the temperature is increased to 120°C, the stirring is turned on, 0.5MPa hydrogen pressure is kept for 2 hours, and the temperature is lowered to below 30°C. The reaction solution is filtered, the filtrate is separated into layers, and the lower oil layer is distilled. Removal of low-chlorinated aromatic hydrocarbons, collecting 1,2,4-trichlorobenzene fractions, gas chromatography analysis content of 99.95%.

Embodiment 2

[0028] Put 400g of 1,2,4-trichlorobenzene containing isomers (0.1% of isomer content, 99.9% of 1,2,4-trichlorobenzene content) into a 1-liter autoclave, and add the concentration of 0.1wt% 88.2g of sodium hydroxide aqueous solution and palladium-carbon catalyst. After nitrogen replacement, the temperature was raised to 80°C, the stirring was turned on, the reaction was kept at 1MPa hydrogen pressure for 0.5hr, and the temperature was lowered to below 30°C. The reaction solution was filtered, the filtrate was separated into layers, and the lower oil layer was distilled. Removal of low-chlorinated aromatic hydrocarbons, collecting 1,2,4-trichlorobenzene fraction, gas chromatography analysis content of 99.96%.

Embodiment 3

[0030] Put 400g of 1,2,4-trichlorobenzene containing isomers (isomer content 2%, 1,2,4-trichlorobenzene content 98%) into a 1 liter autoclave, and add 10wt% 52.9g of sodium hydroxide aqueous solution and palladium-carbon catalyst. After nitrogen replacement, the temperature is raised to 120°C, stirring is turned on, the reaction is performed under 1.5MPa hydrogen pressure for 3.5 hours, and the temperature is lowered to below 30°C. The reaction solution is filtered, the filtrate is separated into layers, and the lower oil layer is distilled to remove Low-chlorinated aromatic hydrocarbons, collected 1,2,4-trichlorobenzene fraction, gas chromatography analysis content of 99.93%.

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Abstract

The invention belongs to the technical field of petrochemical engineering, and relates to the technical field of organic compound purification in the field of fine chemical engineering, in particularto a method for purifying 1,2,4-trichlorobenzene. The method for purifying 1,2,4-trichlorobenzene solves the technical problems that in the prior art, a high purity product of refined 1,2,4-trichlorobenzene is not obtained easily, and isomerization impurities are hard to control. The method has the advantages of being simple and efficient, easy to implement, good in atom economy, high in product purity and the like, isomerization in 1,2,4-trichlorobenzene is removed, and therefore the purity of 1,2,4-trichlorobenzene is improved. According to the technical scheme of the method for efficient hydrodechlorination purification of trichlorobenzene, the isomerization in 1,2,4-trichlorobenzene is converted into low-aryl chloride with the low boiling point, and 1,2,4-trichlorobenzene with the purity larger than 99.9% is obtained through distillation separation.

Description

Technical field [0001] The invention belongs to the technical field of petrochemical industry, and also relates to the technical field of organic compound purification in the field of fine chemical industry, especially a method for purifying 1,2,4-trichlorobenzene. Background technique [0002] 1,2,4-Trichlorobenzene is an important fine organic intermediate, which is widely used in the fields of medicine, pesticides, dyes, and additives. In recent years, the development of its downstream products has gradually emerged at home and abroad, and the market demand is large, especially the content is greater than 99.5%, and the isomer impurities (1,3,5-trichlorobenzene and 1,2,3-trichlorobenzene) are less than The demand for 0.1% high-purity 1,2,4-trichlorobenzene is increasing. [0003] At present, the conventional production method of 1,2,4-trichlorobenzene is benzene chlorination. In this process, the isomers 1,3,5-trichlorobenzene and 1,2,3-trichlorobenzene are generated. Conventi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/395C07C17/383C07C25/10
CPCC07C17/395C07C17/383
Inventor 王根林戚明甫丁克鸿徐林殷恒志刘鑫王铖王刚许越刘相李刘洁郭玉秀
Owner JIANGSU YANGNONG CHEM GROUP
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