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Recycling of 2, 4-dichloroacetophenone isomer 2, 6-dichloroacetophenone

A technology for dichloroacetophenone and isomers, which is applied in the field of recycling and utilization of 2,4-dichloroacetophenone isomer 2,6-dichloroacetophenone, can solve the problem of ineffective treatment of by-products, Resource waste and other problems, to achieve the effect of improving effective utilization, saving production costs, and convenient operation

Active Publication Date: 2021-08-27
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In view of this, the present invention provides the recycling of 2,4-dichloroacetophenone isomer 2,6-dichloroacetophenone, to solve 2,4-dichloroacetophenone production process in the prior art There is no effective treatment of by-products and the problem of

Method used

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  • Recycling of 2, 4-dichloroacetophenone isomer 2, 6-dichloroacetophenone
  • Recycling of 2, 4-dichloroacetophenone isomer 2, 6-dichloroacetophenone
  • Recycling of 2, 4-dichloroacetophenone isomer 2, 6-dichloroacetophenone

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Embodiment 1

[0028] Recovery and Utilization of 2,4-Dichloroacetophenone Isomer 2,6-Dichloroacetophenone

[0029] 500g of the tower bottom residue containing 2,6-dichloroacetophenone was distilled and then pumped into the autoclave. The tower bottom residue included 5.3g of 2,4-dichloroacetophenone, 2,6-dichlorobenzene 472g of ethyl ketone, the rest is other impurities; then add 14g of sodium hydroxide and 28g of deionized water; close the autoclave, start stirring, inject high-pressure air, keep the pressure at 1.2MPa, then raise the temperature to 200°C, and the system pressure will naturally increase to 3.5MPa, keep warm at this temperature and pressure for 3 hours, then cool down to 30°C, and when the system pressure drops to 1.2MPa, open the vent valve and stop stirring; after the reaction system is left to stand for half an hour, separate the lower organic phase to obtain m-dichlorobenzene crude product; the m-dichlorobenzene crude product is washed once with 200g concentration of 3%...

Embodiment 2

[0032] Recovery and Utilization of 2,4-Dichloroacetophenone Isomer 2,6-Dichloroacetophenone

[0033] 500g of the tower bottom residue containing 2,6-dichloroacetophenone was distilled and then pumped into the autoclave. The tower bottom residue included 7.6g of 2,4-dichloroacetophenone, 2,6-dichlorobenzene 472.6g of ethyl ketone, the rest is other impurities; then add 15g of sodium hydroxide and 30g of deionized water; close the autoclave, start stirring, inject high-pressure air, keep the pressure at 1.3MPa, and then raise the temperature to 220°C, the system pressure will naturally increase to 4MPa, keep warm at this temperature and pressure for 3 hours, then cool down to 35°C, and when the system pressure drops to 1.3MPa, open the vent valve and stop stirring; after leaving the reaction system for half an hour, separate the lower organic phase to obtain m-dichlorobenzene crude product; the m-dichlorobenzene crude product is washed once with 200g concentration of 3% hydrochl...

Embodiment 3

[0036] Recovery and Utilization of 2,4-Dichloroacetophenone Isomer 2,6-Dichloroacetophenone

[0037] 500g of the tower bottom residue containing 2,6-dichloroacetophenone was distilled and then pumped into the autoclave. The tower bottom residue included 2.8g of 2,4-dichloroacetophenone, 2,6-dichlorobenzene 478g of ethyl ketone, the remaining is other impurities; then add 16g of sodium hydroxide and 28g of deionized water; close the autoclave, start stirring, inject high-pressure air, keep the pressure at 1.5MPa, then raise the temperature to 250°C, and the system pressure will naturally increase to 4.5MPa, keep warm at this temperature and pressure for 3 hours, then cool down to 40°C, and when the system pressure drops to 1.5MPa, open the vent valve and stop stirring; after leaving the reaction system for half an hour, separate the lower organic phase to obtain m-dichlorobenzene crude product; the m-dichlorobenzene crude product is washed once with 200g concentration of 3% hyd...

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Abstract

The invention discloses recycling of 2, 4-dichloroacetophenone isomer 2, 6-dichloroacetophenone. Recycling comprises the following steps: distilling tower kettle residues containing 2, 6-dichloroacetophenone, pumping the residues into a high-pressure kettle, adding sodium hydroxide and deionized water, and carrying out high-pressure decomposition and layering to obtain an m-dichlorobenzene crude product; washing the m-dichlorobenzene crude product to obtain an m-dichlorobenzene product; and recycling and reusing the m-dichlorobenzene product. The recycling process is simple, the equipment investment is low, operation is convenient, the content of the recycled product is high, the resource waste is avoided, and the production cost is greatly reduced.

Description

technical field [0001] The invention relates to the field of organic synthetic chemistry, in particular to the recovery and utilization of 2,4-dichloroacetophenone isomer 2,6-dichloroacetophenone. Background technique [0002] 2,4-dichloroacetophenone is an important fine chemical intermediate, it is the raw material for the preparation of ω-bromo-2,4-dichloroacetophenone or ω-2,4-trichloroacetophenone, It is mainly used in the synthesis of fungicides such as imazalil, propiconazole, and etheconazole, as well as the insecticide chlorpyramid, and the herbicide Verticillium, and has a wide range of applications in the fields of medicine and pesticides. [0003] At present, the synthesis of 2,4-dichloroacetophenone adopts m-dichlorobenzene as a raw material, uses acetyl chloride as an acylating agent in a cyclohexane solution, and aluminum trichloride as a catalyst, and obtains 2 through Fridel-Crafts acylation. , the crude product of 4-dichloroacetophenone, after the reaction...

Claims

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Application Information

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IPC IPC(8): C07C17/361C07C17/383C07C25/08
CPCC07C17/361C07C17/383C07C25/08
Inventor 王进廖道华祁康旭徐瑶潘光飞曾挺
Owner 浙江禾本科技股份有限公司