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Efficient chlorination process of 3,4-dichlorobenzotrifluoride

A technology of dichlorotrifluorotoluene and dichlorotrichlorotoluene is applied in the field of preparation of pesticide chemical intermediate products, which can solve problems such as inventory backlog, and achieve the effects of less equipment corrosion, lower production costs, and no environmental pollution.

Inactive Publication Date: 2019-11-22
JIANGSU DAHUA CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] At present, a large amount of by-product 3,4-dichlorotoluene is produced during the production of 2,4-dichlorotoluene in China, resulting in a serious inventory backlog

Method used

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  • Efficient chlorination process of 3,4-dichlorobenzotrifluoride

Examples

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Embodiment 1

[0034] (1) Chlorination: Put 800g of 3,4-dichlorotoluene into a 3L reactor, raise the temperature to 115°C, add 40g of catalyst, and start to feed dry chlorine gas with a flow rate of 40-80 m3 / h, and control the temperature at 115-117°C , The reaction time is 24 hours. When the content of 3,4-dichlorodichlorotoluene is less than 0.5%, stop feeding chlorine gas, and change into dry air to discharge unreacted chlorine gas, hydrogen chloride gas and gas impurities produced by the reaction to obtain 3,4-dichlorotrichloride Chlorotoluene.

[0035] (2) Fluorination: Press 4 moles of 3,4-dichlorobenzotrichloride and 12 moles of anhydrous hydrogen fluoride into a 3L reactor, and check the opening status of each valve. Turn on the stirring, slowly feed steam into the jacket, and when the pressure in the kettle reaches 1.5MPa, open the tail gas discharge valve to exhaust, continue to heat up until the temperature in the kettle is 110°C, and control the pressure in the kettle at 1.5-1.7...

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Abstract

The invention discloses an efficient chlorination process of 3,4-dichlorobenzotrifluoride, and belongs to the field of organic synthesis. According to the method, 3,4-dichlorotoluene is used as a rawmaterial, a mixture catalyst of cuprous chloride and copper powder is added, a target compound is obtained through two-step reaction of chlorination and fluorination, the raw materials applied in thereaction process are convenient to purchase, the production cost is low, after-treatment is simple, reaction conditions are mild, and good economic benefits and social benefits are achieved.

Description

technical field [0001] The invention relates to a preparation method of a pesticide chemical intermediate product, which is suitable for the occasion of synthesizing 3,4-dichlorobenzotrifluoride through two steps of chlorination and fluorination by using 3,4-dichlorotoluene as a raw material. Background technique [0002] 3,4-Dichlorobenzotrifluoride (3,4-Dichlorobenzotrifluoride) is a colorless transparent liquid with a halogenated benzene odor. Insoluble in water, miscible with benzene, toluene, ethanol, ether, halogenated hydrocarbons, etc. It is an important organic synthesis intermediate. The fluorine atom in the molecular structure makes it have special activity. It is widely used in fine organic synthesis fields such as medicine, pesticide and dye. Among them, synthetic diphenyl ether herbicides are the most used at present, such as lactofen, fomesafen, acefluorfen, dichlorofluorfen, ethoxyfluorfen, chlorofluorfen, Acifluorfen, flunafenate, flufenate, HC-252, SN1062...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/13C07C17/20C07C17/383C07C17/14C07C25/02
CPCC07C17/14C07C17/206C07C17/383C07C25/02C07C25/13
Inventor 郑龙洲方东张亮李付香
Owner JIANGSU DAHUA CHEM IND
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