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2,4-dichlorobenzotrifluoride preparation method

A technology of dichlorobenzotrifluoride and dichlorotrichlorotoluene, which is applied in the field of preparation of pesticide chemical intermediate products, can solve the problems of high cost, principle, and route without breaking through the step-by-step reaction method, and achieve low equipment corrosion and social Significant benefit and high product yield

Inactive Publication Date: 2020-01-07
JIANGSU FENGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is costly and will produce a mixture of 2,4-dichlorotoluene and 3,4-dichlorotoluene, and the principle and route have not broken through the step-by-step reaction method

Method used

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  • 2,4-dichlorobenzotrifluoride preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Chlorination: put 800g of 2,4-dichlorotoluene into a 3L reactor, raise the temperature to 115°C, add 40g of catalyst, and start to feed the flow at 40-80 m 3 / h of dry chlorine, the temperature is controlled at 115-117°C, and the reaction time is 24 hours. When the content of 2,4-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 2,4-dichlorotrichloride Chlorotoluene.

[0032] (2) Fluorination: Press 4 moles of 2,4-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 1.5-1.7MP...

Embodiment 2

[0036] (1) Chlorination: Put 800g of 2,4-dichlorotoluene into a 3L reactor, raise the temperature to 115°C, add 80g of catalyst, and start to feed the flow at 40-80 m 3 / h of dry chlorine gas, the temperature is controlled at 120-125°C, and the reaction time is 22 hours. When the content of 2,4-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 2,4-dichlorotrichloride Chlorotoluene.

[0037] (2) Fluorination: Press 4 moles of 2,4-dichlorobenzotrichloride and 14 moles of anhydrous hydrogen fluoride into a 3L reactor, and check the opening status of each valve. Turn on stirring, slowly feed steam into the jacket, and when the pressure in the kettle reaches 1.5MPa, open the exhaust valve to exhaust, continue to heat up until the temperature in the kettle is 115°C, and control the pressure in the kettle to 2.2-2.5MPa at the sa...

Embodiment 3

[0041] (1) Chlorination: put 800g of 2,4-dichlorotoluene into a 3L reactor, raise the temperature to 115°C, add 60g of catalyst, and start to feed the flow at 40-80 m 3 / h of dry chlorine gas, the temperature is controlled at 115-120°C, and the reaction time is 20 hours. When the content of 2,4-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 2,4-dichlorotrichloride Chlorotoluene.

[0042] (2) Fluorination: Press 4 moles of 2,4-dichlorotrichlorotoluene and 13 moles of anhydrous hydrogen fluoride into a 3L reactor, and check the opening status of each valve. Turn on stirring, slowly feed steam into the jacket, and when the pressure in the kettle reaches 1.5MPa, open the exhaust valve to exhaust, and continue to heat up until the temperature in the kettle is 110°C, and at the same time control the pressure in the kettle to ...

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Abstract

The invention discloses a 2,4-dichlorobenzotrifluoridepreparation method, wherein the target compound is obtained by using 2,4-dichlorotoluene as a raw material and using a mixture of cuprous chlorideand copper powder as a catalyst through a two-step reaction of chlorination and fluorination. Compared with the method in the prior art, the method of the invention has the following advantages thatthe chlorination side reactions are less, the isomer of 2,4-dichlorobenzotrifluoride cannot be generated in the reaction process, the product purity is high, the raw material sources are wide, the catalyst is low in price and convenient to recover, the production cost of the target compound is reduced, the economic benefit is increased, and environment pollution cannot be generated.

Description

technical field [0001] The invention relates to a preparation method of a pesticide chemical intermediate product, in particular to a preparation method of 2,4-dichlorobenzotrifluoride. The method is suitable for the occasion of using 2,4-dichlorotoluene as raw material to synthesize 2,4-dichlorobenzotrifluoride through two steps of chlorination and fluorination. Background technique [0002] 2,4-Dichlorobenzotrifluoride is a colorless liquid with a specific gravity of 1.484, a boiling point of 117-118°C, a flash point of 72°C, a refractive index of 1.4802, and a relative density of 1.484. Insoluble in water, miscible with ethanol and ether. 2,4-Dichlorotrifluorotoluene is an important intermediate in organic synthesis. The fluorine atom in its molecular structure makes it have special activity. It is widely used in fine organic synthesis fields such as medicine, pesticide, and dye. Among them, it can be used as a raw material for the upland herbicide dichloramine in pesti...

Claims

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Application Information

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IPC IPC(8): C07C17/20C07C25/13
CPCC07C17/14C07C17/20C07C25/02C07C25/13Y02P20/584
Inventor 郑龙生方东张亮李付香
Owner JIANGSU FENGHUA CHEM IND
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