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Method for preparing 2,4-dichlorophenol by microreactor

A technology of dichlorophenol and microreactor, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long production cycle, high operating cost, low efficiency, etc., and achieve low production cost, continuous The effect of simple preparation and process

Inactive Publication Date: 2018-11-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcoming of long production cycle, low efficiency and high operating cost of batch reactor, and utilize the advantages of microreactor in organic synthesis to provide a method for continuously preparing 2,4-dichlorophenol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Prepare a solution of 2,4-dichlorophenol and carbon tetrachloride at a weight ratio of 1:1, mix evenly, pump the phenol solution into a micro-mixer with a channel inner diameter of 200 μm and mix it with the chlorine gas introduced, the residence time 0.03s, the molar ratio of phenol to chlorine is 1:2, the reaction mixture enters the microchannel reaction tube with an inner diameter of 1000μm (purchased from Nanjing Wanqing Industrial Co., Ltd.) and stays for 500s. The temperature of the constant temperature water bath is 60℃. The reaction product is obtained after distilling off the solvent of the product. The purity of the product by gas chromatography analysis was 91%. The tail gas is absorbed with water to obtain dilute hydrochloric acid.

Embodiment 2

[0021] Prepare a solution of 2,4-dichlorophenol and 1,2-dichloroethane at a weight ratio of 1:2, mix evenly, pump the phenol solution into a micro-mixer with a channel inner diameter of 150 μm and feed in chlorine gas Mixing, the residence time is 0.05s, the molar ratio of phenol to chlorine is 1:2.1, the reaction mixture enters the microchannel reaction tube with an inner diameter of 500μm and stays for 200s, the temperature of the constant temperature water bath is 70°C, and the collected product is distilled out of the solvent That is, the reaction product is obtained. The purity of the product by gas chromatography analysis was 93%. The tail gas is absorbed with water to obtain dilute hydrochloric acid.

Embodiment 3

[0023] Prepare a solution of 2,4-dichlorophenol and dichloromethane at a weight ratio of 1.5:1, mix evenly, pump the phenol solution into a micro-mixer with a channel inner diameter of 500 μm and mix it with chlorine gas, and the residence time is 0.1s, the molar ratio of phenol to chlorine is 1:2.2, the reaction mixture enters the microchannel reaction tube with an inner diameter of 800μm and stays for 500s, the temperature of the constant temperature water bath is 55°C, and the collected product is distilled out of the solvent to obtain the reaction product. The purity of the product by gas chromatography analysis was 90%. The tail gas is absorbed with water to obtain dilute hydrochloric acid.

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Abstract

The invention relates to a method for preparing 2,4-dichlorophenol by a microreactor. Phenol is dissolved into a solvent, and is pumped into a miniature mixer to be mixed with introduced chlorine gas;the mixed material is then introduced into a micro passage reaction tube for continuous reaction to obtain a reaction mixture; tail gas is absorbed by water to prepare diluted hydrochloric acid. Thesolvent in the reaction mixture is distilled and recovered to obtain a reaction product. The method has the advantages that the advantages of the miniature reactor in an aspect of heat transfer and mass transfer are utilized; the catalyst addition is not needed; the continuous preparation of 2,4-dichlorophenol can be realized in short time; the advantages of low device cost, continuous and controllable process, high product purity, easy realization of industrialization and the like are realized.

Description

technical field [0001] The invention relates to a method for preparing 2,4-dichlorophenol by using a microreactor, in particular to a method for rapidly and continuously preparing 2,4-dichlorophenol by using a microreactor, and belongs to the field of organic synthesis. Background technique [0002] 2,4-Dichlorophenol is an important organic chemical intermediate widely used in the synthesis of pesticides, medicines and fungicides. In my country, 2,4-dichlorophenol is mainly used in the production of dichlorophenoxyacid and its ester herbicides, of which 2,4-dichlorophenoxyacetic acid (2,4-D) is the most produced. [0003] The production methods of 2,4-dichlorophenol include phenol direct chlorination method, mixed phenol chlorination method, p-chlorophenol chlorination method and phenol catalytic chlorination method. At present, 2,4-dichlorophenol is the most used in China. The most common industrial production method is the direct chlorination of phenol. In this method, ...

Claims

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Application Information

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IPC IPC(8): C07C37/62C07C39/30
CPCC07C37/62C07C39/30
Inventor 谢天明田先国董天雷殷惠琴贺健
Owner CHINA PETROLEUM & CHEM CORP
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