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Method for preparing 2, 5-dichlorophenol through continuous oxidation of p-dichlorobenzene

A technology for p-dichlorobenzene and dichlorophenol, which is applied in the field of producing 2,5-dichlorophenol, can solve problems that have not yet been seen, and achieve the effects of avoiding the phenomenon of flying temperature, maintaining the reaction temperature, and reducing the generation of by-products.

Pending Publication Date: 2020-01-03
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been no technology research and equipment technology reports on the reaction of p-dichlorobenzene to prepare 2,5-dichlorophenol in a continuous microchannel reaction mode. The present invention provides a continuous production of 2,5-dichlorophenol using a microchannel reactor , A new method for 5-dichlorophenol

Method used

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  • Method for preparing 2, 5-dichlorophenol through continuous oxidation of p-dichlorobenzene
  • Method for preparing 2, 5-dichlorophenol through continuous oxidation of p-dichlorobenzene
  • Method for preparing 2, 5-dichlorophenol through continuous oxidation of p-dichlorobenzene

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Effect test

Embodiment 1

[0026] (1) Device: continuous flow microchannel reaction device (3a+3a), refer to figure 2 Determine the connection mode of the microchannel reactor, the length of the microchannel is determined according to the flow rate and the reaction residence time, and the heat transfer medium is heat transfer oil.

[0027] (2) Preparation of 2,5-dichlorophenol: adjust the microchannel reaction device to preheating zone, reaction zone and quenching zone according to the needs of the reaction process. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 60s, the preheating temperature and the reaction temperature are set to 50° C., and the reaction pressure is 5 bar. The mixed solution of the substrate p-dichlorobenzene, iron powder and acetic acid is passed through the preheating zone A of the metering pump 1 input device, and the hydrogen peroxide with a mass fraction of 10% is passed through the preheat...

Embodiment 2

[0029] (1) Device: continuous flow microchannel reaction device (3a+3b), refer to figure 2 Determine the connection mode of the microchannel reactor, the length of the microchannel is determined according to the flow rate and the reaction residence time, and the heat transfer medium is heat transfer oil.

[0030] (2) Preparation of 2,5-dichlorophenol: adjust the microchannel reaction device to preheating zone, reaction zone and quenching zone according to the needs of the reaction process. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 90s, the preheating temperature and the reaction temperature are set to 70° C., and the reaction pressure is 7 bar. The mixed solution of the substrate p-dichlorobenzene, ferric oxide and acetic acid is passed through the preheating zone A of the metering pump 1 input device, and the mass fraction is 20% hydrogen peroxide is passed through the preheating ...

Embodiment 3

[0032] (1) Device: continuous flow microchannel reaction device (3a+3c), refer to figure 2 Determine the connection mode of the microchannel reactor, the length of the microchannel is determined according to the flow rate and the reaction residence time, and the heat transfer medium is heat transfer oil.

[0033] (2) Preparation of 2,5-dichlorophenol: adjust the microchannel reaction device to preheating zone, reaction zone and quenching zone according to the needs of the reaction process. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 120s, the preheating temperature and the reaction temperature are set to 90° C., and the reaction pressure is 8 bar. The mixed solution of substrate p-dichlorobenzene, ferroferric oxide and acetonitrile is passed through the preheating zone A of the metering pump 1 input device, and the mass fraction is 30% hydrogen peroxide is passed through the preheati...

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Abstract

The invention discloses a method for preparing 2, 5-dichlorophenol by directly oxidizing p-dichlorobenzene in a micro-channel reactor, and belongs to the field of fine chemical engineering. Accordingto the method, the p-dichlorobenzene is used as a raw material, hydrogen peroxide is used as an oxidant, acetic acid is used as a solvent, and one or more of iron, iron oxide or an iron metal complexis / are used as a catalyst to complete the preparation process of the 2, 5-dichlorophenol in a micro-channel reactor system. According to the method, the temperature and the retention time in the reaction process can be strictly controlled, the accumulation of oxygen is reduced, the reaction temperature is accurately controlled, temperature runaway is prevented, and the safety of a reaction deviceis improved; due to the strong mass transfer effect of the micro-channel reactor, the mass transfer effect among the raw materials in the reaction system is enhanced, and the reaction efficiency is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and specifically relates to a method for preparing 2,5-dichlorophenol by using p-dichlorobenzene as a raw material through liquid-phase oxidation reaction, more specifically, using p-dichlorobenzene in a microchannel reactor A method for producing 2,5-dichlorophenol by using benzene as a raw material through a liquid-phase oxidation reaction. Background technique [0002] 2,5-Dichlorophenol is an important chemical organic intermediate, which is widely used in medicine, pesticide and other fields, especially the important organic intermediate for the preparation of pesticide herbicide dicamba. At present, the methods commonly used in industry to prepare 2,5-dichlorophenol include 1,2,4-trichlorobenzene hydrolysis method and 2,5-dichloroaniline diazo hydrolysis method. These two preparation methods consume a lot of acid, severely corrode equipment, and produce a large amount ...

Claims

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Application Information

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IPC IPC(8): C07C37/60C07C39/30B01J19/00
CPCC07C37/60B01J19/0093C07C39/30
Inventor 刘建武廖阳群张跃严生虎沈介发辜顺林马晓明陈代祥
Owner CHANGZHOU UNIV
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