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A kind of method that carries out phenolic chlorination reaction in microchannel continuous flow reactor

A chlorination reaction, microchannel technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effects of shortened reaction time, high yield and purity, and reduced energy consumption

Active Publication Date: 2020-11-24
SHANGHAI XIAOMING DETECTION TECH SERVICE CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the prior art, there is no report of carrying out chlorination reaction with a microchannel continuous flow reactor to prepare 2,4-dichlorophenol and 2-methyl 4-chlorophenol. If the microchannel continuous flow reactor can be used for chlorination In the reaction, the yield and efficiency of chlorination can be significantly improved, and the generation of by-products can be reduced

Method used

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  • A kind of method that carries out phenolic chlorination reaction in microchannel continuous flow reactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Embodiment 1: preparation 2,4-dichlorophenol

[0055] (1) the preheating module 1 and the mixed reaction module 2 of the microchannel continuous flow reactor are pressed as follows figure 1 The structures shown are connected in sequence, and the temperature of the circulation system is set to 80°C, so that the reactor reaches a temperature control equilibrium, and the phenol is heated and melted into a liquid;

[0056] (2) Set the flow rate of each raw material metering pump, control the mass flow rate of phenol to 40g / min, control the flow rate of chlorine to 58g / min, make the molar ratio of phenol and chlorine to be 1:2, inject phenol and chlorine into the preheating module 1 respectively preheating in

[0057] (3) phenol and chlorine after preheating enter mixed reaction module 2 simultaneously and carry out mixed reaction, and the control mixed reaction temperature is 80 ℃, and the residence time of phenol and chlorine in mixed reaction module 2 is 35s, and the mat...

Embodiment 2

[0058] Embodiment 2: preparation 2,4-dichlorophenol

[0059] (1) the preheating module 1 and the mixed reaction module 2 of the microchannel continuous flow reactor are pressed as follows figure 1 The structures shown are connected in sequence, and the temperature of the circulation system is set to 75°C, so that the reactor reaches a temperature control equilibrium, and the phenol is heated and melted into a liquid;

[0060] (2) Set the flow rate of each raw material metering pump, control the mass flow rate of phenol to 60g / min, control the flow rate of chlorine to 99.5g / min, make the molar ratio of phenol and chlorine to 1:2.1, and inject phenol and chlorine into the preheating module respectively 1 for preheating;

[0061] (3) phenol and chlorine after preheating enter mixed reaction module 2 simultaneously and carry out mixed reaction, and the control mixed reaction temperature is 75 ℃, and the residence time of phenol and chlorine in mixed reaction module 2 is 25s, and ...

Embodiment 3

[0062] Embodiment 3: Preparation of 2-methyl 4-chlorophenol

[0063] (1) the preheating module 1 and the mixed reaction module 2 of the microchannel continuous flow reactor are pressed as follows figure 1 The structures shown are connected in sequence, and the temperature of the circulation system is set to 68°C, so that the reactor reaches a temperature control equilibrium, and o-cresol is heated and melted into a liquid;

[0064] (2) set the flow rate of each raw material metering pump, control the o-cresol mass flow rate to be 108g / min, control the chlorine flow rate 71g / min, make the mol ratio of o-cresol and chlorine be 1:1, and o-cresol and chlorine are injected into the preheating module 1 respectively for preheating;

[0065] (3) o-cresol and chlorine after preheating enter mixed reaction module 2 to carry out mixed reaction simultaneously, and the control mixed reaction temperature is 68 ℃, and the residence time of o-cresol and chlorine in mixed reaction module 2 is...

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Abstract

The invention provides a method for chlorination of phenols in a microchannel continuous flow reactor. The method comprises the following steps: (a) separately introducing phenol raw materials and chlorine gas into a preheating module of the microchannel continuous flow reactor for separate preheating reaction, wherein a molar ratio of the phenol raw materials and the chlorine gas is controlled to be 1: (0.95-2.5); and (b) separately after and simultaneously conveying the phenol raw materials and the chlorine gas having undergone preheating reaction into a mixed reaction module of the microchannel continuous flow reactor for reaction, and cooling and treating a product obtained after completion of the reaction. According to the invention, the microchannel continuous flow reactor is adopted for chlorination, so process is simple; only a small amount of waste gas, waste water and industrial residues are produced; reaction conditions can be precisely controlled; yield is high; the purity of the product is high; and reaction time is short.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, relates to a chlorination reaction of phenols, in particular to a method for carrying out the chlorination reaction of phenols in a microchannel continuous flow reactor. Background technique [0002] 2,4-dichlorophenol and 2-methyl 4-chlorophenol are important chemical pesticide intermediates, 2,4-dichlorophenol is the main raw material intermediate of herbicide pesticide 2,4-D acid, 2-methyl 4-Chlorophenol is the main raw material of the pesticide dimethyltetrachloride. The safe and environmentally friendly synthesis of chlorophenols is of great significance to the current pesticide companies. [0003] At present, the synthesis of 2,4-dichlorophenol and 2-methyl-4-chlorophenol mainly adopts traditional kettle or tower continuous reaction. [0004] CN 103435453A discloses a method for preparing 2,4-dichlorophenol by directional catalytic chlorination of phenol. The method u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/62C07C39/30C07C39/28
CPCC07C37/62C07C39/30C07C39/28
Inventor 周庆江谢思勉田晓宏
Owner SHANGHAI XIAOMING DETECTION TECH SERVICE CO LTD