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Method for synthesizing chlorophenol compounds in micro-channel continuous flow reactor

A chlorinated phenol and reactor technology, applied in the field of synthesizing chlorinated phenol compounds, can solve the problems of serious equipment corrosion, harsh reaction conditions, high catalyst toxicity, etc., and achieve a high degree of automation, high reaction efficiency, and shortened reaction time. Effect

Inactive Publication Date: 2019-01-11
连云港恒贸化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material price of this method is relatively high, the reaction conditions are relatively harsh, and the equipment is severely corroded, so it is rarely used in the process.
[0007] 2) Sulfonation and chlorination method, that is, using phenol as a raw material, sulfonating concentrated sulfuric acid to obtain p-hydroxybenzenesulfonic acid, and chlorination and hydrolysis to remove sulfonic acid groups to obtain 2,6-dichlorophenol, and the yield is 60 % or so, the process is cumbersome, there are more three wastes, and the pollution is heavy
Many reaction steps, high cost of raw materials
[0009] 4) Using 2,2,6,6-tetrachlorocyclohexanone as raw material, alkyl phosphorus and arsenic compounds as catalysts, directly dechlorinate 2,6-dichlorophenol at 120-180°C, the catalyst of this method High toxicity and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for synthesizing chlorinated phenols in a microchannel continuous flow reactor, comprising the following steps:

[0032] 1) After adding phenol into the microchannel continuous flow reactor, chlorine gas is passed into the microchannel continuous flow reactor, and the temperature of the microchannel continuous flow reactor is kept at 60°C for chlorination reaction; wherein, the phenol and chlorine gas The mol ratio is that the inlet velocity of the chlorine gas of 1:1 is 40 liters / hour; the reaction temperature in the microchannel continuous flow reactor is controlled by an external heat exchanger, and the heat exchanger in the external heat exchanger The heat medium is heat conduction oil;

[0033] 2) Sampling and testing the content of chlorinated phenol compounds in the microchannel reactor on time, when the content of p-chlorophenol reaches 55%, stop the chlorine gas flow;

[0034] 3) The reaction liquid is transported to the p-chlorine rectification tower...

Embodiment 2

[0036] A method for synthesizing chlorinated phenols in a microchannel continuous flow reactor, comprising the following steps:

[0037] 1) After adding phenol into the microchannel continuous flow reactor, chlorine gas is passed into the microchannel continuous flow reactor, and the temperature of the microchannel continuous flow reactor is kept at 80°C for chlorination reaction; wherein, the phenol and chlorine gas The mol ratio is 1:1.2, and the intake velocity of the chlorine gas is 60 liters / hour; the reaction temperature in the microchannel continuous flow reactor is controlled by an external heat exchanger, and the The heat exchange medium is heat conduction oil;

[0038] 2) Sampling and testing the content of chlorinated phenol compounds in the microchannel reactor on time, when the content of p-chlorophenol reaches 55%, stop the chlorine gas flow;

[0039] 3) The reaction liquid is transported to the p-chlorine rectification tower through the pipeline, and the p-chlo...

Embodiment 3

[0041] A method for synthesizing chlorinated phenols in a microchannel continuous flow reactor, comprising the following steps:

[0042] 1) After adding phenol into the microchannel continuous flow reactor, chlorine gas is passed into the microchannel continuous flow reactor, and the temperature of the microchannel continuous flow reactor is kept at 70°C for chlorination reaction; wherein, the phenol and chlorine gas The mol ratio is 1:1.1, and the intake velocity of the chlorine gas is 50 liters / hour; the reaction temperature in the microchannel continuous flow reactor is controlled by an external heat exchanger, and the The heat exchange medium is heat conduction oil;

[0043] 2) Sampling and testing the content of chlorinated phenol compounds in the microchannel reactor on time, when the content of p-chlorophenol reaches 55%, stop the chlorine gas flow;

[0044] 3) The reaction liquid is transported to the p-chlorine rectification tower through the pipeline, and the p-chlo...

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PUM

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Abstract

A method for synthesizing chlorophenol compounds in a micro-channel continuous flow reactor comprises the following steps: introducing phenol and chlorine into the micro-channel continuous flow reactor, carrying out a chlorination reaction, and respectively separating and collecting p-chlorophenol, 2,4-dichlorophenol, 2,6-dichlorophenol and 2,4,6-trichlorophenol by rectifying towers. The method has the characteristics of great shortening of the reaction time, good continuous reaction stability, great improvement of the reaction efficiency, reduction of the energy consumption during reaction, low cost and high quality, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical product synthesis, and relates to a method for synthesizing chlorinated phenol compounds in a microchannel continuous flow reactor. Background technique [0002] Chlorinated phenols are important intermediates with a wide range of uses. For example, p-chlorophenol is used in the preparation of pesticides such as fenoxin, mitrafenone, anti-falling agent, tetramine, profenfos, mite egg ester, acarifen, difenate, pharmaceutical clofibrate, and pharmaceutical intermediate p-chlorophenoxyisobutyl Acid, Sodium 5-Chloro-2-Hydroxybenzoate, Antioxidant BHA (Butylated Hydroxyanisole), Dye Fast Pigment Sauce RH, 1,4-Dihydroxyanthraquinone, 1,4-Diaminoanthraquinone, Para-Aminophenol And hydroquinone, selective solvent in oil refining industry, ethanol discoloration agent and other organic synthesis raw materials; Intermediates and raw materials of Dukesan, glycopyrroate, and thiobisdichlorophenol; 2,6-dich...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/28C07C39/30C07C39/32C07C37/62C07C37/74
CPCC07C37/62C07C37/74C07C39/28C07C39/30C07C39/32
Inventor 韩伟国张林飞靳牛强
Owner 连云港恒贸化工有限公司
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