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Method for synthesizing 4, 4 '-dichlorodiphenyl sulfone by using sulfoxide oxidation method

A technology of dichlorodiphenyl sulfone and dichlorodiphenyl sulfoxide, applied in 4 fields, can solve the problems of serious odor of glacial acetic acid, air pollution, etc., and achieve the effects of low cost, less usage, and short reaction time

Inactive Publication Date: 2021-04-06
JIANGSU AOLUNDA HIGH TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Patent CN106349126 discloses that 4,4'-dichlorodiphenyl sulfoxide is used as raw material, sulfuric acid is used as catalyst, dichloropropane and glacial acetic acid are used as solvent, and hydrogen peroxide is used as oxidant at a reaction temperature of 60-90°C A method for preparing 4,4'-dichlorodiphenylsulfone by oxidizing 4,4'-dichlorodiphenylsulfoxide. Although the yield of this method is high, it needs to use highly corrosive sulfuric acid as a catalyst and glacial acetic acid as a mixed solvent. Glacial acetic acid smells bad and can easily cause air pollution

Method used

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  • Method for synthesizing 4, 4 '-dichlorodiphenyl sulfone by using sulfoxide oxidation method

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Experimental program
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Effect test

Embodiment 1

[0033] Add 135.58 grams (0.5 moles) of 4,4'-dichlorodiphenyl sulfoxide, 135.5 grams of dichloropropane, 130 grams of water, and 8.06 grams of tetrabutylammonium bromide into a 1000ml four-necked flask with a thermometer and a condenser. After the feeding is completed, the temperature is raised to 50°C, and 188.9 grams of hydrogen peroxide with a content of 27% is slowly added dropwise for about 40 minutes-1 hour. After completion, the temperature is kept at this temperature for 7 hours, sampling is carried out, and the content is measured by liquid chromatography. 4,4'-di Chlorodiphenylsulfoxide is less than 0.3%, stop the reaction, cool to 0-5°C, filter, wash the filter cake with water, and dry to obtain 138.5g of 4,4'-dichlorodiphenylsulfone with a content of 99.5% and a yield of 96%.

Embodiment 2

[0035] Add 135.58 grams (0.5 moles) of 4,4'-dichlorodiphenyl sulfoxide, 135.5 grams of dichloropropane, 130 grams of water, and 0.81 grams of tetrabutylammonium bromide into a 1000 ml four-necked flask with a thermometer and a condenser. After the feeding is completed, the temperature is raised to 90°C, and 53.44 grams of hydrogen peroxide with a content of 35% is slowly added dropwise for about 40 minutes-1 hour. After completion, the temperature is kept at this temperature for 6 hours, and samples are taken, and the content is measured by liquid chromatography. 4,4'-di Chlorodiphenyl sulfoxide is less than 0.3%, stop the reaction, cool to 0-5°C, filter, wash the filter cake, and dry to obtain 138.8g of 4,4'-dichlorodiphenyl sulfone, content 99.1%, yield 95.8%.

Embodiment 3

[0037] Add 135.58 grams (0.5 moles) of 4,4'-dichlorodiphenyl sulfoxide, 120 grams of dichloropropane, 120 grams of water, and 3.22 grams of tetrabutylammonium bromide into a 1000ml four-necked flask with a thermometer and a condenser. After feeding, the temperature was raised to 80°C, and 99.6 grams of hydrogen peroxide with a content of 35% was slowly dropped, and the drop was completed in about 40 minutes to 1 hour. After completion, the temperature was kept at this temperature for 3 hours, and samples were taken, and the content was measured by liquid chromatography. 4,4'-di Chlorodiphenyl sulfoxide has been less than 0.4%, stop the reaction. Cool to 0-5°C, filter, wash the filter cake twice, and dry to obtain 137.8g of 4,4'-dichlorodiphenylsulfone, content 99.0%, yield 95.0%

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Abstract

The invention relates to a method for synthesizing 4, 4 '-diaminodiphenyl sulfone by a sulfoxide oxidation method. The method is characterized by comprising the following steps: putting 4, 4 '-dichlorodiphenyl sulfone, dichloropropane, water and a phase transfer catalyst into a reactor, heating to 50-95 DEG C after feeding is finished, slowly dropwise adding hydrogen peroxide, continuously reacting for 3-7 hours, cooling to 0-5 DEG C, filtering, washing a filter cake with water, and drying to obtain the finished product 4, 4'-dichlorodiphenyl sulfone. The method is short in reaction time, thorough in material reaction, high in product yield and low in production cost.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a preparation method of 4,4'-dichlorodiphenyl sulfone. Background technique [0002] 4,4'-Dichlorodiphenylsulfone is the main raw material for preparing special engineering plastics such as polysulfone and polyethersulfone, and it is also the main intermediate of 4,4'-diaminodiphenylsulfone, 4,4'-diaminodiphenylsulfone Diphenyl sulfone is mainly used in the synthesis of polysulfone amide resins and other polymers, anti-leprosy drugs. With the rapid development of sulfone-containing resins, the demand for 4,4'-dichlorodiphenylsulfone is also increasing, and the synthetic method of 4,4'-dichlorodiphenylsulfone is also becoming more and more important. [0003] At present, there are two main methods for synthesizing 4,4'-dichlorodiphenyl sulfone in the world. One is the pyrosulfate method, which is to prepare pyrosulfate by reacting sulfur trioxide with dimethyl su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/02C07C317/14B01J31/02
CPCC07C315/02B01J31/0239B01J2231/70
Inventor 陈盘强陈律钮强
Owner JIANGSU AOLUNDA HIGH TECH IND
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