Process for preparing 4,4'-dichlorodiphenylsulfone employing sulfoxide oxidation method

A technology of dichlorodiphenyl sulfone and dichlorodiphenyl sulfoxide, applied in the field of preparing 4,4'-dichlorodiphenyl sulfone by sulfoxide oxidation method, which can solve the problems of low conversion rate, complex process, incomplete oxidation, etc. question

Inactive Publication Date: 2015-04-29
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sulfuric acid method has low cost and simple raw materials, but the conversion rate is low, the reaction time is long, the melting point of the product is low, and the quality is not good
The chlorosulfonic acid process is relatively mature, and the product quality is good, but the production cost is high and the three wastes are serious
The preparation of DDS by sulfur trioxide method is an improved method, which is adopted by UCC Company in the United States. It uses sulfur trioxide sulfonation and thionyl chloride acyl chloride route, and the process is relatively complicated.
However, during the oxidation process of...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The process for preparing 4,4'-dichlorodiphenyl sulfone by sulfoxide oxidation method comprises the following steps:

[0025] (1) Carry out Friedel-Crafts reaction with chlorobenzene and thionyl chloride under the action of catalyst anhydrous aluminum trichloride, the reaction temperature is 20°C, and the time is 2h to obtain 4,4'-dichlorodiphenyl sulfoxide; Acyl chloride: chlorobenzene: the molar ratio of catalyst is 1:6:1;

[0026] (2) Dissolve 50 g of 4,4'-dichlorodiphenyl sulfoxide obtained in step (1) with 50 g of glacial acetic acid, add 25 g of 30% hydrogen peroxide for oxidation reaction at a temperature of 60° C. and a time of 2 h to obtain 4 , crude 4'-dichlorodiphenyl sulfone;

[0027] (3) Take 53.4g of the 4,4'-dichlorodiphenylsulfone crude product obtained in step (2), with a chromatographic content of 99.1%, dissolve it by heating with 42.8g of glacial acetic acid, and add 8.9g of 30% hydrogen peroxide dropwise at 60°C Oxidation, heat preservation and ox...

Embodiment 2

[0029] The process for preparing 4,4'-dichlorodiphenyl sulfone by sulfoxide oxidation method comprises the following steps:

[0030] (1) Carry out Friedel-Crafts reaction with chlorobenzene and thionyl chloride under the action of catalyst anhydrous aluminum trichloride, the reaction temperature is 30°C, and the time is 1h to obtain 4,4'-dichlorodiphenyl sulfoxide; Acyl chloride: chlorobenzene: the molar ratio of catalyst is 1:8:0.9;

[0031] (2) Dissolve 50 g of 4,4'-dichlorodiphenyl sulfoxide obtained in step (1) with 45 g of glacial acetic acid, add 29 g of 30% hydrogen peroxide for oxidation reaction at a temperature of 80° C. and a time of 1 h to obtain 4 , crude 4'-dichlorodiphenyl sulfone;

[0032] (3) Take 111.7 g of the 4,4'-dichlorodiphenylsulfone crude product obtained in step (2), with a chromatographic content of 98.9%, dissolve it by heating with 100.5 g of glacial acetic acid, and add 14.9 g of 30% hydrogen peroxide dropwise at 70°C Oxidation, heat preservatio...

Embodiment 3

[0034] The process for preparing 4,4'-dichlorodiphenyl sulfone by sulfoxide oxidation method comprises the following steps:

[0035] (1) Carry out Friedel-Crafts reaction with chlorobenzene and thionyl chloride under the action of catalyst anhydrous aluminum trichloride, the reaction temperature is 25°C, and the time is 1.5h to obtain 4,4'-dichlorodiphenyl sulfoxide; Sulfuryl chloride: chlorobenzene: the molar ratio of catalyst is 1:5:1.1;

[0036] (2) Dissolve 50 g of 4,4'-dichlorodiphenyl sulfoxide obtained in step (1) with 60 g of glacial acetic acid, add 26 g of 30% hydrogen peroxide for oxidation reaction at a temperature of 70° C. and a time of 1.5 h to obtain Crude 4,4'-Dichlorodiphenylsulfone;

[0037] (3) Take 180.9 g of the 4,4'-dichlorodiphenylsulfone crude product obtained in step (2), with a chromatographic content of 98.8%, dissolve it by heating with 180.9 g of glacial acetic acid, and add 20.1 g of 30% hydrogen peroxide dropwise at 80°C Oxidation, heat preser...

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PUM

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Abstract

The invention relates to a process for preparing 4,4'-dichlorodiphenylsulfone, in particular to a process for preparing 4,4'-dichlorodiphenylsulfone employing a sulfoxide oxidation method. The process comprises the following steps: carrying out friedel-crafts reaction with chlorobenzene and thionyl chloride under the action of a catalyst to obtain the 4,4'-dichlorodiphenylsulfone; dissolving the obtained 4,4'-dichlorodiphenylsulfone with a solvent; adding hydrogen peroxide and carrying out oxidation reaction to obtain a 4,4'-dichlorodiphenylsulfone crude product; carrying out secondary oxidation refining on the obtained 4,4'-dichlorodiphenylsulfone crude product; and finally preparing high-purity 4,4'-dichlorodiphenylsulfone. The purity of the 4,4'-dichlorodiphenylsulfone purified by the refining process is greater than 99.5%; the refining yield is greater than 98.5%; and the process completely meets the synthesis requirements of high-performance polymers.

Description

technical field [0001] The invention relates to a process for preparing 4,4'-dichlorodiphenyl sulfone, in particular to a process for preparing 4,4'-dichlorodiphenyl sulfone by a sulfoxide oxidation method. Background technique [0002] 4,4'-Dichlorodiphenylsulfone (DDS) is an important chemical monomer, the main raw material for the preparation of engineering plastics such as polysulfone and polyethersulfone, and an intermediate for medicine, dyes and pesticides. A variety of polymer products can be prepared from it, such as resins such as bisphenol A polysulfone, polyphenylene ether sulfone, and polyamide sulfone, and it is also a raw material for the preparation of leprosy drug intermediate 4,4'-diaminodiphenylsulfone. With the wide application of polymer materials, the demand for DDS is also increasing. [0003] There are many ways to produce DDS in industry, such as sulfuric acid method, chlorosulfonic acid method, sulfur trioxide method and sulfoxide oxidation method....

Claims

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Application Information

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IPC IPC(8): C07C315/02C07C317/14
Inventor 杨德耀张泰铭薛居强毕义霞张善民宋国城张聪聪谢圣斌
Owner SHANDONG KAISHENG NEW MATERIALS
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