Process for preparing 4,4'-dichlorodiphenyl sulfone

A dichlorodiphenyl sulfone and process technology, which is applied in the field of preparing 4,4'-dichlorodiphenyl sulfone, can solve the problems of low product melting point, complex process, and low cost of sulfuric acid process, and achieve easy industrial production and economic benefits Good, simple process effect

Inactive Publication Date: 2019-06-07
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. It is reported that UCC Company of the United States adopts this method. It uses sulfur trioxide sulfonation and thionyl chloride acyl chloride route, and the process is relatively complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Perform Friedel-Crafts reaction with thionyl chloride and chlorobenzene under the action of a catalyst, the Friedel-Crafts reaction temperature is 25°C, the time is 1.5h, the molar ratio of thionyl chloride to chlorobenzene is 1:4, and the catalyst is Anhydrous aluminum trichloride and benzyltriethylammonium chloride are 3:1 by mass ratio;

[0019] (2) After the mixed reaction is completed, the temperature is lowered to 10°C for 1 hour, then the temperature is raised to 100°C for 2 hours, then cooled, crystals are precipitated, and 4,4'-dichlorodiphenylsulfoxide is obtained by filtration;

[0020] (3) Then dissolve it in glacial acetic acid, add hydrogen peroxide dropwise for oxidation reaction, the oxidation reaction temperature is 70°C, and the oxidation time is 2h. After the reaction is completed, cool down and filter to obtain 4,4'-dichlorodiphenyl sulfone ; The catalyst used is a mixture of anhydrous aluminum trichloride and benzyl triethyl ammonium chloride. ...

Embodiment 2

[0023] (1) The Friedel-Crafts reaction was carried out with thionyl chloride and chlorobenzene under the action of a catalyst. The Friedel-Crafts reaction temperature was 30°C and the time was 1h. Water aluminum trichloride and benzyl triethyl ammonium chloride are 3:1 by mass ratio;

[0024] (2) After the mixed reaction is completed, the temperature is lowered to 10°C for 1 hour, then the temperature is raised to 100°C for 2 hours, then cooled, crystals are precipitated, and 4,4'-dichlorodiphenylsulfoxide is obtained by filtration;

[0025] (3) Then dissolve it in glacial acetic acid, add hydrogen peroxide dropwise for oxidation reaction, the oxidation reaction temperature is 80°C, and the oxidation time is 1h. After the reaction is completed, cool down and filter to obtain 4,4'-dichlorodiphenyl sulfone ; The catalyst used is a mixture of anhydrous aluminum trichloride and benzyl triethyl ammonium chloride.

[0026] The prepared 4,4'-dichlorodiphenylsulfone has a purity of 9...

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a process for preparing 4,4'-dichlorodiphenyl sulfone. The process comprises the following steps of carrying out aFriedel-Crafts reaction on thionyl chloride and chlorobenzene under the action of a catalyst, carrying out cooling for hydrolyzing after the reaction is finished, then carrying out heating for dissolving, carrying out cooling to separate out crystals, carrying out filtering to obtain 4,4'-dichlorodiphenyl sulfoxide, then dissolving the 4,4'-dichlorodiphenyl sulfoxide in glacial acetic acid, addinghydrogen peroxide to carry out an oxidation reaction, carrying out cooling after the reaction is completed, and carrying out filtering to obtain the 4,4'-dichlorodiphenyl sulfone, wherein the catalyst is a mixture of anhydrous aluminum chloride and benzyl triethyl ammonium chloride. The process disclosed by the invention is simple, low in cost and less in impurity, the composite catalyst is adopted, and no additional solvent is added, so that purity of the obtained product is high, and the content of the obtained product is 99.4% or above. The yield reaches 92% or above, the economic benefitis good, and industrial production is facilitated.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a process for preparing 4,4'-dichlorodiphenyl sulfone. Background technique [0002] 4,4'-Dichlorodiphenylsulfone (DDS) is an important organic synthesis product, the main raw material for the preparation of engineering plastics such as polysulfone and polyethersulfone, and an intermediate for medicine, dyes and pesticides. It can be used to prepare a variety of polymer products, such as resins such as bisphenol A polysulfone, polyphenylene ether sulfone, and polyamide sulfone, and can also be used to prepare 4,4'-diaminodiphenylsulfone, an intermediate of leprosy medicine. With the wide application of polymer materials, the demand for DDS is also increasing. [0003] There are many ways to produce DDS in industry, mainly including sulfuric acid method, chlorosulfonic acid method, sulfur trioxide method and sulfoxide oxidation method. The sulfuric acid method has low cost and s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/14C07C315/04C07C315/02
Inventor 薛居强张泰铭毕义霞张善民张聪聪谢圣斌
Owner SHANDONG KAISHENG NEW MATERIALS
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