New preparation method of 4,4-dichlorodiphenyl sulfone

A technology of dichlorodiphenyl sulfone and dichlorodiphenyl sulfoxide, which is applied in the field of preparation of 4.4-dichlorodiphenyl sulfone, can solve the problems of high production cost, high Friedel-Crafts reaction temperature, and long reaction time, and achieve production The effect of low cost, good product quality and short reaction time

Inactive Publication Date: 2012-02-15
WUJIANG BEISHE SHENGYUAN TEXTILE PROD AUXILIARIES PLANT
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Problems solved by technology

[0004] At present, the commonly used synthetic methods of 4.4-dichlorodiphenyl sulfone include: chlorosulfonic acid method, sulfuric acid method and sulfur trioxide method; wherein, the production cost of 4.4-dichlorodiphenyl sulfone prepared by chlorosulfonic acid method is high, and the three wastes are serious , and the product quality is relatively poor, it is difficult to meet the quality requirements sti

Method used

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Embodiment Construction

[0010] The technical solutions of the present invention will be described in detail below in conjunction with examples.

[0011] The new preparation method of 4.4-dichlorodiphenylsulfone of the present invention, the chemical medicine that adopts has: catalyst AlCl3, chlorobenzene, thionyl chloride, oxygenant hydrogen peroxide and catalytic solvent acetic acid; Specifically comprise the following steps:

[0012] (1) Preparation of 4.4-Dichlorodiphenylsulfoxide

[0013] Using AlCl3 as a catalyst, chlorobenzene and thionyl chloride as reaction raw materials, carry out Friedel-Crafts reaction between 25-35 degrees Celsius, and then hydrolyze the mother liquor after the Friedel-Crafts reaction, and reflux at 95-100 degrees Celsius after hydrolysis After 45-60min, after reflux, cool to below 20°C and divide into organic phase and water phase; the organic phase is distilled under reduced pressure, centrifuged and washed to neutrality, and then used as product A for later use. The ma...

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Abstract

The invention discloses a new preparation method of 4,4-dichlorodiphenyl sulfone. The method comprises the following steps: 1) through using AlCl3 as a catalyst, and chlorobenzene and thionyl chloride as reaction raw materials, performing a Friedel-Crafts reaction at 25-35 DEG C, then hydrolyzing the mother liquor obtained through the Friedel-Crafts reaction, refluxing at 95-100 DEG C for 45-60 minutes, cooling the obtained mother liquor to less than 20 DEG C after refluxing to obtain an organic phase and an aqueous phase; 2) performing reduced pressure distillation on the organic phase, centrifuging, washing the obtained product to be neutral and be used as a product A for later use, wherein the main component of the product A is 4,4-dichlorodiphenyl sulfoxide; and 3) through using the product A and the oxidant hydrogen peroxide as raw materials and acetic acid as satalytic solvent, carrying out an oxidation reaction on the main component 4,4-dichlorodiphenyl sulfoxide of the product A to obtain crude 4,4-dichlorodiphenyl sulfone. Therefore, the existing synthesis method of 4,4-dichlorodiphenyl sulfone is changed, the production cost of 4,4-dichlorodiphenyl sulfone is low, the product quality is good and the reaction time is short.

Description

technical field [0001] The invention relates to a preparation method of 4.4-dichlorodiphenyl sulfone. Background technique [0002] 4.4-Dichlorodiphenylsulfone, referred to as DDS, is a white crystal, sublimable, easily soluble in benzene, chlorobenzene, DMF and other organic solvents; slightly soluble in ethanol and methanol; insoluble in water. Its flash point is 233°C and its boiling point is 397°C. [0003] 4.4-Dichlorodiphenyl sulfone is widely used in the field of engineering plastics and fine chemicals. It is the main raw material for the preparation of engineering plastics such as polysulfone and polyethersulfone, and is also an intermediate for medicine, dyes, and pesticides. [0004] At present, the commonly used synthetic methods of 4.4-dichlorodiphenyl sulfone include: chlorosulfonic acid method, sulfuric acid method and sulfur trioxide method; wherein, the production cost of 4.4-dichlorodiphenyl sulfone prepared by chlorosulfonic acid method is high, and the th...

Claims

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Application Information

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IPC IPC(8): C07C317/14C07C315/02
Inventor 钱华张宁荣
Owner WUJIANG BEISHE SHENGYUAN TEXTILE PROD AUXILIARIES PLANT
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