New preparation method of 4,4-dichlorodiphenyl sulfone

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...

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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 stipulated in the production of polysulfone and polyethersulfone; the reaction temperature of the sulfuric acid method is high, the reaction time is long, the equipment is severely corroded, the product quality is poor, and the yield is low; the sulfur trioxide method The entire process route is long, the Fuckers reaction temperature is high, the reaction time is long, and the refining process route is complicated