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Method for preparing 4, 4'-dichloride diphenyl sulfone

A technology of dichlorodiphenyl sulfone and chlorobenzene, which is applied in the field of the trioxysulfur method manufacturing process of raw materials, can solve the problems of restricting the development of sulfone polymer materials, strong corrosiveness of production equipment, deep color of products, etc., and achieves isomerization. The effect of less body, improved product quality and lower temperature

Inactive Publication Date: 2005-06-08
马炳荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The widely used 4,4'-dichlorodiphenyl sulfone manufacturing methods include sulfuric acid method, chlorosulfuric acid method, and sulfuryl chloride method. The reaction temperature of these methods is high, the reaction cycle is long, the material consumption is large, and the production equipment is expensive. Strong corrosiveness, deep color of the products produced, many impurities produced by side reactions, high manufacturing costs, and a large amount of three wastes
The 4,4'-dichlorodiphenyl sulfone produced by these methods is used as a raw material for the synthesis of sulfone polymer materials, which limits the development of sulfone polymer materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Absorb 800 g of sulfur trioxide (A) at 35° C. with 400 g of dimethyl sulfate.

[0025] Disperse 7 g of activated carbon in A with a disperser, and stir at 28° C. for 20 minutes to obtain catalyst excipient functional solution B.

[0026] 1100 g of chlorobenzene was added dropwise to B at 70°C, and the reaction reached the end point after 190 minutes to obtain reactant C. Slowly cool C to -5°C with cooling water and filter, and the resulting crystal D is washed with clean water and dried to obtain 1000 grams of product 4,4'-dichlorodiphenyl sulfone.

[0027] The resulting 4,4'-dichlorodiphenyl sulfone has a melting point of 147.8°C and a hue of 20AHPA, Fe 3+ It is 0.8×10-5 (mass ratio).

Embodiment 2

[0029] 350 g of dimethyl sulfate was mixed with 800 g of sulfur trioxide at 25° C. (A).

[0030] Disperse 8 grams of aluminum oxide in 120 grams of chlorobenzene with a disperser, and stir at 35° C. for 20 minutes to obtain catalyst excipient functional solution B.

[0031] Add B and A dropwise to 85 grams of recovered 4,4'-dichlorodiphenyl sulfone and 870 grams of chlorobenzene after recovering 4,4'-dichlorodiphenyl sulfone and distilling sulfuric acid respectively. After the addition is completed, adjust the temperature to 75°C , after 180 minutes the reaction reached the end point, and reactant C was obtained. Slowly cool C to -8°C with cooling water and filter, and the resulting crystal D is washed with clean water and dried to obtain 1000 grams of product 4,4'-dichlorodiphenyl sulfone.

[0032] The resulting 4,4'-dichlorodiphenyl sulfone has a melting point of 147.6°C and a hue of 25AHPA, Fe 3+ It is 0.7×10-5 (mass ratio).

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Abstract

A process for preparing 4,4'-dichlorodiphenyl sulfone features that the coupling agent of SO3 is used to lower the free enthalpy of sulfonating and condensating reactions and the catalyst of sulfonating and condensating reactions is used to lower the activating energy of reaction, resulting in low reaction temp, short time and high quality of product.

Description

technical field [0001] The invention relates to a preparation method of 4,4'-dichlorodiphenyl sulfone, a raw material for sulfone polymer polymerization, in particular to the sulfur trioxide method manufacturing process of this raw material. Background technique [0002] Sulfone polymer materials such as polysulfone, polyethersulfone, and polyarylsulfone have been widely used in various important industrial fields and daily life due to their excellent heat resistance, physical and mechanical properties, insulation properties, and chemical resistance. For local applications, 4,4'-dichlorodiphenyl sulfone is used as a raw material for the synthesis of sulfone polymer materials. Its manufacturing cost and product quality are the basis for the development of sulfone polymer materials. [0003] The widely used 4,4'-dichlorodiphenyl sulfone manufacturing methods include sulfuric acid method, chlorosulfuric acid method, and sulfuryl chloride method. The reaction temperature of thes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/00C07C317/14
Inventor 马炳荣
Owner 马炳荣
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