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Preparation method of 3,3'-diamino-4,4'dyhydroxy diphenyl sulfone

A technology of dihydroxydiphenyl sulfone and diamino is applied in the field of preparation of monomer 3,3'-diamino-4,4'-dihydroxydiphenyl sulfone, and can solve long reaction steps, difficulty in filtration and difficulty in separation and other problems, to achieve the effect of solvent recovery and application, simple operation and good repeatability

Active Publication Date: 2016-01-06
天津泰合利华材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method includes three steps, the reaction steps are long, and the efficiency is low. The use of mixed acid nitration is easy to generate isomers, and the separation is difficult; hydrogenation reduction, careless operation is easy to cause explosion, and the safety hazard is large; metal reduction is easy to cause filtration difficulties because the metal is too fine , it is not easy to wash out the product, it needs to consume a lot of solvent, and the waste residue pollutes the environment more

Method used

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  • Preparation method of 3,3'-diamino-4,4'dyhydroxy diphenyl sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 17.3 grams of o-bromophenol, 250 milliliters of chloroform, 84.6 grams of trifluoromethanesulfonic anhydride, 45 grams of trifluoromethanesulfonic acid and 20.2 grams of potassium hydrogen persulfate in the reaction flask (the molar ratio is: o-bromophenol: potassium hydrogen persulfate : Trifluoromethanesulfonic acid: Trifluoromethanesulfonic anhydride: Chloroform=1:1.2:3:3:31), heated up to 50°C for reaction under stirring, after the reaction of the raw materials was complete, the solvent was distilled off under reduced pressure, and the solid was precipitated by cooling down. After filtration, the filter cake was washed with aqueous sodium acetate, washed with water and dried to obtain 18.5 g of 3,3'-dibromo-4,4'-dihydroxydiphenylsulfone, with a yield of 90.5%.

Embodiment 2

[0021] Add 17.3 grams of o-bromophenol, 224 milliliters of chloroform, 56.4 grams of trifluoromethanesulfonic anhydride, 37.5 grams of trifluoromethanesulfonic acid and 18.5 grams of potassium hydrogen persulfate in the reaction flask (the molar ratio is: o-bromophenol: potassium hydrogen persulfate : trifluoromethanesulfonic acid: trifluoromethanesulfonic anhydride: chloroform=1:1.1:2.5:2:28), heated up to 40°C for reaction under stirring, after the reaction of the raw materials was complete, the solvent was evaporated under reduced pressure, and the solid was precipitated by cooling down. After filtration, the filter cake was washed with aqueous sodium acetate, washed with water and dried to obtain 16.4 g of 3,3'-dibromo-4,4'-dihydroxydiphenylsulfone, with a yield of 80.35%.

Embodiment 3

[0023] Add 17.3 grams of o-bromophenol, 272 milliliters of chloroform, 112.8 grams of trifluoromethanesulfonic anhydride, 52.5 grams of trifluoromethanesulfonic acid and 21.9 grams of potassium hydrogen persulfate in the reaction flask (the molar ratio is: o-bromophenol: potassium hydrogen persulfate : trifluoromethanesulfonic acid: trifluoromethanesulfonic anhydride: chloroform=1:1.3:3.5:4:32), heated up to 60°C for reaction under stirring, after the reaction of the raw materials was complete, the solvent was evaporated under reduced pressure, and the solid was precipitated by cooling down. After filtration, the filter cake was washed with aqueous sodium acetate, washed with water and dried to obtain 18.45 g of 3,3'-dibromo-4,4'-dihydroxydiphenylsulfone, with a yield of 90.47%.

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Abstract

The invention relates to a preparation method of 3,3'-diamino-4,4'-dyhydroxy diphenyl sulfone. 2-bromophenol and potassium hydrogen persulfate are heated to 50 DEG C to have a reaction in a mixed solution of trifluoromethanesulfonic acid, trifluoromethanesulfonic anhydride and chloroform, a solvent is evaporated under reduced pressure after the reaction of the raw materials is completely finished, the temperature is reduced, solids are precipitated, filtering is performed, a filter cake is washed with a sodium acetate aqueous solution, and 3,3'-dibromo-4,4'-dyhydroxy diphenyl sulfone is obtained after washing and drying; 3,3'-dibromo-4,4'-dyhydroxy diphenyl sulfone is dissolved in N-methyl pyrrolidone and has a reaction with ammonium hydroxide at the temperature of 150 DEG C, a solvent is evaporated after the reaction of the raw material is completely finished, a remaining reaction solution is poured into water, and 3,3'-diamino-4,4'-dyhydroxy diphenyl sulfone is prepared after filtering, washing and drying. The method has the advantages that a few reaction steps are required, raw materials are easy to purchase, requirements for production equipment are low, the yield is high, the operation is simple, the repeatability is good, the solvents can be recycled and the like.

Description

technical field [0001] The invention relates to a preparation method of a monomer 3,3'-diamino-4,4'-dihydroxydiphenylsulfone which can be used as a polymer functional material. Background technique [0002] 3,3'-diamino-4,4'-dihydroxydiphenyl sulfone is an aromatic heterocyclic monomer, which can be used as a monomer for special polymer functional materials. It is a polymer with heat resistance and mechanical properties. It is mostly used in aerospace industry, textile industry and other fields. [0003] The preparation method of 3,3'-diamino-4,4'-dihydroxydiphenyl sulfone is usually based on phenol as raw material, reacting with concentrated sulfuric acid to obtain 4,4'-dihydroxydiphenyl sulfone (Jia Kuile, et al. Journal of Wuhan Institute of Technology, 2011,30(2),45-47), and then nitrated with mixed acid (CN1660776) to obtain 3,3'-dinitro-4,4'-dihydroxydiphenyl sulfone, and then hydrazine hydrate / Ferric chloride, palladium carbon / hydrazine hydrate, tin (Annaheim, Chem...

Claims

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Application Information

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IPC IPC(8): C07C315/04C07C317/36
Inventor 栗晓东尚振华
Owner 天津泰合利华材料科技有限公司
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