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Method for utilizing 4,4'- dibromodiphenyl ether to prepare 4,4'-dihydroxy diphenyl ether

A technology of dihydroxydiphenyl ether and dibromodiphenyl ether, which is applied in the field of preparation 4, can solve the problems of many side reactions, market promotion restrictions, and high production costs, and achieve shortened reaction time, reduced side reactions, and low actual cost Effect

Inactive Publication Date: 2012-04-25
徐浩清
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 4. The yield of DHDE obtained by hydrolysis of 4,4'-dibromodiphenyl ether is only 50%, and the purity of crude DHDE is about 47%.
[0007] There are many side reactions in the above process methods, low yield and high cost. Therefore, although DHDE is widely used, due to high production cost and high product price, the promotion of the market is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a), the preparation of 4,4'-dibromodiphenyl ether crude product: at 1.5M 3 Put 1000kg of diphenyl ether and 1kg of titanium chloride into the enamel kettle, heat it to 50°C and stir, the diphenyl ether is equivalent to 5882 moles, and add 2260kg of bromine dropwise to the diphenyl ether liquid while stirring the diphenyl ether liquid Bromine, bromine is equivalent to 14125 moles, and the molar ratio of bromine and diphenyl ether is 2.4: 1. After the reaction is finished, excess bromine and HBr gas are evaporated, then washed with water, and residual HBr, bromine and catalyst are washed away. The crude product of 4,4'-dibromodiphenyl ether was obtained;

[0032] b), recrystallization of 4,4'-dibromodiphenyl ether crude product: use chlorobenzene as the recrystallization solvent of 4,4'-dibromodiphenyl ether crude product, in the recrystallization solvent step a) prepared 4 , the crude product of 4'-dibromodiphenyl ether is heated to boiling and kept warm, then stirred, ...

Embodiment 2

[0036] a), the preparation of 4,4'-dibromodiphenyl ether crude product: at 1.5M 3 Put 1000kg of diphenyl ether and 100kg of tin chloride into the enamel kettle, heat it to 20°C and stir, the diphenyl ether is equivalent to 5882 moles, and drop 2070.464kg of diphenyl ether into the diphenyl ether liquid while stirring the diphenyl ether liquid Bromine, bromine is equivalent to 12940.4 moles, and the molar ratio of bromine to diphenyl ether is 2.2:1. After the reaction, excess bromine and HBr gas are evaporated, and then washed with water to remove residual HBr, bromine and catalyst , to obtain the crude product of 4,4'-dibromodiphenyl ether;

[0037] b), recrystallization of 4,4'-dibromodiphenyl ether crude product: o-dichlorobenzene is used as the recrystallization solvent of 4,4'-dibromodiphenyl ether crude product, and prepared in step a) of the recrystallization solvent The crude product of 4,4'-dibromodiphenyl ether is heated to boiling and kept warm, then stirred, then c...

Embodiment 3

[0041] a), the preparation of 4,4'-dibromodiphenyl ether crude product: at 1.5M 3 Put 1000kg of diphenyl ether and 50kg of zinc chloride into the enamel kettle, heat to 50°C and stir, the diphenyl ether is equivalent to 5882 moles, and drop 2352.8kg of diphenyl ether into the diphenyl ether liquid while stirring the diphenyl ether liquid Bromine, bromine is equivalent to 14705 moles, and the molar ratio of bromine to diphenyl ether is 2.5:1. After the reaction, excess bromine and HBr gas are evaporated, and then washed with water to remove residual HBr, bromine and catalyst , to obtain the crude product of 4,4'-dibromodiphenyl ether;

[0042] b), recrystallization of 4,4'-dibromodiphenyl ether crude product: m-dichlorobenzene is used as the recrystallization solvent of 4,4'-dibromodiphenyl ether crude product, and prepared in the recrystallization solvent step a) The crude product of 4,4'-dibromodiphenyl ether is heated to boiling and kept warm, then stirred, then cooled to a...

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Abstract

The invention discloses a method for preparing 4,4'-dihydroxy diphenyl ether, comprising the following steps: I) preparation of crude product of the 4,4'-dihydroxy diphenyl ether; II) recrystallization of the crude product of the 4,4'-dihydroxy diphenyl ether. The method of the invention features low energy consumption, short reaction time and contribution to lowering production cost; in addition,the prepared 4,4'- dibromodiphenyl ether and the final product of 4,4'-dihydroxy diphenyl ether features both high purity and high yield coefficient.

Description

technical field [0001] The invention discloses a preparation method of 4,4'-dibromodiphenyl ether, and discloses a method for preparing 4,4'-dihydroxydiphenyl ether from 4,4'-dibromodiphenyl ether as a raw material. Background technique [0002] 4,4'-dihydroxydiphenyl ether is referred to as DHDE for short. As an important intermediate in the synthesis of various functional polymers, DHDE requires high purity, otherwise it has little use value. The synthesis process route of DHDE generally has the following synthetic routes in the international reports: [0003] 1. DHDE is synthesized by diazotization hydrolysis of 4,4'-diaminodiphenyl ether, the yield is about 50%, and the purity of crude DHDE is about 47%. [0004] 2. DHDE is obtained by high-temperature hydrolysis of 4,4'-dichlorodiphenyl ether, the yield is about 40%, and the purity of crude DHDE is about 38%. [0005] 3. DHDE is obtained by dehydration condensation of hydroquinone, the yield is about 50%, and the puri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/295C07C41/26C07C41/40B01J31/28B01J31/02
Inventor 徐新宇王继华徐浩清
Owner 徐浩清
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