Method for synthesizing high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone through Cu-BTC catalysis

A technology of diphenyl diquinone and tetramethyl, applied in the field of fine chemicals, can solve the problems of easy decomposition, increased separation difficulty and cost, low product yield, etc., and achieves the effects of simple equipment, short cycle and few by-products

Active Publication Date: 2018-01-05
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing technology of preparing 3,3',5,5'-tetramethyl-4,4'-biphenyldiquinone, the catalytic oxidation of 2,6-dimethylphenol coupling synthesis product 3,3',5 is commonly used ,5'-Tetramethyl-4,4'-biphenyldiquinone, the catalyst is mainly metal salt or metal complex, but the product yield is not high, the oxidant is generally oxygen or hydrogen peroxide, the former needs to blow and dis...

Method used

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  • Method for synthesizing high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone through Cu-BTC catalysis
  • Method for synthesizing high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone through Cu-BTC catalysis
  • Method for synthesizing high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone through Cu-BTC catalysis

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 1. Preparation of Cu-BTC

[0033] Weigh 4g copper nitrate trihydrate and add it to 25ml ultrapure water, add 2g trimesic acid to 25ml ethanol, ultrasonically dissolve the two solutions respectively for 20min, slowly add trimesic acid dissolved in ethanol to A mixed solution was formed in the aqueous solution of copper nitrate trihydrate, and after continuing to stir for 30 minutes, the mixed solution was transferred to a 100ml sealed reaction kettle with a polytetrafluoroethylene liner, sealed, heated to 110°C for 18 hours of crystallization, and then cooled to room temperature. The precipitate was obtained, centrifuged, and the precipitate was dried in an oven at 100°C for 6 hours to obtain a blue powder. Transfer the blue powder sample to a Soxhlet extractor, add 40ml of ethanol, and remove it after Soxhlet extraction for 12 hours. Vacuum drying in a vacuum oven at 100° C. and a vacuum degree of 0.1 MPa for 10 hours, and cooling to obtain a Cu-BTC catalyst.

[0034] ...

Embodiment 2

[0036] Example 2 The operation steps are the same as in Example 1, but the surfactant dosage is 0.05 g, and the product quality yield is 91.5%, and the purity is 96.3%.

Embodiment 3

[0037] Example 3 The operation steps are the same as in Example 1, but no surfactant is added to obtain a product with a mass yield of 27.9% and a purity of 32.6%.

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Abstract

The invention discloses a method for synthesizing high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone through Cu-BTC catalysis. According to the method, trimesic acid and copper nitrate hydrateare hydrothermally synthesized into a Cu-BTC catalyst; under the alkaline emulsion reaction condition, hydrogen peroxide is utilized as an oxidizing agent, and 2,6-xylenol is oxidized and coupled intothe high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone; product quality yield of the high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone is 90 to 95%, and a product purity mass percent of the high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone is 98%; reaction temperature is 70 to 85 DEG C, and reaction time is 4 to 8h; the catalyst is easy to separate and recycle; after beingrepeatedly used for four times, quality yield of the 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone still reaches 87.5%, and purity of the 3,3',5,5'-tetramethyl-4,4'-biphenyl diquinone is 97.8%; alkaliemulsified filtrate and washing liquor can be recycled and deployed to be used repeatedly; a reaction condition is moderate, and a synthesizing technology has the advantages of greenness and environmental friendliness.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to a Cu-BTC catalyzed oxidation of 2,6-dimethylphenol coupling to synthesize high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyl diphenyl The quinone method. Background technique [0002] 3,3',5,5'-Tetramethyl-4,4'-biphenyldiquinone is a chemical intermediate, used as a coupling agent and polyphenylene ether redistribution reaction initiator, which can be used in the synthesis of heat resistance It is a flame retardant material with excellent mechanical properties, synthesizes a variety of hydroxyaryl ether, telechelic, block, graft, comb and star polymers, and prepares polyphenylene ether epoxy resins with excellent performance for high-frequency printed circuit boards laminated materials etc. In the existing technology of preparing 3,3',5,5'-tetramethyl-4,4'-biphenyldiquinone, the catalytic oxidation of 2,6-dimethylphenol coupling synthesis product 3,3',5 is commonly used ,5'-Te...

Claims

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Application Information

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IPC IPC(8): C07C46/04C07C50/08B01J31/22B01J35/10
Inventor 刘跃进韩嫣吴志民余荣栋伍巍罗腾
Owner XIANGTAN UNIV
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