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

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...

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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 disperse oxygen, The latter is easy to decompose; or adopt non-catalyzed strong oxidation method, the oxidant is generally periodic acid, potassium permanganate, potassium ferricyanide, chromium pentoxide, silver carbonate, etc., although high yield products can be obtained, but strong The reduced product of the oxidant needs to be further removed, which increases the difficulty and cost of separation

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