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.