Abstract:A charge transfer complex (TMB)3PMo12 was synthesized with molybdophosphoric acid and 3,3',5,5'- tetramethylbenzidine. Morphologies and microstructures were characterized by IR spectrometry and X-ray diffraction. The heteropolyanion shows a keggin structure. Electrocatalytic oxidation of acid red 3R was investigated in the presence of (TMB)3PMo12 supported on γ-Al2O3 as packing materials in the reactor. The results showed that (TMB)3PMo12/γ-Al2O3 had good electrocatalytic activity for decolorization of Acid Red 3R. When (TMB)3PMo12 loading was 0.6%, (TMB)3PMo12/γ-Al2O3 filling was 50g, pH value of Acid Red 3R was 4, the voltage was 15.0V, air-flow was 0.14m3/h, and electrode span was 3.0cm, the decolorization efficiency could reach 79.7%. The treatment efficiency of electro-catalytic process was greatly higher than that of electrochemical oxidation process in two dimensional flat reactor and three dimensional electrode reactor.