Electrochemical oxidation degradation of azo dyes has become a widely used method in recent years. Iron phosphomolybdate (FePMo12) was synthesized with molybdophosphoric acid and ferric salt. Morphology and microstructure of catalyst were chararerized by IR spectrometry and X-ray diffraction. The heteropolyanion showed a Keggin structure. Electrochemical oxidation of acid red 3R was investigated in the presence of FePMo12 supported on modified 4A molecular sieve (4A) as packing materials in the reactor. The results showed that the optimal technological conditions for decolorization of acid red 3R simulated wastewater were as follows: active component load 3% , electrolytic voltage 22 V, initial pH 4, air-flow 0.08 m3 h- ', electrode span 3.0 cm. Under the opñrrizd conditions, the decolorization efficiency, COD and TOC removal efficiencies reached 75.3% , 65.4% and 46.0% after 90 min, respectively. With the addition of NaCI to the dyes solution during electrolysis, the decolorization efficiency increased, while the effect of Na2SO4 on the degradation was negative. The efficiency of degradation and mineralization of the acid red 3R were estimated based on the absorbance measurements by UV-vis. It shows that the conjugated structure of dye was destroyed primarily.