Abstract: The rod-shaped FeMoO4 was synthesized by hydrothermal method using FeSO4·7H2O and Na2MoO4·2H2O as raw materials, and its structure and morphology were characterized by using XRD, Raman and SEM. It studied the performance of FeMoO4 activated persulfate. With phenol as the target pollutant, the effects of sodium persulfate concentrations, phenol initial concentrations, initial pH of phenol solution and temperature on the degradation rate of phenol were investigated, and the types of free radicals that played a major role in the system were initially explored. The results showed that the persulfate activated by FeMoO4 showed good performance in the degradation of phenol between pH=2.00 and pH=11.00, and the maximum dissolution of iron ion was 1.663 mg/L. The optimum degradation conditions were 0.4 g/L of FeMoO4, sodium persulfate/phenol molar rates of 25∶1, the initial pH of 3.00. In the case of this, the phenol degradation rate was 97.20% in 6 h at 30℃. The degradation of phenol by FeMoO4/Na2S2O8 matched first order kinetic. The calculated activation energy was 53.49 kJ/mol. The results of the free radical quenching experiment showed that SO4-· was the primary oxidant for the degradation of phenol.