A new Fenton-like catalyst was prepared to degrade Orange IV in water by catalytic decomposition of H2O2. The optimal preparation conditions were discussed. The catalytic activity of catalyst was evaluated by the degradation of Orange IV and the decomposition of H2O2. The results show that solid super acid (S2O82-/FexOy) soaked in (NH4)2S2O8 is the most effective catalyst among the synthesized iron oxides soaked in other oxidants. The optimal conditions for solid super acid preparation are calcined at 500 for 2 h in the air.