According to the characters of HABS industrial wastewater of high pH, high COD and high concentration of sulfite, a pilot reactor with catalytic oxidation-Fenton combined treatment process was built, and the pilot scale experiments were employed to discuss the optional parameters. A pilot scale is 5 t／d. After optimized, the optimal optional parameters in catalytic oxidation stage were pH 8, aeration rate 50 m³／h, HRT 90 min. The optimal optional parameters in Fenton stage were dosage of H₂O₂(30％) 1.00 mL／L. The effluent quality can meet the first class requirements of Sewage Discharge Standard in GB8978—1996, which suggests the process is economical and feasible.