Azo dye waste water is a serious problem because of the high yield, the low biodegradability and the high toxicity. In this work, the heterogeneous Fenton process was employed to degrade methyl orange (MO) using Copper(II)-benzoic acid (CuBA) as the catalyst in the HCO 3 solution using H 2 O 2 as the oxidant. CuBA was prepared by a complexing reaction. It was analyzed by FTIR and catalytic activity. The e ects of di erent parameters on the degradation e ciency of the process were studied. The results were found that 90.8% MO degradation e ciency was achieved within 30 min under the best conditions of initial pH 7.0, 1.2 mM of CuBA, 25 mg/L of MO, 10 mM of NaHCO 3 and 0.40 g/L (m/V) of H 2 O 2 at 40°C. The kinetics of degradation of MO followed rst-order reaction kinetics. A possible pathway of MO degradation was also proposed based on the detected intermediate products by UV-Vis, IR, mass spectrometry. MO was e ectively degraded by CuBA/NaHCO 3 /H 2 O 2 under the neutral and alkalic conditions. The CuBA/NaHCO 3 /H 2 O 2 system overcomes the two problems faced by the homogeneous Fenton process.