Abstract: 13X zeolite loaded with Cu and Mn were prepared by incipient wetness method and characterized by XRD, BET and atomic absorption spectroscopy (AAS). The decoloration of methyl orange simulated wastewater with different initial pH was tested by the co-processing of the bimetallic 13X zeolite together with zero-valent iron. It is found that the decoloration of methyl orange simulated wastewater is improved by the co-processing and gets more than 81 % decoloration ratio when treating for 3h using the bimetallic zeolite prepared under the optimal conditions. The optimal preparation conditions are: the concentration of impregnation solution is 1.0mol/L，the mole ratio of copper and manganese is 1.0 and the calcination temperature is 300℃. The characterization results indicate that the metals are uniformly loaded on zeolite and the metal leaching is increased with the decreasing calcination temperature. The leaching metal ions can boost the effect of decoloration of methyl orange simulated wastewater in some extent.