The nanoscale zero-valent iron (nZVI) has great potential to degrade organic polluted wastewater. In this study, the nZVI particles were obtained by the pulse electrodeposition and were loaded on the biomass activated carbon (BC) for synthesizing the composite material of BC-nZVI. The composite material was characterized by SEM-EDS and XRD and was also used for the decolorization of methyl orange (MO) test. The results showed that the 97.94% removal percentage demonstrated its promise in the remediation of dye wastewater for 60 min. The rate of MO matched well with the pseudo-second-order model, and the rate-limiting step may be a chemical sorption between the MO and BC-nZVI. The removal percentage of MO can be effectively improved with higher temperature, larger BC-nZVI dosage, and lower initial concentration of MO at the pH of 7 condition.