Implementing mixed metal oxide (MMO) anodes in zinc electrowinning is highly desired due to the considerable reduction in electrical energy consumption. However, the presence of manganese in the electrolyte is a major obstacle for implementing MMO anodes in the zinc cell houses. In this work, we explore the possibility of using plant off-gas, containing SO2, to remove manganese. A SO2/air gas mixture with different SO2 and O2 concentrations was therefore used for the oxidative precipitation of manganese. It was shown that the manganese oxidation reaction is highly pH-dependent. Calcium hydroxide was used to control the pH during the process. Different operating parameters, i.e., pH, SO2/air ratio, reaction time, and effect of cobalt as a reaction catalyst, were investigated. Optimal conditions for manganese removal were reported. Under the optimal conditions, the manganese concentration decreased from 1 g L−1 to less than 1 mg L−1 within 30 min. Precipitates were characterized using EDS, XRF, and XPS techniques and showed coprecipitation of manganese, zinc, gypsum, and cobalt.