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Electrolytic manganese anode slime (EMAS) is produced during the production of electrolytic manganese metal. In this study, a method based on vacuum carbothermal reduction was used for Pb removal in EMAS. A Pb-removal efficiency of 99.85% and MnO purity in EMAS of 97.34 wt.% was obtained for a reduction temperature of 950°C and a carbon mass ratio of 10% for a holding time of 100 min. The dense structure of the EMAS was destroyed, a large number of multidimensional pores and cracks were formed, and the Pd-containing compound was reduced to elemental Pb by the vacuum carbothermal reduction. A recovery efficiency for chemical MnO2 of 36.6% was obtained via preparation from Pd-removed EMAS through the “roasting-pickling disproportionation” process, with an acid washing time of 100 min, acid washing temperature of 70°C, H2SO4 concentration of 0.8 mol/L, liquid-solid mass ratio of 7 mL/g, calcination temperature of 60°C and calcination time of 2.5 h. Moreover, the crystal form of the prepared chemical MnO2 was found to be basically the same as that of electrolytic MnO2, and its specific surface area, micropore volume and discharge capacity were all higher than that of electrolytic MnO2. This study provides a new method for Pd removal and recycling for EMAS.