This paper presents the results of investigation on simultaneous leaching of galena concentrate and pyrolusite in acid medium. It has been confirmed that the leached products as the raw materialsPbCl 2 , MnCl 2 for the PbSO 4 and Mn 3 O 4 preparations could be obtained during the leaching processes. Special emphasizes are placed on the purification of the simultaneous leaching solution including removals of Fe 2+ , Pb 2+ , Zn 2+ , Ca 2+ , and preparations. The factors affecting the purification, such as pH, temperature, agitation rate, and dosages of Cl − and Na 2 S are investigated in leaching cells. The results show that, at appropriate conditions, iron is removed in the form of FeOOH, Pb 2+ and Zn 2+ are vulcanized by Na 2 S, and Ca 2+ is removed in the form of CaF 2 precipitation. After purification and crystallizing-out of PbCl 2 (97.17%), the effects of pH, temperature, reaction time, concentration, stirring rate, and drying methods on preparations are examined. The mechanisms are addressed by theoretical calculations and experiments. The results indicate that the content of PbSO 4 is 99.46% characterized by elemental analysis, XRD, and SEM. The purity of Mn 3 O 4 is identified by TG-DSC, chemical analysis, and XRD, and the Mn in the Mn 3 O 4 product accounts for 71.7%.