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Up to now, separating Pb-Sb alloy obtained from jamesonite by conventional pyrometallurgy processes has many drawbacks such as long technological process, high energy consumption, and unsatisfactory separation efficiency. Thinking about the facts that antimony is used mainly in the form of Sb 2 O 3 , and separation of Sb 2 O 3 with good volatility from the lead melt is very easy under vacuum, vacuum dynamic oxidation process, a new and effective process for separating lead and antimony from Pb-Sb alloy, was developed in this work. Experimental results revealed that the content of antimony in Pb-Sb alloy decreased from 42% to 0.30%, that the removal percent of antimony reached 99.59%, and that the PbO content in the distillate was 0.12% under melt temperature of 953 K, vacuum treatment time of 210 min, and air flow rate of 3 L/min, corresponding to the system pressure of 14 kPa. This study is of significance for separating Pb-Sb alloy obtained from jamesonite. [ABSTRACT FROM AUTHOR]