Abstract:The arsenic-antimony bearing dust produced by pyrometallurgical treatment of lead anode slime was used as the treatment object. Combined with oxygen pressure alkali leaching test and XRD, ICP-OES and other characterization methods, the effects of oxygen pressure, liquid-solid ratio, sodium hydroxide concentration, leaching temperature, leaching time on the distribution behavior of arsenic, antimony and lead were investigated. The results show that under the conditions of oxygen partial pressure of 2.0MPa, liquid-solid ratio of 10mL/g, sodium hydroxide concentration of 2mol/L, leaching temperature of 200℃ and leaching time of 2h, more than 99.5% of arsenic enters the solution, antimony, lead and bismuth enter the leaching residue, and the arsenic content in the washing residue is less than 0.5%,which can be used to prepare high-quality antimony products. The deep separation of arsenic and antimony is realized by oxygen pressure alkali leaching-water washing process.