On the basis of sulphide ore flotation theory, the reagent system and process flow chart of separation of Pb, Zn and S minerals from kaolin tailings were studied. The result showed that galena and sphalerite were liberated from other minerals when the portion of particle sizes of <74 mm was 70%. Pb and Zn minerals could be separated better in the conditions of 30 g/t diethyldithiocarbamate, 1000 g/t ZnSO4 and 300 g/t Na2SO3. And Zn an S minerals could be separated better in the conditions of 300 g/t CuSO4 and 50 g/t sodium isobutylxanthate. Through the flow chart of ore grinding, initial flotation of lead minerals, and separation of zinc and S minerals, Pb concentrate with Pb grade of 64.55% and Pb recovery rate of 84.47%, and Zn concentrate with Zn grade of 45.04% and Zn recovery rate of 91.94% were obtained.