The invention provides a comprehensive method for separating stibium from materials containing the stibium,
tin and lead, which is suitable for removing the stibium and recovering other valuable metals from
tin lead materials containing stibium with high content. The invention puts an emphasis on that the comprehensive method comprises the following steps of: granulating the materials containing the stibium to manufacture irregular
tin grains with the thicknesses of 2-5 mm and the grain diameters of 2-30 mm; then placing tin grain sheets into an
anode frame lined with acid-resisting fibers to manufacture a tin grain
anode; placing the fine tin lead materials as starting sheets into an
electrolytic cell filled with silicofluoric acids to carry out
electrolysis by electrifying DC, wherein tin and lead metals are electrolyzed and deposited on a
cathode to obtain a
cathode product with total tin and lead content more than 99.8 percent and stibium content less than 0.2 percent, and the valuable metals, i.e. the stibium, gold, silver, and the like, are gathered in
anode mud; and finally recovering the valuable metals, i.e. the stibium, the gold and the silver, from the anode mud. A wet-process metallurgical process has advanced and reasonable process and can greatly enlarge the contact area of
electrolyte and the anode, reduce the
current density during the
electrolysis and eliminate the anode
passivation phenomena.