Abstract: This is an essay in the field of metallurgical engineering. Comprehensive utilization of sulfur separation tailings from a coal measure high sulfur rare metal complex ore in Chongqing area was studied, which provided a feasible basis for the recovery of valuable elements such as aluminum, silicon, rare earth and niobium. The experimental results show that the optimum leaching conditions are as follows: sulfuric acid concentration 70%, leaching time 3 h, leaching liquid to solid ratio 3, leaching temperature ≥135 ℃. Under these conditions, the Al₂O₃ leaching rate can reach 87.25%. Acid leaching solution can be used to prepare aluminum sulfate as a water treatment agent. SiO₂ can be obtained from acid leaching residue after enrichment of valuable elements such as silicon, rare earth and niobium by NaOH leaching. The content of more than 85 g/L alkali leaching solution, used for the preparation of sodium silicate products; After enrichment of rare earth and niobium elements, the content of TREO and Nb in alkali leaching residue is 1820 g/t and 274 g/t, which can be used as raw materials for the recovery of rare earth and niobium elements.