<p>Zinc smelters that adopt hydrometallurgical zinc smelting processes generate large amounts of zinc leaching residue, and extracting Pb and Zn from this residue is one of the critical approaches for resource recycling. In this work, the vacuum carbothermal reduction-volatilization method was used to extract Pb and Zn from zinc leaching residue. Thermodynamic calculations were performed to investigate the phase transformations of Pb and Zn in the residue during the vacuum carbothermal reduction process, and experimental studies on the extraction of Pb and Zn were also conducted. The results indicate that under the conditions of a furnace pressure of 10&#xa0;Pa, a carbon content of 18.5%, and holding the pellets at 1000&#xa0;°C for 30&#xa0;min, the volatilization rates of Pb and Zn from the zinc leaching residue reach 98.93% and 95.40%, respectively. The volatilized Pb(g) and Zn(g) can be condensed into a mixture of metallic Pb and Zn. The vacuum carbothermal reduction process of Pb and Zn in the residue is as follows: first, at low temperatures, ZnFe₂O₄ and iron oxides in the residue are reduced by carbon to metallic Zn and Fe, while PbSO₄ is reduced by carbon to PbS; at high temperatures, Zn and Pb in ZnS and PbS are displaced by Fe respectively, generating metallic Zn and Pb, and iron combines with sulfur to form FeS. The research findings provide a reference for the low carbon, environmentally friendly, and clean extraction of Pb and Zn from zinc leaching residue.</p> Graphical Abstract <p></p>