<p>Addressing the issue of lengthy metal extraction processes and large pollutant production in scrap zinc desulfurizers and copper–zinc catalysts, this paper proposes a technique for the efficient and clean co-separation of copper and zinc from these materials using a vacuum carbothermal reduction method. Based on the chemical composition and main phase analysis of scrap zinc desulfurizers and copper–zinc catalysts, experimental research on the vacuum carbothermal co-extraction and separation of copper and zinc was conducted. Optimal conditions for zinc volatilization were obtained by adjusting heating temperature, holding time, and material ratios, and the process mechanism was thoroughly analyzed. The results indicate that scrap zinc desulfurizers with ZnS as the main phase and copper–zinc catalysts with CuO and ZnO as the main phases can effectively volatilize zinc through vacuum carbothermal reduction in a co-processing manner. For the mixture of copper–zinc catalysts, zinc desulfurizers, and carbon at a C:(ZnO + CuO) ratio of 1:1 (molar ratio) and CuO:ZnS at 2:1 (molar ratio), heating to 1100°C and holding for 60&#xa0;min resulted in a zinc volatilization rate of 99.56 . The copper content in the reduced slag reached 59.46%, with the copper primarily in the form of Cu_1.96S, which can be used as a raw material for the copper smelting process.</p>