Copper plant residue (CPR) is a hazardous industrial by-product possessing both high toxicity and valuable metal content, necessitating its high value-added utilization. Traditional practices in smelters involve stockpiling and landfilling of CPR, leading to substantial land occupation and water contamination. This study focused on the preparation of PbO and Pb3O4 using the HCl–NaCl leaching–conversion–thermal decomposition process, employing CPR as the primary raw material. The effect of various leaching process conditions on the metal leaching rate was explored. A maximum lead leaching rate of 87.65% was achieved under optimal conditions including leaching temperature, liquid–solid ratio, leaching time, HCl molar concentration, NaCl mass concentration, and particle size. The lead content in the leachate was 15.85 g/L. Experimental data indicated that ash diffusion control served as the rate-limiting step in the HCl–NaCl leaching process. The apparent activation energy was determined to be 18.374 kJ mol−1, with a reaction order of 0.8986 concerning the HCl concentration and an L/S ratio of 0.8124. Additionally, response surface methodology enabled the determination of technological parameters for refining PbCl2 into PbCO3 precursors, yielding a conversion rate exceeding 96.50%. Moreover, the technical indicators of PbO and Pb3O4 obtained through low-temperature thermal decomposition of PbCO3 were investigated. The fabricated PbO and Pb3O4 exhibited purities of 99.65% and 99.26%, respectively, effectively transforming CPR from hazardous waste residue into valuable products. The process ensures the efficient recovery of lead to its maximum extent and promotes residue recycling.
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