The purpose of this study was to investigate the physicochemical particularities of the regeneration processes that occur in spent sulphate copper-zinc solutions using the reagent methods of crystallization, cementation, and sedimentation. The obtained results show that the method of crystallization is easy-to-implement, though it fails to provide a required level of efficiency during the regeneration process in the solution to extract heavy metal ions (the extraction of Cu2+ and Zn2+ ions was 97.2% and 49.7%, respectively). The displacement (cementation) method does not require additional chemical reagents to implement the stages of processing, the percentage of extraction of Cu2+ and Zn2+ ions were higher in comparison to crystallization method, 99.9% and 95.4%, respectively. The advantages of the sedimentation method are the high rates of chemical transformations at technological process stages, complete deposition of heavy metal ions from spent electrolytes (99.9%) and the energy saving due to the shortened time of the regeneration process.