A two-step process of leaching of soluble fluoride with water and leaching of insoluble electrolyte with aluminum anodizing wastewater was adopted to deal with the spent cathode pot-lining. The effects of stirring speed, ratio of solid to liquid and temperature on the leaching rate of electrolyte were examined. And the corresponding reaction kinetics was also analyzed. The results show that leaching kinetics control link insoluble electrolyte is well interpreted with the unreacted shrinking core model under diffusion reaction control. The leaching rate of electrolyte can be improved by increasing the reaction temperature and reaction time. And the apparent activation energy of the reaction is 12.71 kJ/mol. The spent cathode pot-lining after leaching can be blended into the original cathode, and reach the specifications for resistivity, have a good economical and social benefit.