Abstract: Diamond is synthesized using graphite and metal catalyst at high temperature and high pressure. However, diamond in the synthetic block is tightly wrapped by graphite, catalyst metal and etc, which is difficult to purify through general physical methods. Electrolysis is used to oxidize the metal in the synthetic block on the anode into metal ions and thus solved in the solution, and then the ions are migrated to the cathode through the solution to recover the metal, which is a more efficient and environmentally friendly method at present. Through the electrolysis experiment, the influences of the main components of electrolyte and the conditions of electrolysis process on the efficiency of electrolysis are analyzed.The results show that the best mass concentration of activator in the additives is 15-30 g/L and the best mass concentration of composite stabilizer is 25-30 g/L, the additives can significantly improve the performance of electrolyte. The pH value of the electrolyte is 2-4, electric cathode and anode distance is 50-250 mm and the current of control cabinet is 4000-4200 A, the electrolysis efficiency can be significantly improved.