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Unlike the reported leaching technologies of waste superalloys, the process of the “atomized spray-sulfuric acid leaching nickel and cobalt” technology was put forward in the present work according to the compositions of waste superalloys. The effects of sulfuric acid temperature, concentration, leaching time, stirring speed and size of superalloys on leaching of Ni and Co from waste superalloys have been mainly investigated, and the optimum leaching conditions were determined and reported. The leaching rates for nickel and cobalt were 96.68% and 96.63%, respectively, and the contents of nickel and cobalt in leaching slag were 6.77% and 0.96%, respectively. The obtained leaching solution containing Ni and Co could be used for production of Ni and Co products after removal.