Copper and zinc were recovered from waste diamond cutters through leaching with an ammonia–ammonium sulfate system and air as an oxidant. The effects of experimental parameters on the leaching process were investigated, and the potential–pH (E–pH) diagrams of Cu–NH₃–SO₄ ²⁻–H₂O and Zn–NH₃–SO₄ ²⁻–H₂O at 25°C were drawn. Results showed that the optimal parameters for the leaching reaction are as follows: reaction temperature, 45°C; leaching duration, 3 h; liquid-to-solid ratio, 50:1 (mL/g); stirring speed, 200 r/min; ammonia concentration, 4.0 mol/L; ammonium sulfate concentration, 1.0 mol/L; and air flow rate, 0.2 L/min. The results of the kinetics study indicated that the leaching is controlled by the surface chemical reaction at temperatures below 35°C, and the leaching is controlled by diffusion through the product layer at temperatures above 35°C.