Abstract: Given the surging demand for nickel and cobalt fueled by the rapid expansion of the electric vehicle industry, it is imperative to develop efficient and eco-friendly metallurgical routes for extracting these metals. This work introduces a sustainable and effective method for nickel and cobalt extraction from Ni-Co-Fe alloy powder, which was obtained from a limonitic laterite ore through selective reduction-magnetic separation. The leaching efficiencies of Ni, Co and Fe were 89.4%, 94.8% and 96.5%, respectively, under the leaching conditions of 3M H2SO4, 85°C and a liquid-to-solid ratio of 10 mL/g for 90 min. The incorporation of H2O2 enhanced the leaching efficiencies of Ni, Co and Fe. The redox potential of the solution plays a crucial role in the acid dissolution, with H2O2 modification enhancing Ni and Co dissolution. Phosphate precipitation facilitated the removal of iron from the leachate, achieving 96.1% iron removal ratio with only a 2.26% nickel loss.