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An alternative process of pre-roasting, phosphoric acid leaching followed by solvent extraction of a limonitic laterite ore was described in this work, with emphasis on the solvent extraction of Ni and Co from the phosphoric acid leaching solution by P204 and P507. First, the pH value of the leaching solution was adjusted using ammonia to reduce the content of Al³⁺ and Fe³⁺ by precipitation, then the content of Al³⁺, Fe³⁺ and Mn²⁺ were further decreased by extraction using P204. At last, Ni²⁺ and Co²⁺ were separated by three-stage extraction using P507. After extraction, the extraction ratio of Co²⁺ was 96.61%, while that of Ni²⁺ was 12.32%, and the selective extraction of Ni²⁺ and Co²⁺ could be realized.