Data are presented on the solvent extraction of nickel and cobalt from sulfate solutions imitating the composition of partially neutralized liquors from the leaching of oxidized nickel ores using mixtures of 0.4 M CYANEX 301 (HR) with 0.4–0.5 M C7–C9 fraction of a trialkyl amine (R′3N) as the extractant. Nickel and cobalt are efficiently extracted in the pH range 6.2–6.5 and separated from Mn, Mg, and Ca in the extraction step. The separation factors for Co and Ni are high (102–103). Due to the formation of the stable adduct [R′3NH]+[R]− between the extractant components, nickel and cobalt can be stoichiometrically stripped with H2SO4 (1.0–2.0 M), allowing the production of concentrated solutions (> 100 g/L of total Co and Ni). The nickel strip liquors contain only a small amount of free acid (pH 1.5–2.0) after purification from cobalt, so they can be further processed using traditional technologies. A proposed flowsheet for nickel and cobalt recovery from such leach liquors has the advantages of ease of production of concentrated nickel and cobalt strip liquors in sulfate media and the stability of the extractant and strip liquor to oxidation by air or oxygen compared to other variants of CYANEX 301 applications.