The hydrometallurgical separation and enrichment processes provide an effective way to selectively recover metals from relatively dilute multicomponent sulfuric acid leach solutions. The multicomponent leach solution utilised in this study contained 0.3 g/L Cu, 0.34 g/L Ni, 0.13 g/L Co, and 2.96 g/L Fe, which was obtained after high-pressure oxidative acid leaching (HPOAL) of the copper-nickel smelter slag. The solvent extraction (SX), precipitation, and xanthate complexation processes were employed to recover and upgrade Cu, Ni, and Co from the leach solution. Batch SX tests were carried out using a countercurrent two-stage mixer settler extraction column, and LIX 984N (10 per cent v/v) as a copper extractant. Fundamental parameters influencing the extraction process such as pH, mixing speed, H2SO4 concentration, and organic/aqueous (O/A) phase ratio were investigated. For copper enrichment in solution, a combination of two extraction stages and two stripping stages were employed. Copper was successively separated from Fe, Ni, and Co under optimised extraction conditions (pH 2, 400 rev/min, O/A 0.25, and 20 min contacting) and stripping conditions (175 g/L H2SO4, 400 rev/min, O/A 4, and 20 min contacting). About 97 per cent of copper was extracted with low co-extraction of Fe, Ni, and Co of about 5.90 per cent, 1.47 per cent, and 2.53 per cent, correspondingly. A final Cu-rich solution containing 23 g/L Cu was obtained with a very low Fe concentration of 0.05 g/L. Additionally, for iron removal from the Ni/Co raffinate solution, more than 99 per cent of iron was precipitated at pH 4 by the addition of a calcium carbonate (CaCO3) suspension, with low co-precipitation of nickel and cobalt of around 3.68 per cent and 2.27 per cent, respectively. Furthermore, about 83.6 per cent of nickel and 99.4 per cent cobalt were co-precipitated from the solution by potassium amyl xanthate (PAX) solution at pH 6. The Ni and Co xanthate complexes were thermally decomposed and recovered as cobalt oxide (CoO) and nickel sulfide (NiS) solids.