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Extraction and separation of hexavalent molybdenum from acidic sulfate solutions using Alamine 336 as an extractant and kerosene as diluent is described. Variation of acid concentration influences the percentage of extraction of hexavalent molybdenum indicating the ion exchange type mechanism. Effect of concentration of Alamine 336 on the extraction of hexavalent molybdenum in the presence of divalent copper and trivalent iron is also presented. The upper limit of concentration of extractant for extraction of hexavalent molybdenum free from divalent copper and trivalent iron is observed with 0.1 mol/L of Alamine 336. However, when the concentration of Alamine 336 is increased to 1.0 mol/L, about 48% of copper is extracted along with molybdenum but without any iron. The method is suitable for the separation of molybdenum from copper and iron contained leach liquor. The optimized experimental parameters such as phase contact time, effect of extractant, metal, loading capacity of extractant and followed by stripping studies with ammonia, hydrogen peroxide, sodium hydroxide, sodium thiosulfate and thiourea is presented. From the above experimental data we proposed the aqueous mechanism for hexavalent molybdenum extraction processes.