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Stone coal is carbonaceous shale which contains vanadium and small quantity molybdenum.During the acidolysis of stone coal, vanadium and molybdenum can be leached into solution together.After deacidizing the leach solution with Na2S2O3,10 vol% P204, 5 vol% TBP and 85 vol% sulfonated kerosene was used to extract vanadium and molybdenum in leach solution, and the extraction yield of vanadium and molybdenum can reach above 80%.The stripping yield of vanadium can reach above 99% when using 1.5mol/L H2SO4 as the stripping agent, and molybdenum cannot be stripped under this condition.When using 80g/L NH4HCO3 as the stripping agent, molybdenum can be stripped effectively and the stripping yield can reach above 80%.After being oxidized,vanadium could be precipitated from the vanadium stripping solution by adjusting the solution pH via adding ammonia solution.Molybdenum in stripping solution could be recovered easily via farther enrichment.