Black shale is one of the most representative sources of vanadium, nickel and molybdenum in China. Due to the poor endowment of minerals in black shale, V, Ni, Mo and other metals complex co-associated endowment state, extraction is difficult and long-term unused, resulting in a significant waste of resources. In this paper, it is shown that V, Ni and Mo can be obtained from black shale by a stepwise oxidation leaching process. In a first leaching process, V and Ni are effectively leached simultaneously. Mo is left in the residue. The leaching efficiency of V, Ni and Mo was 86.81%, 89.19% and 5.80% respectively under the leaching conditions of 35wt.% H2SO4, 4wt.% CaF2, 1.2:1 liquid to solid ratio (L/kg), 95℃ and 8h. The residue was then leached twice. The leaching efficiency of molybdenum was 91.10% under the leaching conditions of 25wt.% H2SO4, 8wt.% NaClO3, 1.5:1 liquid to solid ratio (L/kg), 45℃ and 7h. V2O5 products have been successfully prepared, the purity of V2O5 reaches 98.34%. A stepwise oxidation leaching method has been proposed to separate the vanadium, nickel and molybdenum in the leaching process. Vanadium, nickel and molybdenum can be effectively extracted from the black shale by the stepwise oxidation leaching process to maximize the utilization of the resources.
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