To provide a method capable of selectively separating and recovering uranium included in a sulfuric acid leaching liquid of uranium ores from impurities and selectively separating and recovering valuable metals in these impurities.

The sulfuric acid leaching liquid of the uranium ores contg. molybdenum, nickel and impurities, such as arsenic, in addition to the uranium is brought into contact with a porous methylene phosphonic acid type chelate resin, by which the uranium and the molybdenum are selectively adsorbed in the resin. The molybdenum is eluted by using an aq. sodium acetate soln. from the methylene phosphonic acid type chelate agent adsorbing the uranium and the molybdenum. The uranium is then eluted by using an aq. sodium carbonate soln. The molybdenum eluate is treated by the aminomethylene phosphonic acid type chelate agent, by which the trace uranium may be adsorbed away. The nickel and arsenic in the sulfuric acid leaching liquid from which the uranium and the molybdenum are removed may be separated by treating the eluate with the iminodiacetic acid type chelate resin.