Abstract: A process of recovering uranium values as uranium peroxide from an aqueous uranyl solution containing dissolved vanadium and sodium impurities by treating the uranyl solution with hydrogen peroxide in an amount sufficient to have an excess of at least 0.5 parts H.sub.2 O.sub.2 per part of vanadium (V.sub.2 O.sub.5) above the stoichiometric amount required to form the uranium peroxide, the hydrogen peroxide treatment being carried out in three sequential phases consisting of I, a precipitation phase in which the hydrogen peroxide is added to the uranyl solution to precipitate the uranium peroxide and the pH of the reaction medium maintained in the range of 2.5 to 5.5 for a period of from about 1 to 60 minutes after the hydrogen peroxide addition; II, a digestion phase in which the pH of the reaction medium is maintained in the range of 3.0 to 7.0 for a period of about 5 to 180 minutes and III, a final phase in which the pH of the reaction medium is maintained in the range of 4.0 to 7.