The invention discloses a process for preparing nuclear-grade
hafnium oxide and
zirconium oxide through
solvent extractive separation of
zirconium and
hafnium. The process comprises the following steps: (1) mixing
tributyl phosphate or
tributyl phosphate and
ionic liquid, which serve as extractants, and
kerosene, which serves as a
diluent, so as to prepare an organic phase; and then, mixing the organic phase with
nitric acid, and carrying out countercurrent acidification in a
centrifugal extractor; (2) adding
zirconium oxychloride, which serves as a
raw material, into deionized water, carryingout dissolving, and then, adding
hydrochloric acid and
nitric acid into the solution, so as to prepare a feed solution containing zirconium and
hafnium; (3) carrying out countercurrent extraction onthe acidified organic phase and the feed solution containing zirconium and hafnium, prepared in the step (2), in a
centrifugal extractor; (4) carrying out back-extraction on a zirconium-containing organic phase with water, then, carrying out
hydrolysis, and carrying out
calcination, so as to obtain nuclear-grade
zirconium oxide; and (5) enriching hafnium-containing
raffinate with P204, then, carrying out back-extraction, carrying out
hydrolysis, and carrying out
calcination, so as to obtain nuclear-grade
hafnium oxide. According to the process, the problems, i.e., complicated process, much waste liquid and environmental
pollution in the prior art are solved, and the production efficiency is increased.