Separation of hafnium from zircon leach solution using anion-exchange resin and production of high-purity zirconia for nuclear applications

The ion exchange process using an anion exchange resin (Bio-Rex 5) was employed with batch and column techniques to isolate nuclear-grade zirconium/hafnium from a leach solution of zircon ore. Batch studies were conducted to optimize the conditions for sorption and desorption of Zr(IV) and Hf(IV). The highest separation factor of 10.3 was achieved under equilibrium conditions of 11.0 mol/L HCl, contact time of 30.0 min, solution volume-to-mass of resin ratio of 0.10, and 15 °C. The sorption process for both metals obeyed a pseudo-second-order model and the experimental sorption data was well-described by both Langmuir and Freundlich models. The maximum sorption capacities were determined to be 46.2 mg/g for Zr(IV) and 37.8 mg/g for Hf(IV). The Zr(IV) and Hf(IV) ions were effectively desorbed by 0.1 mol/L nitric and 2.0 mol/L hydrochloric acid solutions, respectively, with total yields of 89.7 % Zr(IV) and 85.8 % Hf(IV) via multistage desorption processes. In both batch and column techniques, the resin exhibited sorption selectivity for Zr and Hf over interfering elements in the hydrochloric acid leach solution of zircon sand. The loaded resin from real leach solution was subjected to desorption, zirconium sulfate precipitation, and calcination at 650  °C, resulting in a pure zirconia powder suitable for nuclear applications. This technique presents a promising effective method for the selective separation and recovery of high-purity zirconium and hafnium from their natural sources.