Abstract:High-purity ammonium rhenate was recovered from acid leaching solution of superalloy by D296 resin adsorption, NH4SCN solution desorption, KReO4 crystal precipitation, and impurity removing with C160 resin. The results show that Re adsorption rate with D296 resin is 99.03%. Re desorption rate is 99.55% under the conditions including concentration of NH4SCN solution of 8%, volume ratio of NH4SCN desorption solution to loaded resin of 10︰1, and desorption flow rate of 1BVs/h. KReO4 is crystallized with Re crystallization rate of 95.14% by 10 times of theoretical amount of KCl. High-purity ammonium rhenate with purity of as high as 99.995% is prepared from KReO4 by impurity removal with C160 resin, ammonium hydroxide neutralization, concentrated crystallization and one time recrystallization.