The invention belongs to the technical field of
hydrometallurgy, and particularly relates to a method for separating
metal molybdenum and
rhenium from a
nickel-based
superalloy electrochemical dissolving solution, which comprises the following steps: providing the
nickel-based
superalloy electrochemical dissolving solution, and adjusting the pH value to 0-1.5; the modified MTS9570 resin is used for adsorbing the
nickel-based
superalloy electrochemical dissolving solution to obtain a
molybdenum-absorbed solution, then a
sulfuric acid solution is used for leaching, then an
ammonia water solution is used for
desorption, and a
molybdenum desorption solution is obtained; adjusting the pH value of the molybdenum-absorbed solution to 0.5-1.5, adsorbing with modified MTA1721 resin, leaching with a
sulfuric acid solution, desorbing with an
ammonium sulfate and
ammonia water
mixed solution, and desorbing with an
ammonia water solution to obtain a second-stage
rhenium desorption solution; and the molybdenum desorption solution and the second-stage
rhenium desorption solution are subjected to
evaporation concentration,
crystallization, recrystallization and high-temperature
hydrogen reduction respectively, and
metal molybdenum and rhenium are obtained. According to the method for separating rhenium and molybdenum from the nickel-based high-temperature
alloy electrochemical dissolving solution, the rhenium and molybdenum
recovery rate and rhenium purity are improved, and the process is simple, convenient and practical.