The separation of rhenium from molybdenum in aqueous solution has always been a problem in hydrometallurgy. The separation of rhenium from the electro-oxidation leachate of molybdenite and its mechanism were investigated. The results show that pH of the leachate significantly affects adsorption rate compared with other experimental parameters. When temperature is 30 ℃, pH=8, and adsorbing time is 1 h, adsorption rates of rhenium and molybdenum are 93.46% and 3.57%, respectively, and separation factor of D301 resin for rhenium and molybdenum is 169.56. In addition, the separation factor is higher when the initial molybdenum concentration in model solution is increased. The saturated adsorption capacity of D301 resin for molybdenum and rhenium calculated based on simulated results are 4.263 3 mmol/g and 4.235 5 mmol/g, respectively. D301 resin is an effective separation material of rhenium from electric-oxidation leachate of molybdenite. The adsorption kinetics results also show that the adsorption of rhenium is easier than that of molybdenum, and the adsorption process of D301 for rhenium and molybdenum may be controlled by liquid film diffusion. The separation of rhenium from molybdenum in aqueous solution has always been a problem in hydrometallurgy. The separation of rhenium from the electro-oxidation leachate of molybdenite and its mechanism were investigated. The results show that pH of the leachate significant affect adsorption rate compared with other The adsorption rates of rhenium and molybdenum are 93.46% and 3.57%, respectively, and separation factor of D301 resin for rhenium and molybdenum is 169.56. In addition , the separation factor is higher when the initial molybdenum concentration in model solution is increased. The saturated adsorption capacity of D301 resin for molybdenum and rhenium calculation based on the simulated results are 4.263 3 mmol / g and 4.235 5 mmol / g, respectively. D301 resin is an effective separation material of rhenium from electric-oxidation leachate of molybdenite. The adsorption kinetics results also show that t he adsorption of rhenium is easier than that of molybdenum, and the adsorption process of D301 for rhenium and molybdenum may be controlled by liquid film diffusion.