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The recovery of rhenium from waste acid is an urgent issue due to low rhenium concentration and high sulfuric acidity.To solve the problem,novel coated solvent-impregnated resins consisting of inert resins LS-300,Alamine 300-1 and the PVA film (300-CSIRs) were prepared for the separation of Re(Ⅶ) from high sulfuric acid solutions.It was shown that the PVA film coated completely on the surfaces of LS-300 resins with a thickness of 5 tm,and Alamine 300-1 distributed completely inside the porous of LS-300 resins.The adsorption fitted well with Langmuir model and pseudo-second-order model with the saturation adsorption capacity of 139.40mg·g-1.The maximum separation factor of Re(Ⅶ) versus Cu (Ⅱ) was up to 483,and 304-CSIRs had no adsorptions for As(Ⅴ).The adsorption capacity of Re(Ⅶ) onto 304-CSIRs maintained in 97.79% at the fifth adsorption-desorption cycle.99.87% of rhenium was recovered by 304-CSIRs from waste acid generated from a copper smelter.