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Mesoporous materials substrate functionalized with-NH2 groups were prepared in selective recovery of Mo(Ⅵ) from Re(Ⅶ)-containing aqueous solutions.The NH2/Mesoporous materials adsorbents were prepared by grafting of synthesized different mesoporous materials substrate with different concentrations of 3-aminopropyltriethoxysilane (APTES) in order to determine the optimum amine group concentration.