In this work, we report a novel type of thiol-functionalized magnetic core-shell metal-organic framework (MOF) microspheres that can be potentially used for selective removal of Hg2+ and Pb2+ in the presence of other background ions from wastewater. The monodisperse Fe3O4@Cu-3(btc)(2) core-shell magnetic microspheres have been fabricated by a versatile step-by-step assembly strategy. Further, the thiol-functionalized Fe3O4@Cu-3(btc)(2) magnetic microspheres were successfully synthesized by utilizing a facile postsynthetic strategy. Significantly, the thiol-functionalized Fe3O4@Cu-3(btc)(2) magnetic microspheres exhibit remarkably selective adsorption affinity for Hg2+ (K-d = 5.98 x 10(4) mLg(-1)) and Pb2+ (K-d = 1.23 x 10(4) mLg(-1)), while a weaker binding affinity occurred for the other background ions such as Ni2+, Na+, mg(2+), Ca2+, Zn2+ and Cd2+. The adsorption kinetics follow the pseudo-second-order rate equation and with an almost complete removal of Hg2+ and Pb2+ from the mixed heavy metal ions wastewater (0.5 mM) within 120 min. Moreover, this adsorbent can be easily recycled because of the presence of the magnetic Fe3O4 core. This work provides a promising functionalized porous magnetic Fe3O4@MOF-based adsorbent with easy recycling property for the selective removal of heavy metal ions from wastewater. (C) 2017 Elsevier B.V. All rights reserved.