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New adsorbents were successfully prepared by in-situ growing Fe 3 O 4 nanoparticles on halloysite nanotubes (HNTs) followed by subsequent modification with silane coupling agents. The as-prepared composites were characterized by TEM, XRD, TGA, ATR-FTIR, BET, and Zeta potential. The results confirm that Fe 3 O 4 nanoparticles were successfully decorated on internal nanotube surfaces and silane coupling agents were grafted onto the external surfaces. Among the four types of silane coupling agents modified HNTs/Fe 3 O 4 , anilino-methyl-triethoxysilane (KH-42) modified HNTs/Fe 3 O 4 composite exhibits the highest capacity for single adsorption of Cr(VI) and simultaneously adsorption of Cr(VI) and Sb(V). Moreover, the maximum Sb(V) removal efficiency increases from 67.0% in the single-solute system to 98.9% in the bi-solute system, suggesting that the presence of Cr(VI) enhances the Sb(V) removal by m-HNTs/Fe 3 O 4 . ATR-FTIR and XPS results reveal the existence of N–O–Cr bonds on adsorbent surfaces in the corresponding single-solute system, while Cr–O–Sb binding forms in the bi-solute system, which is responsible for the synergistic promoting effect on simultaneous adsorption of Cr(VI) and Sb(V) by m-HNTs/Fe 3 O 4 . The present work evinces that m-HNTs/Fe 3 O 4 holds the potential in treating industrial wastewater and natrual surface water with coexisting heavy metals such as Cr(VI) and Sb(V). [ABSTRACT FROM AUTHOR]