In this study, a graphene oxide metal–organic framework (MIL-53(Fe)/GO) composite adsorbent was successfully synthesized using a simple method at room temperature.

Contamination of water sources by toxic antimony Sb­(III) ions poses a threat to clean water supplies. In this regard, we have prepared a mesoporous silica nanoparticle (MSN)-derived adsorbent by reverse microemulsion polymerization, using cetyltrimethylammonium chloride (CTAC) and triethanolamine (TEA) as co-templates. The physical and chemical properties were characterized using advanced tools. The MSN exhibits a higher surface area of up to 713.72 m2·g–1, a pore volume of 1.02 cm3·g–1, and a well-ordered mesoporous nanostructure with an average pore size of 4.02 nm. The MSN has a high adsorption capacity for toxic Sb­(III) of 27.96 mg·g–1 at pH 6.0 and 298 K. The adsorption data followed the Langmuir isotherm, while the kinetics of adsorption followed the pseudo-second-order model. Interestingly, the effect of coexisting iron showed a promoting effect on Sb­(III) uptake, while the presence of manganese slightly inhibited the adsorption process. The recyclability of the MSN adsorbent was achieved using a 0.5 M HCl eluent and reused consecutively for three cycles with a more than 50% removal efficiency. Moreover, the characterization data and batch adsorption study indicated physical adsorption of Sb­(III) by mesopores and chemical adsorption due to silicon hydroxyl groups.