A series of three-dimensional (3D) porous nanocomposites, comprised of partially reduced graphene oxide (pRGO) and CO32- containing Mg-Al layered double hydroxide, were synthesized in two steps. In the first step, graphene oxide (GO) was fabricated by a modified Hummers' method, and, subsequently, in the second step layered double hydroxide (LDH) nanosheets were homogeneously grown on the surface of the GO sheets by an in situ crystallization approach, involving a facile coprecipitation technique. The alkaline medium used for the in situ growth of LDH on the GO surface resulted in the partial reduction of GO to pRGO, which was confirmed by XRD. XRD also revealed the successful formation of crystalline LDH nanosheets on the surface of pRGO, whereas FTIR spectroscopy confirmed the presence of different functional groups in the nanocomposites. Nitrogen adsorption-desorption studies of the prepared nanocomposites revealed them as high surface area porous materials. Electron microscopic techniques, like TEM and SEM, confirmed that the architectures of the prepared nanocomposites displayed an interconnected 3D network, where a number of LDH nanosheets were interwoven on the surface of pRGO. The elemental mapping and EDX analysis qualitatively confirmed the presence of all of the expected elements in the fabricated nanocomposites. Because of the unique 3D porous network and the presence of a large number of oxygen-containing functional groups, the prepared nanocomposites proved suitable for the adsorption of Pb2+ ions from aqueous solution with a maximum adsorption capacity of 116.2 mg g-1. Equilibrium was achieved after 180 min on conducting the adsorption experiments at pH 4.5. Desorption experiments established the possibility of recovering the metal ions as well as the regeneration of adsorbents for repeated use.
Keywords: adsorption; coprecipitation; graphene oxide; layered double hydroxides; nanocomposites.