The current study aimed to investigate the effect of counterions on hydrothermally synthesized hydrozincite (zinc hydroxide carbonate), which was thermally converted to generate ZnO nanostructures, which are an efficient nanoadsorbent for the removal of Reactive Black 5 (RB5) dye from wastewater. Hydrozincite nanospheres and flower-like structures were hydrothermally prepared using various zinc salts (sulfate, acetate, and nitrate) and ammonium carbonate in a molar ratio of 1 : 3, respectively, at 120 °C for 3 h. The morphology and crystallite size of the hydrozincite precursor were effectively controlled via the parameters of the hydrothermal reaction. Interestingly, sulfate was the optimum counterion, as zinc sulfate salt produced pure hydrozincite nanospheres with the smallest crystallite size (∼13.57 nm), which were consequently thermally decomposed at 400 °C for 1 h to produce pure nanosized ZnO (∼10 nm). The compositions of the as-synthesized products were determined by means of FT-IR, FE-SEM, HR-TEM, XRD, zeta potential, BET, and thermal analyses. An adsorption study showed a much higher adsorption capacity (80.9 mg g−1) of the as-prepared ZnO nanoparticles toward RB5 dye. The adsorption of RB5 dye followed pseudo-second-order kinetics. In addition, the equilibrium adsorption of RB5 dye was best described by a Langmuir isotherm model and the calculated thermodynamic parameters, ΔG0 (from −4.027 to −7.533 kJ mol−1), ΔH0 (30.798 kJ mol−1), and Ea (29.105 kJ mol−1), indicate the spontaneous, endothermic, and physisorptive nature of the adsorption process.
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