| Summary: | Three-dimensional (3D) urchin-like MnO<sub>2</sub>@poly (sodium 4-styrene sulfonate) (PSS)/poly (diallyl dimethylammonium chloride) (PDDA)/PSS particles were prepared via the layer-by-layer (LBL) assembly of polyelectrolytes for the extraction of Zn<sup>2+</sup> from alkaline media. The adsorption performance of Zn<sup>2+</sup> on MnO<sub>2</sub>, MnO<sub>2</sub>@PSS/PDDA/PSS, and MnO<sub>2</sub>@(PSS/PDDA)<sub>3</sub>/PSS was investigated in batch experiments. The adsorption of Zn<sup>2+</sup> on MnO<sub>2</sub>@PSS/PDDA/PSS has been studied under various conditions, such as initial Zn<sup>2+</sup> concentration, adsorbent dosage, the solution’s pH, and reaction time. The Zn<sup>2+</sup> adsorption process is well represented by the pseudo-second-order kinetic model, and the equilibrium data fit the Freundlich isotherm well. MnO<sub>2</sub>@PSS/PDDA/PSS also showed high efficiency for Pb<sup>2+</sup> and Cu<sup>2+</sup> removal from slightly alkaline water. Thus, our research provides a deep insight into the preparation of 3D manganese oxides with polyelectrolyte films for the extraction of heavy metal ions, such as Pb<sup>2+</sup>, Cu<sup>2+</sup>, and Zn<sup>2+</sup>, from slightly alkaline wastewater.
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