DOI: 10.3390/separations13110311 ISSN: 2297-8739

Solvent-Free Synthesis of an Oxidized β-Cyclodextrin–Phytic Acid Copolymer for the Dual Removal of Heavy Metals and Organic Pollutants from Wastewater

Rasha Borini, Othman Hamed, Abdalhadi Deghles, Bahia Abu Lail, Shehdeh Jodeh, Ghadir Hanbaly, Albasheer Hanene, Raghad Taha

In this study, a novel water-insoluble copolymer of oxidized β-cyclodextrin (β-CDO) and phytic acid (PA) was designed, synthesized, and evaluated for the dual adsorption of heavy metals and organic pollutants from wastewater. β-CD was oxidized using the TEMPO/NaOCl system to yield β-CD containing carboxyl functional groups (β-CDO). The copolymer was synthesized via a solvent-free esterification method by heating the reactants at 120 °C, thereby forming phosphate ester linkages between the hydroxyl groups of β-CDO and PA. Five polymers with different ratios were prepared and characterized by FTIR, SEM, and TGA, confirming linkage formation, porous morphology, and good thermal stability of the β-CDO-co-PA copolymer. Polymer E, with a β-CDO-to-PA ratio of 3:1, exhibited outstanding adsorption capabilities. Polymer E removed 99.0% of Pb(II) from a 50 mg/L solution at pH 5 and 30 °C, reaching equilibrium within 30 min. For methylene blue (MB), it showed a removal efficiency greater than 98%, with a Qe value of 196 mg/g at pH 7.0 through β-CD inclusion complexation and electrostatic interactions with PA. In real wastewater, polymer E efficiently removed several heavy metals, including Pb (99.5%), Cr (98.6%), Cu (98.8%), and As (98.5%), through synergistic adsorption, with PA phosphate groups chelating metal ions and β-CD cavities capturing organic contaminants. The adsorption behavior followed pseudo-second-order kinetics, indicating the predominance of chemisorption, and the Langmuir isotherm, indicating monolayer coverage. Polymer E also retained more than 90% efficiency after six regeneration cycles.

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