This study focuses on the development of eco-friendly biobased adsorbents through a sustainable hydrothermal and freeze-drying synthesis process, utilizing cost-effective bio-sourced materials to minimize energy consumption and waste. The biobased adsorbents were elaborated using hydroxyethyl cellulose-ionic liquids and bentonite clay. The elaborated biocomposites were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy/attenuated total reflection (FTIR/ATR), thermogravimetric analysis (TGA), and electron microscopy-energy dispersive X-ray (SEM–EDX), Brunauer–Emmett–Teller (BET) and zeta potential (ZP). Structural analysis confirms the intercalation and incorporation of HEC-ILs polymeric chains into Be-Na matrix and the formation of biocomposites. The [HEC-ILs/Be-Na] composite was subsequently employed for solid-phase extraction of Co(II) by investigating the effect of pH, initial Co(II) concentrations, time, temperature, and the presence of co-existing ions (Na(I), Li(I), Mn(II), Ni(II), and Al(III)). The adsorption kinetics of Co(II) metal ions were suitably characterized using the pseudo-second-order model (with R2 > 0.99). Furthermore, the adsorption isotherms conformed to the Langmuir model (with R2 > 0.97), suggesting a chemisorption process with an adsorption capacity of 69.8 mg/g. The thermodynamic study reveals that the adsorption process exhibits characteristics of spontaneity and endothermicity (ΔH° = 74.197 kJ mol−1, ΔG° < 0 kJ mol−1). The proposed mechanism for Co(II) adsorption on the developed biocomposite involves electrostatic interactions, ion exchange, and anion-π interactions. The biobased composite exhibited remarkable selectivity for Co(II) and demonstrated great potential as an adsorbent for industrial applications.
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