One-Pot Synthesis of Chitosan/Layered Double Hydroxide Composite and Its Sorption Properties Toward Hexavalent Chromium

A one-pot strategy was developed for preparing a chitosan/Mg–Fe layered double hydroxide (LDH) composite by alkaline coprecipitation from an acidic chitosan solution containing Mg(II) and Fe(III) precursors, avoiding separate LDH synthesis and subsequent incorporation into chitosan. X-ray diffraction confirmed LDH formation within the chitosan matrix, and ICP analysis indicated an LDH-equivalent content of approximately 4.1 wt.% on an anhydrous basis. The composite exhibited enhanced chromate adsorption compared with both starting components. The experimental plateau adsorption capacity reached 137.4 mg/g, exceeding those of chitosan (92.2 mg/g) and Mg–Fe LDH (53.5 mg/g). Nonlinear isotherm fitting showed that Mg–Fe LDH was better described by the Freundlich model, whereas chitosan and the composite were better described by the Langmuir model. The kinetic behavior followed the pseudo-second-order equation, while Weber–Morris analysis indicated multistep uptake involving surface interaction and diffusion-related processes. In simulated groundwater containing chloride, bicarbonate, and sulfate, the composite removed 82% of Cr(VI) at 1.0 g/L. It also retained complete chromate uptake over five sorption/desorption cycles, although desorption efficiency decreased from 97.3% to 90.3%. A limitation of this study is that performance was evaluated mainly in batch systems and simplified simulated groundwater; validation with real contaminated waters and dynamic flow conditions is still required.