Separation and Purification Technology, cilt.401, 2026 (SCI-Expanded, Scopus)
This study investigates m-nitrophenol (mNP) adsorption onto β-cyclodextrin nanosponges (β-CDNSs) and their regeneration using supercritical CO2 (scCO2). The β-CDNSs synthesized via epichlorohydrin (EPI) crosslinking were characterized using Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET) analysis, and zeta potential measurements. Batch adsorption experiments showed that operational parameters, including mNP concentration, adsorbent dosage, temperature, pH, agitation speed, and particle size, significantly influenced performance, yielding 59.15 ± 2.56% removal efficiency and 9.86 ± 0.43 mg/g adsorption capacity under selected conditions (C0 = 100 mg/L, m/V = 6 g/L, T = 25 °C, pH = 5.5, N = 200 rpm, Dp = 150–500 μm, t = 120 min). Co-existing inorganic ions, humic acid, mixed-ion systems, and tap water caused modest changes in removal efficiency, indicating preliminary matrix tolerance under simplified aqueous conditions. Kinetic modelling, supported by operating-parameter experiments, suggested a stage-dependent multistep uptake process without a single dominant rate-controlling step. Isotherm modelling indicated non-ideal equilibrium behavior, best described by the Redlich–Peterson model, although this remains a descriptive representation rather than definitive evidence of heterogeneous or multisite adsorption. Thermodynamic analysis suggested a weakly favorable and exothermic adsorption process based on an apparent concentration-based framework. Complementary density functional theory (DFT) and molecular docking analyses provided qualitative molecular-level support, suggesting that hydrogen bonding, hydrophobic inclusion-like interactions, and dispersion forces may contribute to mNP retention. The scCO2-assisted regeneration at 40 oC and 300 bar with 5% (v/v) ethanol achieved high desorption efficiency (98.45 ± 1.25%) and maintained stable adsorption–desorption performance up to 12 cycles, supporting β-CDNS structural stability and reusability, as confirmed by post-regeneration characterization.