Freeze-Cast Chitosan/Resole Aerogels: Effect of Resole Fraction on Properties and Their Efficiency for Cr(VI) Uptake

Aligned CS/Rx aerogels were fabricated by inducing non-directional ice growth (freeze-molding) followed by low-temperature curing, resulting in monoliths with interconnected channels, a high void fraction, and moldability. The swelling index (S%) was calculated to be 1029, the apparent density 0.496 g·cm−3, and the estimated porosity 90% based on micrographic analysis. Aerogels have mechanical behavior Shore A hardness greater than 25. Batch metal removal tests were performed (10 mL, 100 mg·L−1 Cr(VI), 0.19 g adsorbent, 24 h, and pH 5–5.5), and the material achieved 95% metal removal. Additional kinetic and isothermal results were obtained using CS85R15 on a packed column (20 to 140 mg·L−1, 1000 mL Cr(VI), 0.80 g adsorbent, 24 h, and pH 5–5.5). Equilibrium data were consistent with a heterogeneous surface hosting a specific site, as reflected in the joint Freundlich/Langmuir fit (qmax 100.8 mg·g−1 for Langmuir). This confirmed the preservation of chitosan functionalities (–OH/–NH) after processing, while XPS detected chromium on the surface with signals consistent with the partial reduction of Cr(VI) to Cr(III) on the aerogel surface. This highlights the relevance of adsorption-based technologies for water remediation, where high-porosity and low-density materials allow for short diffusion pathways and capture electrostatics by protonated amines and redox conversion of hazardous substances. The soft-cure freeze-molding technique is simple, scalable, and compatible with packed-bed/column operation, providing a material platform for tailoring the microstructure (sheets and channels) and surface chemistry to regenerable sorbents for industrial wastewater treatment.