Study of the microstructure of chitosan aerogel beads prepared by supercritical CO2 drying and the effect of long-term storage

Abstract

In order to investigate the pore properties and effect of storage time on the microstructure of CO₂-dried aerogels, chitosan aerogel beads were obtained from chitosan hydrogels with an initial concentration in the range of 1.5–3.0 wt% through SCCO₂ drying and freeze-drying (as a comparison). The SCCO₂-dried chitosan aerogels showed a three-dimensional network structure, and had higher BET surface area (200 m² g⁻¹) and higher crystallinity (0.62/XRD, 0.80/ATR-FTIR) than the freeze-dried aerogels. The stability of the microstructure of the SCCO₂-dried chitosan aerogel beads during 10 months was studied. The BET surface area of the aerogel beads at each concentration declined by 30.5% at 2 months, 56.7% at 6 months and 67.2% at 10 months. Accelerated aging tests of the chitosan aerogel beads were carried out to study the effect of humidity on the chitosan aerogel beads. The average diameter of the chitosan aerogel decreased from 2.3 mm to 0.9 mm when stored at 65 °C with 90% relative humidity (RH). In contrast, there was no obvious change during storage at 65 °C with 20% RH. The amount of adsorbed water increased from 4% to 12% at 65 °C with 90% RH for 96 h, and the bound water content of the aerogel beads gradually increased. This study demonstrates that SCCO₂-dried chitosan aerogel beads could be better at maintaining their mesoporous structure, and the adsorption of water from the surrounding air had a significant effect on the microstructure and shrinkage of the chitosan aerogel beads.