Effects of deacetylation degree of chitosan on the structure of aerogels

Chitosan aerogels, obtained by (supercritical) CO2 drying of hydrogels, are novel adsorbents because of their large surface area and high porosity. Intrinsic properties of chitosan such as molecular weight (MW) and degree of deacetylation (DDA) had large impacts on the characteristics of chitosan aerogels. Although there are a few studies about the effects of solely DDA or MW on aerogel structure, none of them has focused on the mutual effects. The study aims to investigate the combined effects of MW and DDA of chitosan on aerogel properties. Hydrogels were produced in beads form by physical gelation of the chitosan solutions (2 % w/v in acetic acid of 1 %, v/v) in an alkaline environment (NaOH, 4 N). Supercritical CO2 dried aerogels were examined with respect to the bulk density, diameter as well as pore characteristics, and surface area by Barrett-Joyner-Halenda (BJH) and Brunauer-Emmett-Teller (BET) methods, respectively. Morphologies of aerogels were also examined by Scanning Electron Microscopy (SEM) images and structural changes of aerogels were observed by Fourier Transform Infrared (FTIR) Spectroscopy. Additional to BET-BJH analysis, proton relaxation dispersion was measured by Fast Field Cycling NMR (FFC-NMR) to determine the pore volume of the aerogels. Compact structures were obtained for higher MW chitosan and lower MW chitosans with higher DDA increasing the aerogel diameters. All types of aerogels obtained by different chitosan characteristics (MW and DDA) showed a porous structure and the highest DDA with the lowest MW caused the minimum bulk density with the highest water absorption rate. Although different N2 adsorption-desorption profiles were obtained in terms of pore volumes; all aerogels had Type IV isotherms with Type H1 hysteresis curve. FFC-NMR experiments showed that the coherence length values were associated with the pore volumes and FFC-NMR experiments were found to be meaningful as supportive experiments for the characterization of aerogels.