Study on the preparation and mechanism of chitosan-based nano-mesoporous carbons by hydrothermal method

In this paper, the hydrothermal method to synthesize and characterize nano-mesoporous carbons and their synthesis mechanism are reported. Using tri-block Pluronic F127 as a structuring agent and chitosan (CS) as a carbon source, the nano-mesoporous carbons were synthesized by a one-step sol polymerization and hydrothermal process, followed by carbonization at high temperature. The pore structure of the carbon materials was characterized by physical adsorption analyzer, and the morphology was characterized by SEM and TEM. Fourier-transform infrared, Raman and x-ray photoelectron spectroscopy were used to study the synthesis mechanism. The results showed that the self-assembly polymerization reaction between CS and F127 in a weakly acidic system was only implemented driven by the hydrogen bond auxiliary electrostatic interactions initiated by protonated amino groups. The nitrogen from amino groups and acetylamino groups, the oxygen in acetylamino groups, hydroxyl groups and the glycosidic bonds of CS, and the oxygen from the hydrophilic segments of F127 were the main active sites. The mesoporous material possesses a high Brunauer-Emmett-Teller surface area (163 m²/g) and large pore volume (0.462 cm³/g) with pore diameter around 2.1 nm. The nitrogen content was 1.08% and existed in the pore wall as the form of pyridine, pyrrole and quaternary nitrogen.