Green Sulfation of Arabinogalactan in the Melt of a Sulfamic Acid-Urea Mixture.

Abstract

Sulfation of arabinogalactan (AG) from larch wood (Larix sibirica Ledeb.) in the melt of a sulfamic acid-urea mixture has been first examined. The impact of the AG sulfation temperature on the AG sulfate yield and the sulfur content has been established. The high sulfur content (11.3-11.6%) in sulfated AG has been obtained in the temperature range of 115-120 °C for a sulfation time of 0.5 h. The process effectively prevents molecular degradation under these conditions. The incorporation of sulfate groups into the arabinogalactan structure has been confirmed by the appearance of absorption bands in the FTIR spectrum that are typical of sulfate group vibrations. The ¹³C NMR spectroscopy study has proven that the AG sulfation in the melt of a sulfamic acid-urea mixture leads to the substitution of some free hydroxyl groups for C6, C4, and C2 carbon atoms of the AG β-D-galactopyranose units. The advantage of the proposed AG sulfation method is that the reaction occurs without solvent, and the reaction time is only 0.5 h. The kinetics of the thermal decomposition of the initial AG and sulfated AG samples have been studied. It has been found that the sulfated AG samples have a lower thermal resistance than the initial AG. The kinetic analysis has revealed a decrease in the activation energy of the thermal degradation of the sulfated samples as compared to the initial AG.