Levdansky Vladimir A, Levdansky Alexander V, Malyar Yuriy N, Ivanenko Timur Yu, Fetisova Olga Yu, Kazachenko Aleksandr S, Kuznetsov Boris N
Institute of Chemistry and Chemical Technology SB RAS, Federal Research Center, Krasnoyarsk Science Center SB RAS, Akademgorodok 50, Bld. 24, Krasnoyarsk 660036, Russia.
School of Non-Ferrous Metals and Material Science, Siberian Federal University, Pr. Svobodny 79, Krasnoyarsk 660041, Russia.
Polymers (Basel). 2025 Feb 27;17(5):642. doi: 10.3390/polym17050642.
Sulfation of arabinogalactan (AG) from larch wood () 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 C 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.
首次研究了落叶松木阿拉伯半乳聚糖(AG)在氨基磺酸 - 尿素混合物熔体中的硫酸化反应。确定了AG硫酸化温度对AG硫酸盐产率和硫含量的影响。在115 - 120°C的温度范围内,硫酸化时间为0.5小时,得到的硫酸化AG中硫含量较高(11.3 - 11.6%)。在这些条件下,该过程有效地防止了分子降解。FTIR光谱中出现典型的硫酸根基团振动吸收带,证实了硫酸根基团已掺入阿拉伯半乳聚糖结构中。13C NMR光谱研究证明,在氨基磺酸 - 尿素混合物熔体中对AG进行硫酸化会导致AGβ - D - 吡喃半乳糖单元的一些游离羟基被C6、C4和C2碳原子取代。所提出的AG硫酸化方法的优点是反应在无溶剂条件下进行,且反应时间仅为0.5小时。研究了初始AG和硫酸化AG样品的热分解动力学。发现硫酸化AG样品的热稳定性低于初始AG。动力学分析表明,与初始AG相比,硫酸化样品热降解的活化能降低。