A simple and efficient method for the preparation of a novel soluble chitosan derivative, diethoxy phosphoryl chitosan （PH-chitosan）, has been developed. Ph-chitosan was characterized by elemental analysis, FT-IR, NMR, ICP, XRD, TG and SEM, respectively. The chemical identity of PH-chitosan was determined by FT-IR and confirmed by NMR, and those results unequivocally demonstrated that diethoxy phosphoryl groups were grafted onto the amino and hydroxyl groups of chitosan. The results of XRD indicated that the crystalline structure of chitosan was destroyed due to the incorporation of diethoxy phosphoryl group resulting in loss of hydrogen bond. The analysis of TG demonstrated that PH-chitosan was less thermal stable than chitosan. This simple synthetic method provided a new and available approach to prepare a soluble high molecule weight chitosan derivative.
以水杨醛(SA)为改性试剂,在离子液体1-丁基-3-甲基咪唑氯盐(BmimCl)介质中对壳聚糖(CS)进行了席夫碱化改性研究.考察了反应条件(反应物摩尔比、反应温度和反应时间)对产物取代度的影响,得到的最佳反应条件为:0.15 g壳聚糖溶解于10 g BmimCl中,壳聚糖中氨基与水杨醛摩尔比为1∶2.5,反应温度为80℃,反应时间为2 h.在最佳反应条件下,壳聚糖水杨醛席夫碱衍生物的取代度可达29.2%.利用红外、核磁及XRD等表征技术对产物进行了表征,并在最佳试验条件下合成了系列壳聚糖席夫碱衍生物.
