棕榈酸葡甘聚糖酯的合成及取代度的测定  

Synthesis of konjac glucomannan ester of palmitic acid and determination of degree of substitution

作　　者：黄红[1] 王雪梅[1] 郑雪琴[1] 刘俊亮[1] 

机构地区：[1]安徽大学化学化工学院,安徽合肥230039

出　　处：《安徽大学学报（自然科学版）》2009年第3期82-86,共5页Journal of Anhui University(Natural Science Edition)

基　　金：安徽省绿色高分子材料重点实验室基金资助项目

摘　　要：采用无溶剂法合成表面活性剂——棕榈酸葡甘聚糖酯（PKGM），并选择无毒复合溶剂进行分离、精制．实验确定最佳合成条件为：KGM：EP质量比为8：15，碳酸钠质量含量为1．0％，棕榈酸钠为13．5％，甘油为5％，反应时间2．5h，反应温度120—130℃．在此条件下，PKGM的产率为63．9％，取代度0．48．产物的红外吸收光谱图显示3400、1642、1077cm^-1等处与羟基有关的吸收峰明显减弱，1739cm^-1处酯羰基伸缩振动吸收峰显著增强，并在719cm^-1处出现长链亚甲基的面内摇摆振动峰，由此证明PKGM的生成．依据对反应物KGM与产物PKGM红外谱图上羟基和羰基峰的吸收强度的测定及理论推导，计算出了产物的取代度，该方法新颖、便捷，且理论上可行．In the paper, surfactant palmitoylated konjac glucomannan （PKGM） was synthesized by solventless method and refined by non-toxic compounded solvent. The optimum synthetic condition was the mass ratio of KGM to EP 8： 15, the mass concentration of sodium carbonate 1.0%, sodium palmitate 13.5%, glycerin 5%, reaction time 2.5 hours and the temperature 120 - 130℃. On this condition, the final yield was 63.9% and degree of substitution was 0.48. Infrared absorption spectra of products showed the absorption peaks of hydroxyl group obviously weaken at 3 400, 1 642, 1 077 cm^-1 ; the stretching vibration absorption peak of carbonyl enhanced evidently at 1 739cm^-1; and the plane rocking vibration peak of long chain methylene appeared at 719 cm^-1. It proved the producing of PKGM. The degrees of substitution were calculated based on absorption intensity of hydroxyl and carbonyl of KGM and PKGM in IR spectra and theoretical derivation. The method was novel, convenient and feasible in theory.

关 键 词：魔芋葡甘聚糖 棕榈酸葡甘聚糖酯 无溶剂法 取代度 

分 类 号：O636.1[理学—高分子化学]