合成了甘氨酸盐酸盐离子液体([Gly]Cl),由^1H-NMR对其结构进行了确证,并以其质量分数2%的水溶液为反应介质,制备水溶性丁二酰化壳聚糖。用XRD和FT-IR对产物进行了表征,结果表明:壳聚糖(CS)中引入了丁二酰基,并削弱了壳聚糖分子内和分子间的氢键作用,大大改善其水溶性。考察了反应时间、温度和反应物配比对丁二酰化壳聚糖取代度(DS)的影响,得到较佳的反应条件:反应时间4h,n(丁二酸酐):n(壳聚糖)=2.75,反应温度40℃,在该条件下丁二酰化壳聚糖的取代度达到90%以上。离子液体具有重复使用性,反应后的离子液体未经处理重复使用3次后,丁二酰化壳聚糖的取代度仍大于90%。
The [Gly]Cl ionic liquid was synthesized and its structure was confirmed by ^1H-NMR,and then the succinyl chitosan was prepared successfully in the aqueous solution of 2% [Gly]Cl ionic liquid. The structure of the product was characterized by XRD and FT-IR. The results indicate that the -OCH2CH2COOH is introduced to the chitosan molecule. The intra and inter hydrogen bonds in the chitosan are weakened,therefore,its water-solubility is improved remarkably. The influences of the mole ratio of succinic anhydride and the amino group of chitosan,and the reaction time and temperature on the degree of substitution were investigated respectively. The suitable reaction conditions found are as follows:n(succinic anhydride):n(chitosan)=2.75:1,reaction time is 4 h and reaction temperature is 40℃. Under above conditions,the degree of substitution of succinyl chitosan can be over 90%. The reusability of the ionic liquid was also investigated,and it was found that the [Gly]Cl ionic liquid can be reused for 3 times without any retreatment,and the degree of substitution still can keep being above 90%.