[Asp]Cl离子液体中合成N-苄基壳聚糖的研究
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摘要
合成了天冬氨酸盐酸盐([Asp]Cl)离子液体,以其水溶液为反应介质,将壳聚糖与苯甲醛进行反应制备了N-苄基壳聚糖(NBCS)。考察了[Asp]Cl离子液体的浓度对产物NBCS产率的影响,研究了NBCS的结构与性能。结果表明:傅里叶变换红外光谱表征所合成的[Asp]Cl离子液体和NBCS为目标产物;NBCS产率随着[Asp]Cl离子液体的浓度增大而先增加后降低,当[Asp]Cl质量分数为3%时,NBCS产率最大高达133%;NBCS/二氯乙酸溶液在偏光显微镜下呈现液晶相,NBCS为溶致液晶。
The ionic liquid of aspartic acid hydrochloride([Asp]Cl) was synthesized. N-benzyl chitosan(NBCS) was prepared by reacting chitosan and benzaldehyde using an aqueous solution of [Asp]Cl ionic liquid as reaction medium. The effect of the concentration of [Asp]Cl ionic liquid on the yield of NBCS was investigated, and the structure and properties of NBCS were studied. The results showed that [Asp]Cl ionic liquid and NBCS were proved to be the target products by Fourier transform infrared spectroscopy; the yield of NBCS increased first and then decreased with the increase of [Asp]Cl ionic liquid concentration, and the maximum yield of NBCS was 133% when the mass fraction of [Asp]Cl was 3%; and NBCS/dichloroacetic acid solution showed liquid crystal phase under polarizing microscope, and NBCS was lyotropic liquid crystal.
The ionic liquid of aspartic acid hydrochloride([Asp]Cl) was synthesized. N-benzyl chitosan(NBCS) was prepared by reacting chitosan and benzaldehyde using an aqueous solution of [Asp]Cl ionic liquid as reaction medium. The effect of the concentration of [Asp]Cl ionic liquid on the yield of NBCS was investigated, and the structure and properties of NBCS were studied. The results showed that [Asp]Cl ionic liquid and NBCS were proved to be the target products by Fourier transform infrared spectroscopy; the yield of NBCS increased first and then decreased with the increase of [Asp]Cl ionic liquid concentration, and the maximum yield of NBCS was 133% when the mass fraction of [Asp]Cl was 3%; and NBCS/dichloroacetic acid solution showed liquid crystal phase under polarizing microscope, and NBCS was lyotropic liquid crystal.
引文
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[2] 徐德增,门秀龙,唐玲俊,等.N-苄基壳聚糖液晶材料的制备及表征[J].合成纤维工业,2011,34(2):7-10.
[3] 吴玉松,李珺,黄剑莹,等.N-烷基壳聚糖的合成及其溶致液晶行为[J].物理化学学报,2001,17(11):1049-1052.
[4] 董炎明,袁清.生物高分子液晶的新家族-甲壳素及其衍生物[J].高分子通报,1999(12):48-56.
[5] 董炎明,吴玉松,王勉,等.N-苄基壳聚糖的合成和液晶性表征[J].厦门大学学报(自然科学版),2001,40(1):63-67.
[6] 董奇志,郭振楚,谭凤娇.微波作用下壳聚糖的O-苄基化反应[J].合成化学,2001,9(6):560-562.
[7] 董炎明,郭振楚,吴玉松,等.热塑性甲壳素衍生物N,O-苄基壳聚糖的合成与表征[J].高等学校化学学报,2003,24(12):2230-2232.
[8] 寇元,逃过宏,何玲,等.氨基酸盐离子液体及其制备方法:1631539A[P].2005-06-29.
[9] 张莉,梁伯润.甲壳质及其衍生物溶致液晶的研究进展[J].东华大学学报(自然科学版),2002,28(2):119-124.
[10] 董炎明,樱井谦资,玉松,等.N-乙基壳聚糖的针状结晶[J].高分子学报,2002(5):662-666.