共溶剂存在下N-烯丙基吡啶氯盐离子液体对纤维素的溶解性能研究  

STUDY ON THE DISSOLUTION OF CELLULOSE IN N-ALLYLPYRIDINIUM CHLORIDE IONIC LIQUID AND CO-SOLVENT COMPOSITES

作　　者：赵地顺[1] 付林林[1,2] 张娟[1] 李贺[1] 刘猛帅[1] 付江涛[1] 王薇[1] 

机构地区：[1]河北科技大学化学与制药工程学院,石家庄050018 [2]河北华飞科技咨询有限责任公司,石家庄050032

出　　处：《高分子学报》2012年第9期937-942,共6页Acta Polymerica Sinica

基　　金：国家自然科学基金(基金号20976107);河北科技大学2011年度大学生科技创新基金资助项目

摘　　要：采用一步法合成N-烯丙基吡啶氯盐离子液体([APy]Cl),考察其对纤维素的溶解性能.结果发现,在120℃下对棉浆粕(聚合度(DP)=556)的溶解度可高达19.71%,但再生后聚合度为223,热降解严重.通过添加不同种类共溶剂的方法克服此缺点.结果表明,有机溶液(DMSO,DMAc,DMF或吡啶)作为[APy]Cl的共溶剂时,[APy]Cl/DMAc复合溶剂对棉浆粕的溶解效果最佳,100℃下溶解度为15.03%,再生后聚合度为403.此外降低了溶剂成本.但70℃下,溶解度仅为1.36%,溶解能力较弱.继续探讨了[AMIM]Cl作为[APy]Cl的共溶剂时对纤维素的溶解性能,结果表明,70℃下,[APy]Cl/[AMIM]Cl复合溶剂对棉浆粕的溶解度为8.78%,再生后聚合度为516.可知添加上述2种共溶剂均使[APy]Cl在低于自身熔点下形成液体并能够溶解一定量纤维素,拓宽了溶解温度区间及应用平台.对FTIR,XRD和TGA谱图分析,结果表明上述为纤维素的直接溶剂,可将其晶型由Ⅰ型转变成Ⅱ型,再生后热稳定性稍有降低.通过照片和SEM表明再生膜无色透明,结构致密.N-allylpyridinium chloride ionic liquid（Cl） was synthesized by one-step process and its property of dissolving cellulose was investigated.The results showed that the solubility of cotton linter pulp cellulose（degree of polymerization（DP）=556） was 19.71% at 120℃,and the thermostability of regenerated cellulose（DP=223） seriously decreased.The performance of regenerated cellulose could be enhanced by adding cosolvents into Cl.Compared with other cosolvent（DMSO,DMF or pyridine）,the Cl/DMAc composite solvent exhibited a better dissolution to cotton linter pulp cellulose.The solubility was 15.03% and the DP of regenerated cellulose was 403 at 100℃ with lower cost.But the solubility of Cl/DMAc was only 1.36% at 70℃.So,the Cl/1-N-ally1-3-methylimidazolium chloride ionic liquid（Cl） solvent was discussed afterwards.The results showed that the solubility of cotton linter pulp was 8.78% and the DP of regenerated cellulose was 516 in Cl/Cl composite solvent at 70℃.Besides,Cl/DMAc and Cl/Cl were liquid respectively below the melting point of Cl and they were the potential cellulose solvent.The FTIR,XRD and TGA spectrograms showed that these solvents were non-derivatizing solvents for cellulose,the cellulose was changed from cellulose Ⅰ to cellulose Ⅱ during dissolution and regeneration and the thermal stability of the regenerated cellulose slightly decreased.The photographs and SEM image indicated that the regenerated cellulose membrane was homogeneous and dense.

关 键 词：离子液体 纤维素 合成 共溶剂 溶解 

分 类 号：O636.11[理学—高分子化学]