氯化1-烯丙基-3-乙基-咪唑盐的合成及其对微晶纤维素的微波溶解  

Synthesis of [AEIM]Cl and Its Dissolution of Microcrystalline Cellulose by Microwave

作　　者：郭立颖[1] 史铁钧[1] 段衍鹏[1] 

机构地区：[1]合肥工业大学化工学院,合肥230009

出　　处：《应用化学》2009年第9期1005-1010,共6页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金(50773017)资助项目

摘　　要：合成了新型离子液体氯化1-烯丙基-3-乙基-咪唑盐([AEIM]Cl),并采用红外光谱和核磁共振测试技术对其化学结构进行了表征。研究了微波加热条件下[AEIM]Cl对微晶纤维素(MCC)的溶解性能,考察了NaOH、微波和高压等3种预处理方式对微晶纤维素的结晶度、聚合度及溶解率的影响。采用FT-IR、XRD、TGA和SEM测试技术分别对溶解后得到的再生纤维素的化学结构、晶型变化、热稳定性及表观形貌进行了分析。结果表明,[AEIM]Cl是微晶纤维素的直接溶剂。与原生纤维素相比,当选用15%的NaOH在高压釜中140℃条件下处理微晶纤维素时,处理过的纤维素结晶度由92.0%降至49.2%,聚合度由306降至153,溶解率从5.2%提高至28.8%。溶解过程中纤维素没有发生衍生化反应,溶解后得到的再生纤维素晶型由原来的纤维素Ⅰ转变为纤维素Ⅱ,且微晶尺寸从4.92nm降至1.76nm,热分解温度从246.6℃降至183.0℃。A novel ionic liquid, 1-allyl-3-ethyl imidazolium chloride （ [ AEIM ] Cl）, was synthesized and its chemical structure was confirmed by FT-IR and ^1H NMR. The solution of microcrystalline cellulose（MCC） in [ AEIM ] Cl was prepared by microwave heating. Influences of three treatment methods, such as NaOH, micro- wave and high pressure, on the crystallinity, degree of polymerization（DP） and dissolution rate of MCC were studied. Chemical structure, change of crystal form, thermostability and appearance of the regenerated cellulose after dissolution were analyzed by FT-IR, XRD, TGA, and SEM, respectively. It showed that the ionic liquid was a direct solvent for MCC. Compared to original MCC, crystallinity of MCC treated decreased from 92. 0% to 49.2%, DP decreased from 306 to 153, and dissolution rate increased from 5.2% to 28. 8% when the MCC was treated with 15% （ mass fraction） NaOH in a high pressure pot at 140 ℃. Chemical reaction did not occur during the dissolution of MCC. Crystal form of the regenerated cellulose changed from original cellulose Ⅰto cellulose Ⅱ , crystallite dimension of the regenerated cellulose was decreased from 4. 92 nm to 1.76 nm, and thermal decomposition temperature decreased from 246. 6 ℃to 183.0℃.

关 键 词：离子液体 微晶纤维素 溶解率 结晶度 再生纤维素 聚合度 

分 类 号：O636[理学—高分子化学]