葡萄糖與纖維素之(甲基)丙醯胺酯之合成與鑑定

Abstract

本研究係以接枝方法來破壞纖維素之結晶性而改質成為可溶性且可交聯之高分子材料。將纖維素及葡萄糖分別溶於LiCl/DMAc並與methacryloyl isocyanate (MAI)反應，分別得到cellulose N-methacryloylcarbamate(CELL-MAC)及glucose N-methacryloylcarbamate(GLU-MAC)。實驗中使用溴來滴定C＝C以鑑定每單位葡萄糖之平均取代率(DS)。取代率亦由元素分析之數值來計算。CELL-MAC由WAXD鑑定發現其失去原有纖維素的結晶度。CELL-MAC可溶於DMF、DMAc、DMSO等溶劑。其C＝C可用BPO交聯。纖維素、CELL-MAC、GLU-MAC、交聯後之CELL-MAC及GLU-MAC分別經曲FT-IR及固態13CNMR來鑑定其結構。而熱性質由DSC及TGA來分析，發現120℃為其分解溫度，推斷應為Carbamate group的裂解。

This research deals with the grafting of crystalline cellulose to a soluble and crosslinkable cellulose derivative. The reaction of cellulose or glucose with methacryloyl isocyanate in LiCl/DMAc resulted in cellulose N-methacryloylcarbamate(CELL-MAC) or glucose N-methacryloylcarbamate(GLU-MAC). The degree of substitution (DS) per anhydroglucose unit was determined from the titration of C=C moiety with bromine. The DS was also calculated from the data of elemental analyses. The CELL-MAC lost its crystallinity as it was found from WAXD, and became soluble in such solvents as DMF, DMAC, DMSO, ..., etc. The C=C moiety in the CELL-MAC and GLU-MAC were able to be crosslinked by BPO. Structures of the cellulose, CELL-MAC, GLU-MAC, crosslinked CELL-MAC and crosslinked GLU-MAC were further characterized with FTIR and solid state 13C NMR. Thermal properties were characterized with DSC and TGA, which showed a decomposition temperature of 120 ℃, presumably due to the breakdown of the carbamate group.