纳米纤维素柠檬酸酯的“一锅法”绿色制备  

One-pot green preparation of citric acid esterified cellulose nanocrystals

作　　者：吴嘉茵 黄彪[1] 卢麒麟[1,2] WU Jiayin;HUANG Biao;LU Qilin(College of Material Engineering,Fujian Agriculture and Forestry University,Fuzhou 350002,China;Fujian Key Laboratory ofNovel Functional Textile Fibers and Materials,Minjiang University,Fuzhou 350108,China)

机构地区：[1]福建农林大学材料工程学院,福州350002 [2]闽江学院福建省新型功能性纺织纤维及材料重点实验室,福州350108

出　　处：《丝绸》2021年第10期44-51,共8页Journal of Silk

基　　金：福建省科技创新重点项目(高校类)(2021G02011);福建省自然科学基金面上项目(2021J011034);闽江学院引进人才项目(MJY18010);闽江学院科研项目(MYK20005)。

摘　　要：文章针对纳米纤维素制备改性过程中操作复杂、得率低、使用有毒试剂对环境不友好等问题,以竹纤维为原料,在机械力化学作用下,以磷钨酸-柠檬酸催化水解“一锅法”制备了纳米纤维素柠檬酸酯(E-CNCs),该方法工艺简单、绿色环保,且E-CNCs得率高。机械力化学作用能显著提高纤维素的反应活性,加快纤维素水解速度,提高了E-CNCs的结晶度和酯化反应接枝率。在球磨1.5 h、磷钨酸(PTA)质量分数6%、反应6 h、超声1.5 h的优化条件下,E-CNCs得率为75.6%,取代度为0.25,结晶度为80%,长度为180~210 nm,直径为8~10 nm,且热稳定性良好。To address issues during the preparation and modification process of cellulose nanocrystals,such as complex operations,low yields,and environmentally unfriendly use of toxic reagents,bamboo fibers were selected as the raw materials in this study to prepare citric acid esterified cellulose nanocrystals(E-CNCs)under the catalytic hydrolysis of phosphotungstic acid(PTA)-citric acids by mechanochemical process in one-pot reaction.The method is simple in process,green and environmentally friendly,with a high yield of E-CNCs.The reactivity of cellulose was improved significantly and the hydrolysis rate was accelerated under the effect of mechanochemistry.Meanwhile,the crystallinity and graft ratio of esterification reaction were also improved,with a yield of 75.6%,degree of substitution of 0.25 and crystallinity of 80%under the optimized conditions of ball-milling of 1.5 h,PTA concentration of 6%,reaction time of 6 h and ultrasonic time of 1.5 h.Moreover,E-CNCs exhibited excellent thermal stability,with the length of 180 to 210 nm and the diameter of 8 to 10 nm.

关 键 词：纳米纤维素 机械力化学 柠檬酸 磷钨酸 酯化反应 绿色环保 热稳定性 

分 类 号：TS102.511.3[轻工技术与工程—纺织工程] TQ352.1[轻工技术与工程—纺织科学与工程]