一步法制备乙酰化纳米纤维素及其性能表征  

Preparation and characterization of acetylated nanocellulose by one-step method

作　　者：林凤采 卢麒麟[1] 林咏梅[1] 庄森炀 李现艳[1] 黄彪[1] 

机构地区：[1]福建农林大学材料工程学院,福建福州350002

出　　处：《化工进展》2016年第2期559-564,共6页Chemical Industry and Engineering Progress

基　　金：国家林业局948项目(2014-4-30);国家自然科学基金项目(31370560;31170520)

摘　　要：采用机械力化学方法,在4-二甲氨基吡啶（DMAP）催化下一步法制备乙酰化纳米纤维素（A-NCC）。通过单因素研究方法,对影响A-NCC得率的DMAP用量、球磨时间、反应温度、超声时间、反应时间等因素进行探讨及分析。采用透射电子显微镜（TEM）、X射线衍射仪（XRD）、热分析仪（TGA）、傅里叶变换红外光谱仪（FTIR）和X射线光子能谱分析（XPS）等对所制备A-NCC的形貌、热稳定性和谱学性能进行分析表征,采用滴定法测量表面羟基的取代度。结果表明：机械力化学法制备的A-NCC呈细长状,直径约为10~30nm,长度约为200~750nm,结晶度为76%,取代度（DS）在0.125~0.214之间;TGA分析表明,A-NCC热分解温度为311℃,低于竹浆。采用机械力化学法制备乙酰化纳米纤维素具有工艺简便、绿色环保的优点。Acetylated nanocellulose（A-NCC） was prepared via a one-step reaction with 4-dimethylaminopyridine（DMAP） as catalyst under mechanochemical conditions. Various factors affecting the A-NCC output,such as the catalyst dosage,milling time,reaction temperature,ultrasonic time and reaction time were explored individually. The structural, morphological, thermo and spectroscopic characteristics of A-NCC were studied using transmission electron microscopy（TEM）,X-raydiffraction（XRD）,thermographic analyzer（TGA）,Fourier transformation infrared spectroscopy（FTIR） and X-ray photoelectron spectroscopy（XPS）. The results indicated that the diameters of A-NCC prepared by this method ranged from 10 nm to 30 nm and the length ranged from 200 nm to 750 nm. XRD results showed a 76% crystallinity index and DS was determined to be around 0.125—0.214. The A-NCC produced by the one-step method also exhibited lower decomposition temperature than pulp fiber, which was proved by the TGA results. This work provided a simple and environmentally benign approach to prepare modified NCC（acetylated nanocellulose）.

关 键 词：一步法 机械力化学 乙酰化 纳米纤维素 4-二甲氨基吡啶 

分 类 号：TQ352[化学工程]