Chemical Industry and Engineering Progree ›› 2016, Vol. 35 ›› Issue (02): 559-564.DOI: 10.16085/j.issn.1000-6613.2016.02.034

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Preparation and characterization of acetylated nanocellulose by one-step method

LIN Fengcai, LU Qilin, LIN Yongmei, ZHUANG Senyang, LI Xianyan, HUANG Biao   

  1. College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, Fujian, China
  • Received:2015-07-08 Revised:2015-07-23 Online:2016-02-05 Published:2016-02-05

一步法制备乙酰化纳米纤维素及其性能表征

林凤采, 卢麒麟, 林咏梅, 庄森炀, 李现艳, 黄彪   

  1. 福建农林大学材料工程学院, 福建 福州 350002
  • 通讯作者: 黄彪,教授,博士生导师,主要从事植物纤维化学和炭材料的研究。E-mail:fjhuangbiao@hotmail.com。
  • 作者简介:林凤采(1990-),男,硕士研究生。E-mail:linfengcai8@163.com。
  • 基金资助:

    国家林业局948项目(2014-4-30)及国家自然科学基金项目(31370560,31170520)。

Abstract: 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 10nm to 30nm and the length ranged from 200nm to 750nm. 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).

Key words: one-step method, mechanochemical, acetylated, nanocellulose, DMAP

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。

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

CLC Number: 

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