欢迎访问《生物质化学工程》,

生物质化学工程 ›› 2019, Vol. 53 ›› Issue (2): 47-53.doi: 10.3969/j.issn.1673-5854.2019.02.008

• 研究报告 • 上一篇    下一篇

纤维素纳米晶体制备工艺优化的研究

段敏,林涛*(),殷学风,李静   

  1. 陕西科技大学 轻工科学与工程学院; 轻化工程国家级试验教学示范中心; 陕西省造纸技术及特种纸品开发重点实验室,陕西 西安 710021
  • 收稿日期:2018-07-18 出版日期:2019-03-30 发布日期:2019-04-09
  • 通讯作者: 林涛 E-mail:lintao@sust.edu.cn
  • 作者简介:段敏(1993—),男,陕西宝鸡人,硕士生,主要从事纳米纤维素材料的开发应用
  • 基金资助:
    陕西省自然科学基础研究计划(2018JM2034);咸阳市科技计划项目(2017k02-20);国家自然科学基金资助项目(20876092)

Optimization of Preparation Process of Cellulose Nanocrystals

Min DUAN,Tao LIN*(),Xuefeng YIN,Jing LI   

  1. College of Bioresources Chemical and Materials Engineering; National Demonstration Center for Experimental Light Chemistry Engineering Education; Shaanxi Province Key Laboratory of Papermaking Technology and Specialty Paper, Shaanxi University of Science & Technology, Xi′an 710021, China
  • Received:2018-07-18 Online:2019-03-30 Published:2019-04-09
  • Contact: Tao LIN E-mail:lintao@sust.edu.cn
  • Supported by:
    陕西省自然科学基础研究计划(2018JM2034);咸阳市科技计划项目(2017k02-20);国家自然科学基金资助项目(20876092)

摘要:

以微晶纤维素(MCC)为原料经硫酸水解制备纤维素纳米晶体(CNC)。采用单因素法结合正交试验系统地研究了硫酸质量分数、反应温度和反应时间对纤维素纳米晶体得率以及平均粒径的影响,并通过扫描电镜(SEM)、原子力显微镜(AFM)、X射线衍射仪(XRD)、纳米激光粒度仪对CNC的性能进行了表征,揭示了酸水解制备CNC的机理。结果表明:CNC制备的最佳工艺参数为硫酸质量分数64%、反应温度45 ℃、反应时间90 min,在此条件下CNC的得率为24.6%,粒径为204.8 nm。CNC水悬浮液呈一种稳定的淡蓝色胶体状态,其微观形貌比较规整,呈短棒状,直径约10~20 nm,长度在150~300 nm之间;XRD结果显示CNC的晶型为纤维素Ⅰ型,结晶度为80.2%。

关键词: 纤维素纳米晶体, 酸水解, 得率, 粒径

Abstract:

Cellulose nanocrystals(CNC) were prepared from microcrystalline cellulose(MCC) by sulfuric acid hydrolysis. The effects of sulfuric acid mass fraction, reaction temperature and reaction time on the yield and average particle size of cellulose nanocrystals were studied by single factor method combined with orthogonal test. The performance of CNC was characterized by scanning electron microscopy(SEM), atomic force microscopy(AFM), X-ray diffractometer(XRD) and nano-laser particle size analyzer, and the mechanism of acid hydrolysis to prepare CNC was revealed. The results showed that the optimum process parameters of CNC preparation were sulfuric mass fraction 64%, reaction temperature 45 ℃ and reaction time 90 min. Under these conditions, the yield of CNC was 24.6% and the particle size was 204.8 nm. The CNC aqueous suspension was a kind of stable light blue colloidal state, and its microscopic morphology was relatively regular, which was short rod-shaped, with diameter of about 10-20 nm and length between 150-300 nm; XRD results showed that the crystal form of CNC was cellulose type Ⅰ, and the crystallinity was 80.2%.

Key words: cellulose nanocrystals, acid hydrolysis, yield, particle size

中图分类号: