天然纤维素的核磁共振碳谱表征.doc

天然纤维素的核磁共振碳谱表征 何建新1,2 王善元1 (1.东华大学 纺织学院，上海201620；2.中原工学院 纺织学院，郑州 450007) 摘要：利用核磁共振碳谱和X衍射研究了几种常见的天然纤维素纤维苎麻、亚麻、棉纤维以及两种浆粕纤维竹浆和硬木浆的结晶结构，探究了两种方法之间的差异。这些纤维素纤维的核磁共振碳谱被详细的解析，一些结构特征参数如结晶度、侧向微纤尺寸以及晶型的组成被确定。研究表明韧皮纤维如苎麻和亚麻要比棉纤维、竹浆和木浆有更高的Iα/Iβ比，不过苎麻主要是由于Iα的含量高和次晶的含量低，而亚麻是由于Iβ的含量低和次晶的含量高。利用核磁共振计算的几种纤维素的结晶度和晶粒尺寸要比利用X衍射计算的要小，只有在高结晶的纤维素如苎麻和亚麻偏差才比较小，主要原因在于NMR对小范围有序更为敏感，只有晶区内的材料才能看作结晶区。通过结合两种方法能更全面地反映天然纤维素纤维之间的结构。 关键词：纤维素；核磁共振碳谱；结晶结构；X-衍射 中图分类号：TS 182 文献标识码：A 作者简介：何建新（1977―），男，汉族，讲师，博士。研究方向：新型纺织材料与绿色纺织品。Email: hejianxin771117@163.com Characterization of native cellulose using solid-state 13C-CP/MAS NMR spectroscopy He Jianxin1,2 Wang shanyuan1 (1. College of textile, Donghua University, Shanghai 201620, China 2. College of textile, Zhongyuan University of Technology，Zhengzhou 450007, China) Abstract: Several common native cellulose, ramie, flax, cotton fibers, as well as bamboo pulp and hardwood pulp were investigated using 13C-CP/MAS NMR spectroscopy and X-ray diffraction, and the differences between two methods were discussed. NMR spectra of these fibers were analyzed in detail and some structure parameters such as crystallinity, lateral microfiber size, and allomorphs content were determined. The study shows that bast fibers ramie and flax have a higher Iα/Iβ ratio than that of cotton, bamboo pulp and wood pulp, however, for ramie the cause is a higher Iα content, and for flax a lower Iβ content. Crystallinity and crystalline size calculated by NMR method are less than these obtained by X-ray diffraction. The reason is that in contrast with X-ray analysis, 13C NMR is more sensitive to short range order and only material within the crystalline domain appears as crystalline in 13C NMR spectra. The structure of native cellulose can be understood by combination of the two methods. Keywords: cellulose; 13C NMR; crystalline structure; X-ray diffraction 1. 引言 纤维素是由D-葡萄吡喃糖基以1,4-β-苷键连接而成的线性均聚物，是高等植物细胞壁的最常见的成分。尽管同为纤维素纤维，来自于不同植物来源的天然纤维的物理性能有很大的差异，这种差异主要源于其不同的结晶结构。天然纤维素主要由两种不同的晶型Iα和