高等学校化学学报 ›› 2003, Vol. 24 ›› Issue (12): 2321.

• 研究快报 • 上一篇    下一篇

结晶性间同立构1,2-聚丁二烯的单晶结构

陈晔1, 杨德才1, 胡雁鸣2, 张学全2   

  1. 1. 中国科学院长春应用化学研究所高分子物理与化学国家重点实验室;
    2. 高分子工程实验室, 长春 130022
  • 收稿日期:2003-06-23 出版日期:2003-12-24 发布日期:2003-12-24
  • 通讯作者: 杨德才(1940年出生),男,研究员,博士生导师,主要从事高分子凝聚态结构研究.E-mail:dcyang@ciac.jl.cn E-mail:dcyang@ciac.jl.cn
  • 基金资助:

    国家自然科学基金(批准号:20234020);国家重大基础研究发展规划项目(批准号:G1999064805)资助

Single Crystal Structure of Crystalline Syndiotactic1,2-Polybutadiene

CHEN Ye1, YANG De-Cai1, HU Yan-Ming2, ZHANG Xue-Quan2   

  1. 1. Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, State Key Laboratory of Polymer Physics and Chemistry;
    2. Polymer Engineering Laboratory, Changchun 130022, China
  • Received:2003-06-23 Online:2003-12-24 Published:2003-12-24

关键词: 间同立构1, 2-聚丁二烯, 单晶结构, TEM, 电子衍射技术

Abstract: The crystalline syndiotactic 1,2-polybutadiene was synthesized with a catalytic system consisting of iron acetylacetonate, triisobutylaluminum and diethyl phosphite (DEP), and its single crystal structure was studied by transmission electron microscopy (TEM) and electron diffraction (ED) techniques. The polymer with melting point 179 ℃ was found to have 89.3% 1,2 content and 86.5% sydiotacticity based on 13CNMR measurement. The single crystals of the polymer were achieved by melt crystallization of the solution cast thin films at 150 ℃ for 2h. Bright field electron micrograph shows that the single crystal exhibits a hexagonal prism shape with its long axis along the crystallographic b-axis, as revealed by the corresponding ED pattern. The strong (hk0) reflections of the ED pattern indicate that the single crystal possesses a very good crystallographic orientation with the c-axis perpendicular to the film plane. According to the orthorhombic packing of the planar zigzag chains, all of the diffraction points can be indexed, and the unit cell parameters calculated from the ED result are a=1.102 nm and b=0.664 nm. In order to obtain the unit cell parameter c, α highly oriented thin filMOf the polymer was prepared with a special melt drawn technique. The TEM bright field image indicates that the melt drawn thin films contain highly oriented lamellae with their growing direction perpendicular to the drawing direction. The corresponding ED pattern reveals the molecular chains are highly oriented, with the c-axis parallel to the drawing direction. The unit cell parameter c is 0.513 nm, as calculated from the (hk0) reflections.

Key words: Syndiotactic1,2-polybutadiene, Single crystal structure, TEM, Electron diffraction technique

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