高等学校化学学报 ›› 2014, Vol. 35 ›› Issue (8): 1795.doi: 10.7503/cjcu20140357

• 高分子化学 • 上一篇    下一篇

超声辅助的硅中心多孔芳香材料的合成与表征

高旭, 路萍(), 马於光   

  1. 吉林大学超分子结构与材料国家重点实验室, 长春 130012
  • 收稿日期:2014-04-16 出版日期:2014-08-10 发布日期:2019-08-01
  • 作者简介:联系人简介: 路 萍, 女, 博士, 副教授, 主要从事高分子化学与物理领域的研究. E-mail: lup@jlu.edu.cn
  • 基金资助:
    国家自然科学基金(批准号: 21174050)资助

Ultrasound-assisted Synthesis and Characterization of Silicon Centered Porous Aromatic Frameworks

GAO Xu, LU Ping*(), MA Yuguang   

  1. State Key Laboratory of Supramolecular Structure and Materials, Jilin University, Changchun 130012, China
  • Received:2014-04-16 Online:2014-08-10 Published:2019-08-01
  • Contact: LU Ping E-mail:lup@jlu.edu.cn
  • Supported by:
    Supported by the National Natural Science Foundation of China(No21174050)

摘要:

以四(4-溴苯基)硅烷为基元, 利用超声辅助的Yamamoto 偶联反应, 合成了硅中心的多孔芳香材料(Si-PAF). 通过调节超声参数, 优化了反应条件. 采用红外光谱、 元素分析、 扫描电子显微镜和透射电子显微镜等手段表征了Si-PAF的结构及形貌, 利用氮气吸附实验考察了其孔道结构.

关键词: 超声, Yamamoto 偶联反应, 硅中心, 多孔芳香材料, N2气吸附

Abstract:

Silicon centered porous aromatic frameworks(Si-PAF) was synthesized by ultrasound-assisted Yamamoto coupling reaction. The ultrasound amplitude and reaction time were adjusted to optimize the reaction parameters. The obtained Si-PAF exhibits high chemical stability. It is insoluble in common organic solvents such as CHCl3, tetrahydrofuran(THF), ethanol, acetone and dimethylformamide(DMF). The polymer was characterized by Fourier transform infrared spectroscopy(FTIR), scanning electron microscopy(SEM), high-resolution transmission electron microscopy(TEM), powder X-ray diffraction(PXRD), and N2 gas absorption. From the disappearance of the C—Br bands(at 529 cm-1) in the FTIR spectra, the formation of the product can be confirmed. SEM image shows that Si-PAF affords a spherical morphology. Simultaneously, TEM reveals that it possesses a worm-like texture. PXRD result indicates the amorphous texture which might be due to distortion and interpenetration of the phenyl rings. The N2 sorption isotherms were measured at 77 K to characterize the porosity of the Si-PAF networks. All networks give rise to typeⅠ nitrogen gas adsorption isotherms with a distinct hysteresis for the whole range of relative pressure. Si-PAF exhibits high surface areas(up to 601 m2/g) and good adsorption ability of N2.

Key words: Ultrasound, Yamamoto coupling reaction, Silicon centered, Porous aromatic framework, N2 adsorption

中图分类号: 

TrendMD: