超声辅助的硅中心多孔芳香材料的合成与表征

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.

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

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.