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。
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 reac-tion parameters. The obtained Si-PAF exhibits high chemical stability. It is insoluble in common organic sol-vents 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 ab-sorption. 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 .