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

doi:10.7503/cjcu20140357

Abstract

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

CLC Number:

O631.5

TrendMD:

GAO Xu, LU Ping, MA Yuguang. Ultrasound-assisted Synthesis and Characterization of Silicon Centered Porous Aromatic Frameworks^†[J]. Chem. J. Chinese Universities, 2014, 35(8): 1795.

Figures/Tables 4

Fig.1 Ultrasound-assisted synthesis of Si-PAF

Fig.2 FTIR spectra of monomer(a), Si-PAF(amplitude 50%) for 60 min(b) and 90 min(c)

Fig.3 SEM(A), HRTEM images(B) and PXRD pattern of PAF-Si(C)(amplitude 50%, time 90 min)

Fig.4 Nitrogen gas adsorption(a)-desorption(b) isotherms(A) and pore distribution(B) of Si-PAF(amplitude 50%, time 90 min)

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