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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 29, Number 3
BKCSDE 29(3)
March 20, 2008 

Synthesis of Periodic Mesoporous Organosilica by Microwave Heating
Sang-Soon Yoon, Won-Jin Son, Kalidas Biswas, Wha-Seung Ahn*
Periodic mesoporous silica, Microwave, HPLC, Ti-grafting, Epoxidation
A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2- bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 μm size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 μ m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.
609 - 614
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