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http://dx.doi.org/10.5012/bkcs.2008.29.3.609

Synthesis of Periodic Mesoporous Organosilica by Microwave Heating  

Yoon, Sang-Soon (Department of Chemical Engineering, Inha University)
Son, Won-Jin (Department of Chemical Engineering, Inha University)
Biswas, Kalidas (Department of Chemical Engineering, Inha University)
Ahn, Wha-Seung (Department of Chemical Engineering, Inha University)
Publication Information
Bulletin of the Korean Chemical Society / v.29, no.3, 2008 , pp. 609-614 More about this Journal
Abstract
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 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m 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.
Keywords
Periodic mesoporous silica; Microwave; HPLC; Ti-grafting; Epoxidation
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