Citation: HONG Zhi-Fa, WEI Qi, LI Guo-Hua, WANG Xue-Wei, NIE Zuo-Ren, LI Qun-Yan. Preparation, H2 Separation and Hydrothermal Stability of Trifluoropropyl-Modified Silica Membranes[J]. Chinese Journal of Inorganic Chemistry, ;2013, 29(5): 941-947. doi: 10.3969/j.issn.1001-4861.2013.00.161
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Trifluoropropyl-modified silica membranes were prepared by sol-gel technique using tetraethyl orthosilicate (TEOS) and (trifluoropropyl)trimethoxysilane (TFPTMS) as precursors. The effect of trifluoropropyl modification on the hydrophobic pore structure, properties, hydrogen permeation and separation properties and long-term hydrothermal stability of the modified silica membranes were investigated in detail. The results show that the modified membranes retain a desirable microporous structure with a pore size distributed from 0.45 to 0.7 nm. The hydrophobic property of silica membranes has been considerably enhanced after modification, with a water contact angle of (102.7°±0.1°) at a TFPTMS/TEOS molar ratio of 0.6. The hydrogen transport in the modified silica membranes complies with a micropore diffusion mechanism, with a single H2 permeance of 4.77×10-7 mol·m-2·s-1·Pa-1, a H2/CO2 permselectivity of 6.99 and a H2/CO2 binary gas mixture separation factor of 6.93 at 300 ℃, higher than Knudsen permselectivity (4.69). Under a humid condition with a temperature of 200 ℃ and a water vapor molar ratio of 5%, the single H2 permeance slightly decrease in the first 3 hours and then almost remain constant for at least 220 hours, indicating that the modified membranes are more hydrothermally stable than pure SiO2 membranes.
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