以正硅酸乙酯(TEOS)和异丁基三乙氧基硅烷(iTES)为前体,通过溶胶-凝胶法在酸性条件下制备异丁基修饰的二氧化硅溶胶,并采用浸渍提拉法在γ-Al2O3/α-Al2O3支撑体上制备异丁基修饰的微孔二氧化硅膜材料.分别通过动态光散射技术、接触角测量、红外光谱、核磁共振以及N2吸附等测试手段对溶胶的粒径分布、膜材料的疏水性能以及孔结构进行表征,并深入研究异丁基修饰膜材料的氢气渗透和分离性能.结果表明,当摩尔比n(iTES)/n (TEOS)=0.6时,溶胶的平均粒径约为5.1 nm,膜材料的孔径狭窄分布在0.45～0.8nm,其对水的接触角达到(114.0±0.5)°.H2在膜材料中的渗透率随测试温度的升高而增大,300℃时达到9.07×10-7mol/(m2·s·Pa),H2/CO2和H2/CO的理想分离系数分别为6.79和15.37,双组份混合气体分离系数分别为7.09和15.72,均高于对应的Knudsen扩散分离因子,H2在膜材料中的输运主要遵循活化扩散机理.在250℃水蒸气物质的量摩尔分数为5％的环境中陈化200 h后,异丁基修饰的SiO2膜具有良好的水热稳定性.
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