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In order to obtain a steam-stable hydrogen permselectivity membrane, with tetraethylorthosilicate (TEOS) as the silicon source, zirconium nitrate pentahydrate (Zr(NO 3 ) 4 ·5H 2 O) as the zirconium source, and methyltriethoxysilane (MTES) as the hydrophobic modifier, the methyl-modified ZrO 2 -SiO 2 (ZrO 2 -MSiO 2 ) membranes were prepared via the sol-gel method. The microstructure and gas permeance of the ZrO 2 -MSiO 2 membranes were studied. The physical-chemical properties of the membranes were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscope (SEM), and N 2 adsorption-desorption analysis. The hydrogen permselectivity of ZrO 2 -MSiO 2 membranes was evaluated with Zr content, temperature, pressure difference, drying control chemical additive (glycerol) content, and hydrothermal stability as the inferred factors. XRD and pore structure analysis revealed that, as n Zr increased, the MSiO 2 peak gradually shifted to a higher 2θ value, and the intensity gradually decreased. The study found that the permeation mechanism of H 2 and other gases is mainly based on the activation-diffusion mechanism. The separation of H 2 is facilitated by an increase in temperature. The ZrO 2 -MSiO 2 membrane with n Zr = 0.15 has a better pore structure and a suitable ratio of micropores to mesopores, which improved the gas permselectivities. At 200 °C, the H 2 permeance of MSiO 2 and ZrO 2 -MSiO 2 membranes was 3.66 × 10 -6 and 6.46 × 10 -6 mol·m -2 ·s -1 ·Pa -1 , respectively. Compared with the MSiO 2 membrane, the H 2 /CO 2 and H 2 /N 2 permselectivities of the ZrO 2 -MSiO 2 membrane were improved by 79.18% and 26.75%, respectively. The added amount of glycerol as the drying control chemical additive increased from 20% to 30%, the permeance of H 2 decreased by 11.55%, and the permselectivities of H 2 /CO 2 and H 2 /N 2 rose by 2.14% and 0.28%, respectively. The final results demonstrate that the ZrO 2 -MSiO 2 membrane possesses excellent hydrothermal stability and regeneration capability.

Zirconia-Doped Methylated Silica Membranes via Sol-Gel Process: Microstructure and Hydrogen Permselectivity