Several novel strategies of synthesis were designed to prepare modified silica membrane materials in order to improve the surface properties of the silica matrix towards molecular sieve applications in moisture environments. Over the last decades, the sol– gel technique was postulated as an interesting strategy to prepare new hybrid organic–inorganic silica-based microporous materials with enhanced properties. For example, surface modification using different organic template agents increase the hydrophobicity of the silica membranes. Using this technique, researchers have prepared molecular sieving architectures by calcining templated sol– gels in inert atmospheres [14-16]. However, such methods may alter the micropore structure of the materials and hinder their molecular separation properties [16,17]. Templates can be classified as organic covalent ligands, such as methyl groups, or non- covalently bonded, such as surfactants. One remarking case to introduce hydrophobic moieties in the silica membrane material was reported by De Vos et al. [16]. Methyltriethoxysilane (MTES) was embedded into a sol–gel process prepared with tetraethylorthosilicate (TEOS), water, ethanol and nitric acid. This process introduces methyl groups to the silica matrix as template agents to enhance hydrophobicity. These silica membrane material showed high hydrophobicity compared with silica membrane material prepared without MTES. On the other hand, various research groups have used noncovalently bonded organic templates, such as C6 and C16 surfactants [5,17] and alkyltriethoxysilanes [18], to tailor the pore size of intermediate or top layers of membranes. At high temperature under oxidizing conditions these organic templates trapped in the gel structure are burnt off, thus producing a cavity with similar dimensions to that of the template molecule [19,20].