A composite catalytic membrane with a crosslinked PVA dense active layer coated on a porous ceramic plate support was prepared using a novel method and evaluated with a pervaporation setup fbr tile separation of several organic aqueous mixtures. Several key problems occurred during the preparation procedure are discussed. SEM (scanning electron microscopy), IR (infra-red) (ATR) (attenuated total refraction) and XPS (X-ray photoelectron spectrometry) were used to characterize the catalytic membrane natures. N-Butyl alcohol-acetic acid esterification was used as a model system for investigating into the coupling of reaction with pervaporation in a batch reactor. Different reaction parameters, temperatures, catalyst concentrations and initial reactant molar ratios were studied experimentally.