Catalytic composite PVA membranes crosslinked with glutaraldehyde were prepared and used in form of disks in the acetalisation of phenylacetaldehyde and glycerol. Catalytic runs were carried out in batch reactors in order to study the effect of catalyst loading, crosslinking degree and hydrophilic/hydrophobic behavior. It was also preformed catalytic runs in pervaporation assisted catalytic membrane reactor to improve the efficiency of the process. The catalysts were characterized by thickness measurements, contact angles and swelling degree as well as by Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM) and scanning electron microscopy (SEM).