Zeolite membranes have uniform and nano-sized pores, and they separate molecules based on differences in the molecules size and diffusion properties. Different routes used to prepare zeolite composite membranes include growing zeolite layers from gels on porous supports. Our approach to membrane synthesis was based on hydrothermally converting films of layered aluminosilicates into zeolite films. In this research, synthesis of nano NaA zeolite membrane from kaolin was investigated. In the first step, kaolin has been calcined at 700 °C to the metakaolinite phase. As a second step, the zeolitisation experiments have been carried out under hydrothermal conditions. The metakaolinite obtained has been reacted with NaOH solutions in autoclaves at 100°C. X-ray diffraction (XRD) patterns of the membranes exhibited peaks corresponding to the support and the zeolite. The morphology of the support and membrane subjected to crystallization was characterized by Scanning electron microscopy (SEM). Separation performance of the NaA membranes was evaluated using pervaporation of water–Ethanol mixtures. The membranes showed high water selectivity in the water–Ethanol mixtures.