Pervaporation of water/2,2,2-trifluoroethanol (TFEA) mixtures was performed using a NaY zeolite membrane which was prepared by a hydrothermal synthesis. Pervaporation with a zeolite membrane is one of the economic separation technologies for liquid mixtures including organic/water solutions. The effects of a TFEA feed concentration and a temperature were studied on the permeation flux and the separation factor. Not only the water flux increased significantly with the increase of the operating temperature, but also the TFEA flux through the NaY zeolite membrane rapidly increased with the increase of the temperature at the feed concentration below 0.8 mole fraction of TFEA.