2,2,2-Trifluoroethyl rnethacrylate (TFEMA) is used in the preparation of functional water-repellent paints and optical fiber coating agents. and is manufactured by esterification of 2.2.2-trifluoroethanol (TFEA) and rnethacrylic acid (MA) via a dehydration process using azeotropic distillation. To substitute for the hazardous dehydration process, composite-type PVA pervaporation membranes were prepared using glutaraldehyde on a porous polyethersulfone Support and their basic pervaporation properties were determined for TFEA/water and MA/water mixtures. The effect of the degree of crosslinking agent, feed concentration, and operating temperature on the pervaporation properties was determined. The PVA composite membranes showed excellent dehydration performances that are suitable for application to the esterification of TFEMA. (C) 2004 Elsevier B.V. All rights reserved.