Synthesis of n-butyl acrylate by esterification of acrylic acid with n-butyl alcohol was carried out in a batch membrane reactor. Optimization and design of the experiment was accomplished by response surface methodology with Box-Behnken experimental design. The effects of different parameters like reaction temperature, catalyst concentration, molar ratio of alcohol to acid, and ratio of membrane surface to initial volume on water flux and conversion of acrylic acid were evaluated. A kinetic model for the esterification-coupled pervaporation process was developed. Kinetic parameters were estimated by a nonlinear optimization technique in the MATLAB optimization toolbox. The experimental and simulation results were applied for developing a concept to effectively conduct a pilot-scale esterification-pervaporation experiment.