The kinetics of transesterification of methyl acetate with ethylene glycol catalyzed by acidic ion-exchange resin NKC-9 is investigated in detail. The effects of reaction temperature, catalyst loading, and initial reactants molar ratio on the reaction rate are studied in the absence of mass transfer resistance. The kinetic equation is obtained by utilizing the PH model to correlate the experimental data. Then a distillation process is designed to produce high-purity ethylene glycol diacetate, which includes a reactive distillation column, an extractive distillation column, and a solvent recovery column. The extractive distillation column and solvent recovery column are used to recycle excess methyl acetate and entrainer. Operational and structural parameters are optimized by minimizing the total annual costs (TAC) while meeting the product specifications.