Abstract: Cation-exchange resins were used as catalysts in the hydrolysis of a mixture of methyl acetate and methanol by catalytic distillation. Catalyst-bundles of ion exchange resin were packed in a column as a reaction zone. The influences of operation parameters on the conversion of methyl acetate, such as height of the reaction and stripping zones, feed location, the amount of methanol in the feed, mole ratio of feed water to MeOAc, volume ratio of reflux to feed MeOAc, the ratio of the feed volume flow rate of MeOAc to the volume of catalyst bed, were investigated,. and the optimal operation parameters were determined. The conventional hydrolysis separation technology was analyzed and a new process was proposed. The decrease in heat requirement was estimated to be about 39.99% of the conventional process under the optimal operating condition.