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Coupling of a pervaporation membrane unit with an esterification reactor has been undertaken with a view to improve the overall efficiency of the esterification process through removal of one of the products. The esterification reaction of acetic acid with methanol in the presence of two alternative heterogeneous catalysts (Nafion resin and silica sulfuric acid) is investigated on the laboratory scale. The effect of different parameters on the esterification/pervaporation system is explored. The studied parameters include reactants molar ratio, temperature, and catalyst weight percent.