Diethoxymethane was prepared in batch mode as well as in continuous Reactive Distillation Column (RDC) from ethanol and aqueous formaldehyde in the presence of a macroporous cation-exchange resin Indion-130. The batch reaction was studied for the effect of catalyst loading, mole ratio, concentration, temperature, etc. A pseudo homogeneous model was used to explain the batch kinetics and the kinetic parameters were evaluated. In the case of RDC, the effect of various parameters such as residence time, reflux ratio, mole ratio, feed concentration, feed configuration, etc. on the conversion and product purity was studied and evaluated.