Ethanol dehydration of azeotropic mixture was performed by using diffusion distillation apparatus consisting of a wetted-wall column with two concentric tubes. Ethanol-water mixtures evaporated below the boiling point was separated during the diffusion through the gap filled with an inert gas. As the temperature difference between evaporation part and condensation part was increased, the total flux increased but the selectivity decreased. The effect of the annular width on the selectivity was not significant but the total flux was decreased with decreases in the annular width. Inert gas has an effect on the diffusivity of evaporated gas components. The total flux in case of helium as inert gas was larger than that in case of air but the selectivity in case of using helium was lower.