This study provides novel details about the industrial use of cyclic distillation in the production of food-grade alcohol, which confirmed the theoretical predictions of increasing separation efficiency. Increasing the profitability of the production of ethanol food grade is primarily associated with an increase in product quality and reduction of energy costs per unit of production. One of the ways to solve these problems is to improve the ethanol purification technology by using cyclic distillation, which allows reduction of energy costs and higher productivity by removing impurities at a higher concentration (leading also to waste reduction). The purification of ethanol from impurities (head and intermediate type) is carried out in hydro-selection columns. Critically, the volatility of most components depends on the actual ethanol concentration on the stage. This study investigated the distribution of ethanol on the trays depending on the water feed stage to the column and showed the optimal distribution of hydro-selective water in an industrial column to allow the highest possible separation efficiency of components during cyclic distillation. A cyclic distillation column with 15 Maleta trays was superior in separation capacity and performance as compared to a traditional column with 50 bubble cap trays.