Abstract: The technological scheme of azeotropic mix separation by means of the selective water absorption with use of KA zeolite molecular gate properties is developed. It is shown that initial mix will be divided into two phases in a three-phase separator where from azeotropic mix the phase of liquid hydrocarbons and water-methanol mix separates. The following stage of water-methanol mix gets on the block of adsorbers where methanol dehydration takes place. Technological parameters of operating the block of adsorbers are also determined, on the basis the test research the cycles of adsorbents regeneration are established. Comparison of test and experimental data of liquid adsorption process on solid adsorbents is carried out. The mathematical model reflecting process of adsorption in KA brand zeolite is developed.