The paper aims to show a search method for optimal conditions of 3A, 13X, ZSM-5 zeolite thermal regeneration after adsorption from a liquid water-isopropanol mixture. Comparative TGA-DTG results for heating of wet zeolites with different structure and hydrophobicity showed characteristic effects corresponding to the optimal temperature of zeolite regeneration. The consequences of overheating and collapse of the 3A, 13X, ZSM-5 zeolite structure at temperatures of 850, 900, 1000 °C, respectively, were recorded with XRD method. Moreover, XRD and NIR/DRS tests of loaded and regenerated zeolite samples showed interaction of adsorbate and co-adsorbed water with adsorbent and revealed influence of adsorption and regeneration processes on the adsorbent structure. Investigations of the regeneration of the zeolite 3A bed after adsorption of water from the isopropanol solution in the temperature swing adsorption (TSA) process were carried out by heating the bed with inert gas at 250 °C and different purge gas streams in the range of 1.68–2.40 kg/h. Four stages of wet bed regeneration were distinguished, which corresponded to the effect observed during TGA-DTG tests. For each stage, the specific demand for purge gas and energy was determined depending on the gas stream and its minimum value of 2.16 kg/h was indicated.