Zeolite membranes were synthesized using metakaolin, sodium hydroxide, and alumina with 6Al2Si2O7 : 12NaOH : 2Al2O3 molar ratio as raw ingredients. For this purpose, a combined approach was employed which involved ultrasonic processing of the initial suspension and microwave crystallization. The synthesis was followed by a comparative assessment of the separation capacity of the samples prepared by physicochemical treatment versus the samples obtained by conventional methods, such as crystallization under convective heating. The highest content of LTA crystalline phase was achieved by a combination of ultrasonic processing and microwave crystallization. Moreover, this approach produced defect-free membranes which did not contain non-zeolite pores and ensured a high degree of ethanol/water pervaporation at 60 degrees C.