Abstract: NaA zeolite membranes were prepared by secondary growth method on the outer surface of α-Al₂O₃ hollow fiber supports. Vacuum seeding method was used for planting zeolite seeds on the support surfaces. Hydrothermal crystallization was then carried out in a synthesis solution with molar ratio of Al₂O₃:SiO₂:Na₂O:H₂O = 1:2:2:120 at 100 ℃ for 4 h. Effects of seeding conditions on preparation of hollow fiber NaA zeolite membranes were extensively investigated. Moreover, hollow fiber membrane modules with packing membrane areas of ca. 0.1 and 0.2 m² were fabricated to separate ethanol/water mixture. It is found that the thickness of seed layer is obviously affected by seed suspension concentration, coating time and vacuum degree. Close-packing seed layer is required to obtain high-quality membranes. The optimized seeding conditions (seed suspension mass concentration of 0.5%-0.7%, coating time of 5 s and vacuum degree of 10 kPa) lead to dense NaA zeolite layer with a thickness of 6-8 μm. Typically, an as-synthesized hollow fiber NaA zeolite membrane exhibits good pervaporation performance with a permeation flux of 7.02 kg·m^-2·h^-1 and separation factor >10000 for separation of 90% (by mass) ethanol/water mixture at 75 ℃. High reproducibility has been achieved for batch-scale production of hollow fiber NaA zeolite membranes by the hydrothermal synthesis approach.

Key words: NaA zeolite membrane, Vacuum seeding method, Hollow fiber, Pervaporation

摘要： NaA zeolite membranes were prepared by secondary growth method on the outer surface of α-Al₂O₃ hollow fiber supports. Vacuum seeding method was used for planting zeolite seeds on the support surfaces. Hydrothermal crystallization was then carried out in a synthesis solution with molar ratio of Al₂O₃:SiO₂:Na₂O:H₂O = 1:2:2:120 at 100 ℃ for 4 h. Effects of seeding conditions on preparation of hollow fiber NaA zeolite membranes were extensively investigated. Moreover, hollow fiber membrane modules with packing membrane areas of ca. 0.1 and 0.2 m² were fabricated to separate ethanol/water mixture. It is found that the thickness of seed layer is obviously affected by seed suspension concentration, coating time and vacuum degree. Close-packing seed layer is required to obtain high-quality membranes. The optimized seeding conditions (seed suspension mass concentration of 0.5%-0.7%, coating time of 5 s and vacuum degree of 10 kPa) lead to dense NaA zeolite layer with a thickness of 6-8 μm. Typically, an as-synthesized hollow fiber NaA zeolite membrane exhibits good pervaporation performance with a permeation flux of 7.02 kg·m^-2·h^-1 and separation factor >10000 for separation of 90% (by mass) ethanol/water mixture at 75 ℃. High reproducibility has been achieved for batch-scale production of hollow fiber NaA zeolite membranes by the hydrothermal synthesis approach.

关键词: NaA zeolite membrane, Vacuum seeding method, Hollow fiber, Pervaporation