针对中空纤维分子筛膜批量化制备过程中晶种涂覆问题,提出真空抽吸晶种涂覆技术,以简化晶种涂覆工艺过程。利用真空抽吸法在α—Al2O3中空纤维支撑体外表面涂覆NaA分子筛晶种层,继而采用二次生长法制备NaA分子筛膜。利用粒径分析仪、X线衍射仪(XRD)以及场发射扫描电子显微镜(FESEM)对NaA分子筛晶种及所制备的分子筛膜进行了系统表征。实验考察晶种涂覆条件对膜性能的影响,并优化真空抽吸条件。研究结果显示:采用质量浓度为5g/L的小粒径晶种悬浮液,在10kPa真空度下抽吸5s可获得均匀的晶种层,并制得高性能的中空纤维NaA分子筛膜。在348K下,所制备中空纤维NaA分子筛膜用于质量分数为90%的乙醇/水溶液分离时,其渗透水通量为5.89kg/(m2·h),分离因子为11800。
Vacuum seeding method was proposed to solve the seeding problems existing in mass produc- tion of hollow fiber zeolite membranes. The α-Al2O3 hollow fiber substrates were pre-coated with NaA zeo- lite seeds by a vacuum seeding method, then NaA zeolite membranes were synthesized by a secondary growth method on these substrates. NaA zeolite seeds and as-synthesized membranes were characterized by particle size analyzer, X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM). The effects of seeding conditions on membrane quality were investigated to achieve optimal vacuum conditions. Resuhs showed that the uniform seeding layer could be obtained under the conditions of 5 g/L seed suspension, vacuum degree of 10 kPa and coating time of 5 s. The as-synthesized hollow fi- ber NaA zeolite membranes exhibited excellent pervaporation performance. The permeation flux was 5.89 kg/( m2- h) and separation factor was 11 800 for the separation of ethanol solution with the mass fraction of 90% at 348 K.