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Synthesis of silicalite-1 membrane with two silicon source by secondary growth method and its pervaporation performance

机译:二次生长法合成二硅源的silicalite-1膜及其全蒸发性能

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Silicalite-1 membranes supported on macroporous alumina (α-Al2O3) tubes for pervaporation were successfully prepared by introducing ethyl triethoxysilane (ETES) during the preparation of synthesis solutions. The effects of synthesis parameters (i.e., [ETES] content, crystallization time, and crystallization temperature) on the membranes thickness and pervaporation performance were investigated for silicalite-1 membranes grown onto seeded supports. The as-synthesized membranes were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and pervaporation testing. The results indicated that the as-synthesized membranes were typical MFI-type zeolite membranes and the ETES promoted the crystal growth of the silicalite-1 membranes. The optimum molar composition (lTEOS:0.17TPAOH:120H2O:[0.02-0.04]ETES:4EtOH), more than 16h crystallization time at low-temperature (413 K) was better for obtaining a dense and continuous silicalite-1 membranes with a good pervaporation performance. The M3 membrane shows a relatively low selectivity for ethanol/water system but a high selectivity for acetone/water and butanol/water systems. The total fluxes of the M3 membrane were 1.55, 0.10, and 1.51 kg m~(-2)h~(-1) towards acetone/H2O, butanol/H2O and ethanol/H2O mixtures, respectively for 3 wt.% acetone/water, 2 wt.% butanol/water and 5 wt.% ethanol/water mixture, respectively and the corresponding separation factor was 211,150, and 39, respectively.
机译:通过在合成溶液的制备过程中引入乙基三乙氧基硅烷(ETES),成功地制备了支撑在大孔氧化铝(α-Al2O3)管上进行全蒸发的Silicalite-1膜。对于生长在种子载体上的silicalite-1膜,研究了合成参数(即[ETES]含量,结晶时间和结晶温度)对膜厚度和全蒸发性能的影响。合成后的膜通过X射线衍射(XRD),扫描电子显微镜(SEM)和渗透蒸发测试进行了表征。结果表明,合成后的膜是典型的MFI型沸石膜,而ETES促进了silicalite-1膜的晶体生长。最佳摩尔组成(lTEOS:0.17TPAOH:120H2O:[0.02-0.04] ETES:4EtOH),在低温(413 K)下超过16h的结晶时间更适合获得致密且连续的litelite-1膜渗透性能。 M3膜对乙醇/水系统的选择性较低,但对丙酮/水和丁醇/水系统的选择性较高。对于3 wt%的丙酮/水,M3膜对丙酮/水,丁醇/水和乙醇/水的混合物的总通量分别为1.55、0.10和1.51 kg m〜(-2)h〜(-1)。分别为2 wt%的丁醇/水和5 wt%的乙醇/水混合物,相应的分离系数分别为211,150和39。

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