无机材料学报 ›› 2018, Vol. 33 ›› Issue (3): 345-351.DOI: 10.15541/jim20170205

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超稀溶液体系中高性能MFI型沸石膜的制备及表征

黄攀1, 周亮1, 李华征1, 李洪健1, 杨建华2, 王金渠1, 2   

  1. 大连理工大学1. 盘锦校区, 精细化工国家重点实验室, 石油与化学工程学院, 盘锦 124221;
    2. 精细化工国家重点实验室, 吸附与无机膜研究所, 大连 116024
  • 收稿日期:2017-04-28 修回日期:2017-06-08 出版日期:2018-03-20 发布日期:2018-03-12
  • 作者简介:黄 攀(1988-), 男, 硕士研究生. E-mail: huangpanchem@sina.com
  • 基金资助:
    国家高新技术研究发展计划(863计划) (2015AA03A602)

Preparation and Characterization of High Performance MFI Zeolite Membrane in Ultradilute Solution

HUANG Pan1, ZHOU Liang1, LI Hua-Zheng1, LI Hong-Jian1, YANG Jian-hua2, WANG Jin-Qu1, 2   

  1. 1. School of Petroleum and Chemical Engineering, State Key Laboratory of Fine Chemicals, Dalian University of Technology, Panjin Campus, Panjin 124221, China;
    2. Institute of Adsorption and Inorganic Membrane, State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, China
  • Received:2017-04-28 Revised:2017-06-08 Online:2018-03-20 Published:2018-03-12
  • About author:HUANG Pan. E-mail: huangpanchem@sina.com
  • Supported by:
    National High Technology Research and Development Program of China (2015AA03A602)

摘要:

以廉价管状大孔α-Al2O3作为载体, 采用二次生长法, 在超稀溶液体系(H2O/SiO2=1000)中成功制备了高性能MFI型沸石膜, 分别考察晶种尺寸和H2O/SiO2对沸石膜的形貌及渗透蒸发性能的影响。结果表明, 尺寸为0.4 μm晶种制备的晶种层具有更大的晶核密度, 能够增加载体表面的成核位点, 因此对沸石膜的生长具有更强的诱导作用。超稀溶液体系中低浓度的模板剂和硅源环境能够控制沸石晶体的生长速率, 从而降低沸石膜厚度, 同时可以抑制晶间缺陷的形成。将制备的沸石膜用于60℃渗透蒸发分离5wt%乙醇/水混合物, 分离因子α(乙醇/水)和渗透通量分别为47和4.09 kg/(m2·h)。采用超稀的合成液配方和廉价大孔载体, 既可以降低沸石膜制备的原料成本, 又可以提高沸石膜的渗透通量, 显示出MFI型沸石膜在脱除水中低浓度有机物潜在的工业化应用前景。

 

关键词: MFI型沸石膜, 管状大孔α-Al2O3载体;, 超稀溶液, 渗透蒸发

Abstract:

High performance MFI-type zeolite membrane was successfully prepared in ultradilute solution (H2O/SiO2= 1000) on inexpensive and macroporous α-Al2O3 tubular support by secondary growth. Influences of seed size and H2O/SiO2 on morphology and pervaporation performance of the zeolite membranes were investigated. Results showed that the seed layer prepared with 0.4 μm seeds had higher crystal nucleus density which could increase the amount of the nucleation site on the support surface, resulting in a stronger induced effect on the growth of zeolite membrane. The low-concentration template and silicon source in ultradilute solution decreased the growth rate of zeolite crystals, which could reduce the zeolite membrane thickness and effectively inhibited the formation of intercrystalline defects. The flux and separation factor (αethanol/water) of the resulting MFI zeolite membrane achieved 4.09 kg/(m2·h1) and 47, respectively, for separation of 5wt% ethanol/water mixture at 60℃. Ultradilute solution and low-cost macroporous α-Al2O3 tubular support reduced the preparation cost of MFI zeolite membranes and increased the flux, showing prospect of the potential industrial application of MFI-type zeolite membrane for removal of the low-concentration organic compounds in water.

Key words: MFI zeolite membrane, macroporous α-Al2O3 tubular support;, ultradilute solution, pervaporation

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