有机-无机复合SiO2膜的制备及水蒸气稳定性能研究

doi:10.3724/SP.J.1077.2010.00758

无机材料学报 ›› 2010, Vol. 25 ›› Issue (7): 758-764.DOI: 10.3724/SP.J.1077.2010.00758 CSTR: 32189.14.SP.J.1077.2010.00758

有机-无机复合SiO₂膜的制备及水蒸气稳定性能研究

漆虹, 韩静, 江晓骆, 邢卫红, 范益群

(南京工业大学膜科学技术研究所, 材料化学工程国家重点实验室, 南京 210009)

收稿日期:2009-11-09 修回日期:2010-01-31 出版日期:2010-07-20 网络出版日期:2010-06-10
基金资助:
国家重点基础研究发展计划(2009CB623400); 国家自然科学青年基金(20906047); 材料化学工程联合国家重点实验室开放课题(SKL–ChE–09A01); 南京市留学回国人员基金

Preparation and Hydrothermal Stability of Organic-inorganic Hybrid Silica Membrane

QI Hong, HAN Jing, JIANG Xiao-Luo, XING Wei-Hong, FAN Yi-Qun

(State Key Laboratory of Materials-oriented Chemical Engineering, Membrane Science and Technology Research Center, Nanjing University of Technology, Nanjing 210009, China)

Received:2009-11-09 Revised:2010-01-31 Published:2010-07-20 Online:2010-06-10

摘要/Abstract

摘要：

以1, 2-二(三乙氧基硅基)乙烷为前驱体, 通过溶胶-凝胶法合成出稳定的纳米复合SiO₂溶胶, 采用浸浆法在具有g-Al₂O₃/α-Al₂O₃结构的片状载体上涂膜, 然后在N₂气氛下烧成得到完整无缺陷的有机-无机复合SiO₂膜. 以TG/DSC、BET和气体渗透性能测试等手段对复合SiO₂膜及粉体进行了表征. 该膜对小分子气体(He、CO₂、O₂、N₂、CH₄和SF₆)的分离表现出分子筛分效应, 对He的渗透通量为(1.0~3.5)´10^-7mol/(m²·s·Pa)(200℃, 0.3MPa). 500℃烧成的膜对He/CO₂的理想分离因子为47, 远远高于Knudsen扩散时He/CO₂的理想分离因子(3.3). 详细考察了烧成温度对膜水热稳定性的影响. 结果表明: 在450、500和550℃三个温度下烧成的膜水蒸气稳定条件(分压)分别为200、500和1000kPa.

关键词: 微孔陶瓷膜, 有机-无机复合SiO₂膜, 水热稳定性, 气体分离

Abstract:

A new organic-inorganic hybrid microporous membrane was prepared via Sol-Gel method with bridged silsesquioxane (1, 2-bis(triethoxysilyl)ethane, BTESE) as a precursor. Macroporous α-Al₂O₃disk supported mesopo- rous γ-Al₂O₃ layer was used as support. Defect-free hybrid silica membrane was deposited on such support by using a stable nano-sized sol and subsequently calcining in pure nitrogen atmosphere. The hybrid SiO₂ membrane as well as the powder was characterized by TG/DSC, BET and gas permeation. The hybrid silica membranes exhibit molecular sieve properties for small gases like He, CO₂, O₂, N₂, CH₄, and SF₆ with helium permeance in the range of (1.0-3.5)´10^-7mol/(m²·s·Pa)(at 200℃, 0.3MPa). Considering the membrane calcined at 500℃, it is found that the permselectivity of the He (0.255nm) with respect to CO₂(0.33nm) is 47, which is much higher than the corresponding Knudsen value (He/CO₂=3.3). Effect of calcination temperature on hydrothermal stability of those microporous membranes was studied in detail. Results show that the performances of hybrid SiO₂ membranes calcined at 450℃, 500℃ and 550℃ deteriorate under a H₂O partial pressure of 200, 500 and 1000kPa, respectively.

Key words: microporous ceramic membrane, hybrid organic-inorganic SiO₂membrane, hydrothermal stability, gas separation

中图分类号:

O484

漆虹, 韩静, 江晓骆, 邢卫红, 范益群. 有机-无机复合SiO₂膜的制备及水蒸气稳定性能研究[J]. 无机材料学报, 2010, 25(7): 758-764.

QI Hong, HAN Jing, JIANG Xiao-Luo, XING Wei-Hong, FAN Yi-Qun. Preparation and Hydrothermal Stability of Organic-inorganic Hybrid Silica Membrane[J]. Journal of Inorganic Materials, 2010, 25(7): 758-764.

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有机-无机复合SiO₂膜的制备及水蒸气稳定性能研究

Preparation and Hydrothermal Stability of Organic-inorganic Hybrid Silica Membrane

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