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

作　　者：漆虹[1] 韩静[1] 江晓骆[1] 邢卫红[1] 范益群[1] 

机构地区：[1]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

出　　处：《无机材料学报》2010年第7期758-764,共7页Journal of Inorganic Materials

基　　金：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

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γ-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。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-Al2O3 disk 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/（m^2·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.

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 

分 类 号：O484[理学—固体物理]