二次生长法制备微纤复合纯硅分子筛膜  

Preparation of Microfibrous Supported Silicalite-1 Zeolite Membrane by Secondary Growth Method

作　　者：刘剑[1] 鄢瑛[2] 张会平[2] 

机构地区：[1]衡阳师范学院功能金属有机材料湖南省高校重点实验室,湖南衡阳421008 [2]华南理工大学化学与化工学院,广东广州510641

出　　处：《高校化学工程学报》2015年第2期432-437,共6页Journal of Chemical Engineering of Chinese Universities

基　　金：国家自然科学基金资助项目(21176086);广东省绿色化学产品技术重点实验室资助(GC201203);湖南省重点学科基金资助项目;衡阳师范学院科学基金项目(12B25)

摘　　要：以正硅酸乙酯为硅源,采用二次生长法制备了不锈钢微纤复合纯硅分子筛膜,考察了载体预处理方式、晶化温度和晶化时间对分子筛膜性能的影响,利用X射线衍射仪(XRD)、扫描电镜(SEM)和ASAP-2020自动吸附仪对其形态和微观结构进行分析表征。结果表明,采用阳极氧化法预处理载体所制备的纯硅分子筛膜较采用高温煅烧法预处理的膜表观形态更为连续规整。随着晶化温度从100℃升高到160℃或晶化时间从12 h延长到96 h,分子筛膜表面更加致密,晶体颗粒尺寸增加。不锈钢微纤复合纯硅分子筛膜的比表面积、总孔容和微孔孔容分别为93.24 m2?g?1、0.0654cm3?g?1和0.0382 cm3?g?1,微孔孔容占总孔容的58%,相应的纯硅分子筛膜负载量为23.3%(wt)。Stainless steel microfibrous supported silicalite-1 zeolite membrane（silicalite-1 membrane/SMF） was prepared by secondary growth method from TEOS as Si source. The effects of different operation parameters such as support pretreatment methods, crystallization temperature and crystallization time on the silicalite-1 membrane/SMF were studied. The morphology and microstructure of silicalite-1 membrane/SMF were characterized by XRD, SEM and ASAP-2020 automatic adsorption instrument, respectively. The results show that the silicalite-1 zeolite membrane prepared by treating support with anodic oxidation method is more continuous and denser than that with calcinations. The surface of zeolite membrane is much denser and the size of crystal grains increases with increasing the crystallization temperature from 100℃ to 160℃ or prolonging the crystallization time from 12 h to 96 h. The specific surface areas, total pore volume and micropore volume of the silicalite-1 membrane/SMF are 93.24 m2·g^1, 0.0654 cm3？g？1 and 0.0382 cm3·g^1, respectively. The percentage of micropore volume is 58% of total pore volume. The silicalite-1 membrane content determined for silicalite-1/SMF composite is 23.3 %（wt）.

关 键 词：分子筛膜 不锈钢纤维 二次生长法 阳极氧化法 晶化温度 晶化时间 

分 类 号：O647.33[理学—物理化学]