小晶粒TS-1分子筛膜的制备及表征

doi:10.3724/SP.J.1077.2011.00085

无机材料学报 ›› 2011, Vol. 26 ›› Issue (1): 85-90.DOI: 10.3724/SP.J.1077.2011.00085 CSTR: 32189.14.SP.J.1077.2011.00085

小晶粒TS-1分子筛膜的制备及表征

王晓东, 延静, 黄伟

太原理工大学煤科学与技术重点实验室,太原030024

收稿日期:2010-04-01 修回日期:2010-05-13 出版日期:2011-01-20 网络出版日期:2010-12-23
作者简介:王晓东(1973-), 女, 博士, 讲师. E-mail: xiaodongwang1973@yahoo.com.cn
基金资助:
国家自然科学基金(20676087); 山西省青年科技研究基金(2009021013); 太原理工大学煤科学与技术教育部与山西省重点实验室开放基金(2008012013-5)

Preparation and Characterization of Ultrafine Crystal TS-1 Films

WANG Xiao-Dong, YAN Jing, HUANG Wei

Key Laboratoryof Coal Science and Technology of Ministry of Education and Shanxi Province,Taiyuan University of Technology, Taiyuan 030024, China

Received:2010-04-01 Revised:2010-05-13 Published:2011-01-20 Online:2010-12-23
Supported by:
National NaturalScience Foundation of China (20676087); Natural Science Foundation of Shanxi(2009021013); The Open Foundation of Key Laboratory of Coal Science andTechnology of Ministry of Education and Shanxi Province (2008012013-5)

摘要/Abstract

摘要： 以椭球形小晶粒TS-1分子筛为晶种, 采用超声法在多孔α-Al₂O₃载体上获得紧密、均匀、连续的晶种层, 经二次生长形成小晶粒的TS-1分子筛膜. 通过改变合成液碱度(OH^-/Si)和晶化时间等合成参数, 调变分子筛膜的微结构. SEM和XRD检测结果表明, 当OH^-/Si＝0.09, 水热合成24h时, 晶种没有交联成膜, 延长晶化时间至48h, 可得到致密交联的TS-1分子筛膜, 晶体的大小约为500nm, 进一步延长晶化时间至72h时, 膜的结晶度降低, 表面覆盖一层无定形物质. 提高碱度, OH^-/Si＝0.21, 水热反应24h, 得到的膜结构不对称, 上层是高度交联的致密分子筛膜, 晶粒大小约为400nm, 致密膜与载体之间没有交联生长的晶种.

关键词: 小晶粒, TS-1分子筛膜, 二次生长法

Abstract: The compact, uniform and continuousseed layers were prepared on porous α-Al₂O₃ substrateswith oval-shaped and ultrafine seed crystals by ultrasonic seeding, and then TS-1films were formed after secondary growth. The microstructure of the films couldbe regulated by changing the ratios of OH^-/Si and the crystallizationtime. SEM and XRD results reveal that when the ratio of OH^-/Si is equal to0.09, after 24h of crystallization time, the film is not interconnected. If thecrystallization time is prolonged to 48h, the film have become dense and interconnected,the crystals in which are about 500nm, and when the reaction time is prolongedto 72h, the crystallinity of the film decreases, and the surface of the film iscovered with a layer of amorphous materials. When the ratio of OH^-/Si is increasedto 0.21, after 24h of crystallization time, the crystal grains in the top layerare about 400nm and the structure of the TS-1 film is asymmetric, with a denseand uniform TS-1 layer on top, the support at the bottom, and the seed layer inbetween.

Key words: ultrafinecrystal, TS-1Films, secondary growth

中图分类号:

TQ174

王晓东, 延静, 黄伟. 小晶粒TS-1分子筛膜的制备及表征[J]. 无机材料学报, 2011, 26(1): 85-90.

WANG Xiao-Dong, YAN Jing, HUANG Wei. Preparation and Characterization of Ultrafine Crystal TS-1 Films[J]. Journal of Inorganic Materials, 2011, 26(1): 85-90.

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小晶粒TS-1分子筛膜的制备及表征

Preparation and Characterization of Ultrafine Crystal TS-1 Films

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