Synthesis and characterization of the microporous silica phase RUB-3 (RTE)

被引:5
作者
Grünewald-Lüke, A [1 ]
Marler, B [1 ]
Gies, H [1 ]
机构
[1] Ruhr Univ Bochum, Inst Mineral, D-44780 Bochum, Germany
关键词
RUB-3; synthesis; magic-angle spinning nuclear magnetic resonance spectroscopy; RTE; characterization;
D O I
10.1016/S1387-1811(98)00212-1
中图分类号
O69 [应用化学];
学科分类号
081704 ;
摘要
RUB-3 (structure type code: RTE) was hydrothermally synthesized at 150-170 degrees C from reaction mixtures of the following composition: 1.0 SiO2:1.0-5.3 template:0.0-0.67 LiOH:55.5-111.0 H2O. So far, exo-2-aminobicyclo[2.2.1]-heptane is the only known structure-directing agent to stabilize RUB-3. RUB-3 crystallizes together with three other microporous materials: nonasil (NON), dodecasil 1H (DOH) and dodecasil 3C (MTN). The use of LiOH not only reduced the crystallization time but also suppressed the formation of the additional phases. X-ray diffraction analysis and Si-29 magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy proved that the RUB-3 materials possess excellent crystallinity and a perfectly ordered structure. Moreover, the NMR spectra revealed that RUB-3 has a four-connected three-dimensional SiO2 framework that occludes exo-2-aminobicyclo[2.2.1]heptane in the pore system. The SiO2 framework of RUB-3 is stable up to at least 1000 degrees C. Calcination of the as-synthesized RUB-3, however, needs several days for completion. (C) 1998 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:37 / 48
页数:12
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