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http://dx.doi.org/10.14478/ace.2014.1029

Preparation Nanosized TPA-Silicalite-1 with Different Silica Sources and Promoters  

Jung, Sang-Jin (Department of Advanced Materials Engineering, Kyungsung University)
Publication Information
Applied Chemistry for Engineering / v.25, no.3, 2014 , pp. 286-291 More about this Journal
Abstract
In this study, nanosized TPA-silicalite-1 was synthesized with a suitable molar composition of TPAOH: $SiO_2$: $H_2O$ for the development of zeolite ceramic membranes to utilize as gas separation. As silica sources, TEOS, LUDOX AS-40 and CAB-O-SIL were used with the starting material of TPAOH. $NaH_2PO_4$, and a variety of acids and bases were used as promoters after TPAOH, $SiO_2$, $H_2O$ gel synthesis. To decrease synthesis time, a two step temperature change method was applied to the synthesis of TPA-silicalite-1 at a low temperature. TPA-silicalite-1 synthesized was analyzed with XRD, SEM, BET and TGA. As a result, TPA-silicalite-1 powders with a particle size of 100 nm and a specific surface area of $416m^2/g$ were obtained as optimum synthesis conditions when the two stage temperature change method was used with $NaH_2PO_4$ as promoter.
Keywords
silicalite-1; silica source; promoter; nano size; two-stage temperature change;
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1 B. J. Scheoman, J. Sterte, and J. E. Otterstadt, Analysis of the crystal growth mechanism of TPA-silicalite-1, Zeolite, 14, 568-575 (1994).   DOI   ScienceOn
2 Q. Li, Boriana Mihailova, D. Creaser, and J. Sterte, Aging effects on the nucleation and crystallization kinetics of colloidal TPA-silicalite-1, Micro. Meso. Mater., 43, 51-59 (2001).   DOI   ScienceOn
3 S. H. Hyun, J. H. Kim, and J. K. Song, Synthesis and Characterization of Zeolite Composite Membranes (I) : Synthesis of ZSM-5 Type Zeolites, J. Ko, Ceram. Soc., 33, 1064-1072 (1996).   과학기술학회마을
4 D. A. Jacobs and J. A. Marteus, Synthesis of High-Silica Aluminosilicate Zeolite, Studies in Surface Science and Catalysis, 33, 80-101 (1987).
5 E. L. Wu, S. L. Lawton, D. H. Olson, A. C. Rohrman, and G. T. Kokatailo, ZSM-5 Type Materials : Factors Affecting Crystal Symmetry, J. Phy. Chem., 83, 2777-2781 (1979).   DOI
6 E. M. Flanigen, Review and New Perspectives in Zeolite Crystallization, Adv. Chem. Ser., 121, 119-139 (1973).   DOI
7 Z. Gabelica, E. G. Derouane, and N. Blom, Synthesis and characterization of pentasil type zeolites: II. Structure-directing effect of the organic base or cation, Appl. Catal., 5, 109-117 (1983).   DOI   ScienceOn
8 G. T. Kokatailo, S. L. Lawton, D. H. Olison, and W. M. Meier, Structure of Synthetic Zeolite ZSM-5, Nature, 272, 437-438 (1978).   DOI
9 R. Szostak, Molecular Sieves: Principles of Synthesis and Identification, Van Nostrand Reinhold, 79-101, NY, USA (1989).
10 S. H. Hyun, J. K. Song, and J. H. Kim, Synthesis and characterization of zeolite composite membrane (II): Synthesis and $CO_2$ seperation efficiency of ZSM-5 zeolite composite membrane, J. Ko, Ceram. Soc., 34, 747-757 (1997).
11 R. Kumar, P. Mikherjee, R. K. Pandey, P. Rajmohanan, and A. Bhaumik, Role of oxyanions as promoter for enhancing nucleation and crystallization in the synthesis of MFI-type microporous materials, Micro. Meso. Mater., 22, 23-31 (1998).   DOI   ScienceOn
12 C. S. Tsay and A. S. T. Chiang, The synthesis of colloidal zeolite TPA-silicalite-1, Micro. Meso. Mater., 26, 89-99 (1998).   DOI   ScienceOn
13 Q. Li, D. Creaser, and J. Sterte, The nucleation period for TPA-silicalite-1 crystallization determined by a two-stage varying-temperature synthesis, Micro. Meso. Mater., 31, 141-150 (1999).   DOI   ScienceOn
14 S. Mintova and V. Valychev, Effect of the silica source on the formation of nanosized silicalite-1: an in situ dynamic light scattering study, Micro. Meso. Mater., 55, 171-179 (2002).   DOI   ScienceOn
15 R. W. Grose and E.M. Flanigen, Crystalline silica, US Patent 4,061,724 (1977).
16 B. P. Perline, Synthesis of zeolite ZSM-5, US Patent 4,100,262 (1978).
17 A. Erdern and L. B. Sand, Crystallization and metastable phase transformations of zeolite ZSM-5 in the $(TPA)_2O $ $Na_2O$ $K_2O$ $Al_2O_3$ $SiO_2$ $H_2O$ system, J. Catal., 60, 241-256 (1979).   DOI   ScienceOn
18 C. H. Lee, B. J. Ahn, W. Chang, and Y. D. Park, A Study of Quartz Formation from ZSM-5 Zeolite, Appl. Chem, 2, 1016-1019 (1998).
19 R. J. Argaure and G. R. Landolt, Crystalline zeolite zsm-5 and method of preparing the same, US Patent 3,702,886 (1972).
20 Q. Li, Boriana Mihailova, D. Creaser, and J. Sterte, The nucleation period for crystallization of nanosized TPA-Silicalite-1 with varying silica source, Micro. Meso. Mater. 40, 53-62 (2000).   DOI   ScienceOn
21 R. van grieken, J. L. Sotelo, J. M. Menendez, and J. A. Melero, Anomalous crystallization mechanism in the synthesis of nanocrystalline ZSM-5, Micro. Meso. Mater. 39, 135-147 (2000).   DOI   ScienceOn
22 C. Baerlocher, L. B. McCusker, and D. H. Olson, Atlas of zeolite framework types, 6th ed., 212-213, Elsevier, NY, USA (2007).
23 Y. H. Ko, S. J. Kim, M. H. Kim, J. H. Park, J. B. Parise, and Y. S. Uh, New route for synthesizing Mn-silicalite-1, Micro. Meso. Mater., 30, 213-218 (1999).   DOI   ScienceOn