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Adsorptive Properties of Vanadium Substituted ETS-10 Open Access


Other title
Type of item
Degree grantor
University of Alberta
Author or creator
Mani, Farnaz
Supervisor and department
Steven M. Kuznicki (Chemical and Materials Engineering Department)
Examining committee member and department
Dr. Rajender Gupta (Chemical and Materials Engineering Department)
Dr. Anthony Yeung (Chemical and Materials Engineering Department)
Dr. Zhenghe Xu (Chemical and Materials Engineering Department)
Dr. Natalia Semagina (Chemical and Materials Engineering Department)
Dr. Albert Sacco (Chemical Engineering Department, Texas Tech University)
Dr. Steven M. Kuznicki (Chemical and Materials Engineering Department)
Department of Chemical and Materials Engineering
Chemical Engineering
Date accepted
Graduation date
Doctor of Philosophy
Degree level
High purity microporous vanadosilicate (EVS-10/AM-6) has been hydrothermally synthesized by a simple template-free, reducing agent-free method in the absence of titanosilicate ETS-10 seeds. Direct comparison between EVS-10 and ETS-10 showed successful isomorphous substitution of titanium with vanadium in the framework. The existence of vanadium is confirmed by energy dispersive X-ray spectroscopy and inductively coupled plasma mass spectrometry. The scan electron microscopy and the X-ray diffractometer show similar crystal morphology and structure. The structural and adsorptive characteristics of EVS-10 with ETS-10 have been compared. The Henry Law constants and heats of adsorption were calculated for both adsorbents from low pressure adsorption data using CH4, C2H6, C2H4, N2, O2, and CO2 for pressures up to 100 kPa and temperatures of 303, 323, and 343 K. The adsorption data were fit using Langmuir, Toth, and Redlich-Peterson isotherms. The best model was selected based on the quality of fit to the data and how closely the model predicted the saturation concentration. The structural properties for EVS-10 are almost indistinguishable from ETS-10. The adsorption data reflects this similarity in that both adsorbents have similar heats of adsorption and selectivities for a wide range of gases. These results suggest that heteroatom substitution in ETS-10 does not necessarily affect its adsorption properties if the framework dimensions and composition remain similar. A proposal for the differences in the adsorption characteristic for ETS-10 is created by contrasting the adsorption properties of as-synthesized ETS-10 with 13X and high siliceous ZSM-5. To determine whether adsorption on Na-ETS-10 is driven predominately by cationic or van der Waals effects, the adsorption affinity for several gases was measured on all three adsorbents. The adsorption mechanism was probed by using the isotherms to calculate both the enthalpy and entropy of adsorption as a function of loading and by contrasting the behaviour of ETS-10 against both 13X and ZSM-5. The results of the analysis indicate that ETS-10 has, simultaneously, a high affinity for molecules both with and without strong quadrupole moments. This behaviour is believed to result from a sparse number of highly deshielded cations that exist in the otherwise non-polar channels. The phenomenon associated with the ion-exchange of silver ions into the microporous vanadosilicate EVS-10 is explored. The divalent charge on the vanadium is offset by mobile and exchangeable cationic counter-ions. It was found that silver replaces sodium quantitatively and that, unexpectedly, the silver ions are spontaneously reduced to silver metal which appear as nano-scale metal clusters in the TEM images. The reduction of the silver ions is accompanied by an oxidation of the framework vanadium and this redox pair is established through XPS and Raman spectroscopy. The mechanism for this unique behaviour is believed to be explained by a galvanic reaction between the incoming Ag+ and the framework V4+. Separation of ethane from methane from a binary gas mixture was conducted by adsorption on EVS-10. In this study a feed consisted of 80% methane and 20% ethane was used. The bed selectivity resulted from adsorptive separation on EVS-10 was 36 at room temperature and atmospheric pressure. This study suggested that EVS-10 could be an effective candidate for separation of ethane from the gas streams highly enriched in methane. In other words, EVS-10 could be potentially used in cases such as natural gas purification.
Permission is hereby granted to the University of Alberta Libraries to reproduce single copies of this thesis and to lend or sell such copies for private, scholarly or scientific research purposes only. The author reserves all other publication and other rights in association with the copyright in the thesis and, except as herein before provided, neither the thesis nor any substantial portion thereof may be printed or otherwise reproduced in any material form whatsoever without the author's prior written permission.
Citation for previous publication
F. Mani, J. Sawada, S. Kuznicki, A Comparison of the Adsorptive Behaviour of ETS-10, 13X, and Highly Siliceous ZSM-5, Microporous and Mesoporous Materials, 214, 2015, 32-40
. Mani, J. Sawada, S. Kuznicki, Comparative adsorption study of EVS-10 and ETS-10, Microporous and Mesoporous Materials, 204, 2015, 43-49
. Mani, L. Wu, S. Kuznicki, A simplified method to synthesize pure vanadium silicate analogue of ETS-10, Microporous and Mesoporous Materials, 177, 2013, 91-96

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