Zones, S. I. and Hwang, Son-Jong (2011) A novel approach to borosilicate zeolite synthesis in the presence of fluoride. Microporous and Mesoporous Materials, 146 (1-3). pp. 48-56. ISSN 1387-1811 http://resolver.caltech.edu/CaltechAUTHORS:20111108-160000068
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A synthetic route to borosilicate zeolites is described which yields relatively boron-rich products. The reaction takes place under high reactant concentrations and utilizes fluoride delivered as the ammonium fluoride salt rather than as hydrofluoric acid. The reaction is an adaptation of the conditions (HF) initially used to discover zeolite SSZ-70. Exploring a range of structure-directing agents (SDA), several boron-rich phases crystallized. Reactions are generally quite slow, however. A more in-depth study with an adamantyl SDA finds zeolite SSZ-23 favored over SSZ-13. Multinuclear NMR experiments were carried out to better understand the boron substitution in SSZ-23 and to probe if there are key B–F interactions in its formation. Finally, providing alkali cation sources of fluoride shifts the product selectivity away from SSZ-23 and back toward SSZ-13.
|Additional Information:||© 2011 Elsevier B.V. Received 14 March 2011; revised 27 May 2011; Accepted 27 May 2011. Available online 14 June 2011. The authors thank Anna Jackowski at Chevron for help in the synthesis studies and Dr. JinYi Han at Chevron for help in the analysis of the x-ray data related to the boron levynite product. We thank Dr. Ray Archer for providing imidazolium SDA C104-106 and 123. Chevron managers, Dr. Charles Wilson and Georgie Scheuerman are thanked for their continued support of the New Materials research program. Kelly Harvey is thanked for graphics work in the paper. The NMR facility at Caltech was supported by the National Science Foundation (NSF) under Grant Number 9724240 and partially supported by the MRSEC Program of the NSF under Award Number DMR-520565.|
|Subject Keywords:||Borosilicate molecular sieves; Fluoride structure-direction; SSZ-13; 19F–11B HETCOR NMR; Adamantyl quaternary ammonium cations|
|Official Citation:||S.I. Zones, Son-Jong Hwang, A novel approach to borosilicate zeolite synthesis in the presence of fluoride, Microporous and Mesoporous Materials, Volume 146, Issues 1-3, December 2011, Pages 48-56, ISSN 1387-1811, 10.1016/j.micromeso.2011.05.034.|
|Usage Policy:||No commercial reproduction, distribution, display or performance rights in this work are provided.|
|Deposited By:||Jason Perez|
|Deposited On:||09 Nov 2011 15:45|
|Last Modified:||09 Nov 2011 15:45|
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