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Catalysts 2017, 7(7), 204; doi:10.3390/catal7070204

Acidity-Reactivity Relationships in Catalytic Esterification over Ammonium Sulfate-Derived Sulfated Zirconia

1
Chemistry Department, Faculty of Science, Minia University, El-Minia 61519, Egypt
2
European Bioenergy Research Institute, Aston University, Birmingham B4 7ET, UK
*
Author to whom correspondence should be addressed.
Received: 31 May 2017 / Revised: 29 June 2017 / Accepted: 29 June 2017 / Published: 5 July 2017
(This article belongs to the Special Issue Mesostructured Materials and Their Catalytic Applications)
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Abstract

New insight was gained into the acidity-reactivity relationships of sulfated zirconia (SZ) catalysts prepared via (NH4)2SO4 impregnation of Zr(OH)4 for propanoic acid esterification with methanol. A family of systematically related SZs was characterized by bulk and surface analyses including XRD, XPS, TGA-MS, N2 porosimetry, temperature-programmed propylamine decomposition, and FTIR of adsorbed pyridine, as well as methylbutynol (MBOH) as a reactive probe molecule. Increasing surface sulfation induces a transition from amphoteric character for the parent zirconia and low S loadings <1.7 wt %, evidenced by MBOH conversion to 3-hydroxy-3-methyl-2-butanone, methylbutyne and acetone, with higher S loadings resulting in strong Brønsted-Lewis acid pairs upon completion of the sulfate monolayer, which favored MBOH conversion to prenal. Catalytic activity for propanoic acid esterification directly correlated with acid strength determined from propylamine decomposition, coincident with the formation of Brønsted-Lewis acid pairs identified by MBOH reactive titration. Monodispersed bisulfate species are likely responsible for superacidity at intermediate sulfur loadings. View Full-Text
Keywords: zirconia; sulfated zirconia; solid acid; XPS; IR; esterification zirconia; sulfated zirconia; solid acid; XPS; IR; esterification
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Rabee, A.I.M.; Mekhemer, G.A.H.; Osatiashtiani, A.; Isaacs, M.A.; Lee, A.F.; Wilson, K.; Zaki, M.I. Acidity-Reactivity Relationships in Catalytic Esterification over Ammonium Sulfate-Derived Sulfated Zirconia. Catalysts 2017, 7, 204.

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