NDLI: Synthesis of ordered porous zirconia containing sulfate ions and evaluation of its surface acidic properties

Content Provider	Springer Nature Link
Author	Haneda, Masaaki Takamura, Kenji Doi, Yasuyuki Bion, Nicolas Vivier, Laurence
Copyright Year	2017
Abstract	The synthesis and characterization of sulfated ZrO$_{2}$ with ordered pores as a solid acid catalyst were investigated. Ordered porous ZrO$_{2}$ containing sulfate ions was synthesized by hydrolysis of zirconium n-propoxide in the presence of HCl, surfactant and (NH$_{4}$)$_{2}$SO$_{4}$ dissolved in distilled water, when the SO$_{4}$/Zr molar ratio was changed in the range of 0.8–1.4. BET surface area of sulfated ZrO$_{2}$ thus synthesized was found to be 150–160 m$^{2}$ g$^{−1}$. The presence of sulfate ions in ZrO$_{2}$ was confirmed by an appearance of IR band at ca. 1398 cm$^{−1}$ in the IR spectra of sulfated ZrO$_{2}$. Since two IR bands due to surface hydroxyl groups were still observed for sulfated ZrO$_{2}$, the possibility that sulfate ions are highly dispersed on the surface of ordered porous ZrO$_{2}$ was suggested. From the evaluation of surface acidity by NH$_{3}$-TPD measurements, not only the amount of NH$_{3}$ desorption but also the strength of acid sites related to NH$_{3}$ desorption temperature were found to be increased with increasing the SO$_{4}$/Zr ratio up to 1.2. On the other hand, FTIR spectroscopy following pyridine adsorption revealed that the maximum surface density of Brønsted acid sites was attained for sulfated ZrO$_{2}$ with SO$_{4}$/Zr ratio of 1.0. Sulfate species interacting strongly with nano-sized tetragonal ZrO$_{2}$ was considered to be responsible for the creation of Brønsted acid sites. In accordance with the surface density of Brønsted acid sites, sulfated ZrO$_{2}$ with SO$_{4}$/Zr ratio of 1.0 showed the highest activity for the skeletal isomerization of 3,3-dimethylbut-1-ene, which predominantly occurs on Brønsted acid sites.
Starting Page	5835
Ending Page	5845
Page Count	11
File Format	PDF
ISSN	00222461
Journal	Journal of Materials Science
Volume Number	52
Issue Number	10
e-ISSN	15734803
Language	English
Publisher	Springer US
Publisher Date	2017-01-24
Publisher Place	New York
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Materials Science Characterization and Evaluation of Materials Polymer Sciences Continuum Mechanics and Mechanics of Materials Crystallography and Scattering Methods Classical Mechanics
Content Type	Text
Resource Type	Article
Subject	Ceramics and Composites Mechanics of Materials Mechanical Engineering Polymers and Plastics

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