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Effect of the method and impregnation time on the surface acidity of zirconia modified with boron

  • Original Paper: Characterization methods of sol-gel and hybrid materials
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Abstract

In this paper, the synthesis and characterization of boron-modified zirconia is reported. The zirconium hydroxide obtained by sol-gel was modified with boric acid, in order to increase the surface acidity of the zirconia. For this purpose, two impregnation methods were used: conventional and ultrasonic, and the impregnation time was set at 1 or 4 h. The synthesized materials were characterized by thermal analyses, X-ray diffraction, infrared spectroscopy, nitrogen physisorption, and scanning electron microscopy. The boron incorporation delayed the crystallization of solids, which were mainly amorphous but with tendency toward the formation of the tetragonal phase. The modified materials were micro-mesoporous and their specific area was improved, while the pure zirconia showed a lower nitrogen adsorption. Units BO3 and BO4 were identified, confirming the boron presence. In general, the solids showed spherical particles; however, the ultrasonic treatment originated elongated particles. In addition, the acidic properties were evaluated by potentiometric titration and ethanol decomposition. The maximum acid strength of the zirconia increased from −28 mV to over 200 mV; consequently, all the boron-modified materials showed strong and very strong acid sites. The influence on the catalytic activity, due to the method and impregnation time, was clearly observed in the ethanol decomposition. The most active catalysts were those obtained by the ultrasonic method and the best was that impregnated during 1 h.

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Acknowledgements

The authors are grateful to the National Council of Science and Technology (CONACyT) for the Scholarship (227552) granted to María Isabel Arregoitia Quezada, and we also wish to thank the National Technological of Mexico (TecNM) for financial support given during development of this research work (5531.15-P).

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Authors and Affiliations

  1. Centro de Investigación en Petroquímica Secundaria del Instituto Tecnológico de Ciudad Madero (CIPS-ITCM), Prolongación Bahía de Adair, Av. de las Bahías, Parque de la Pequeña y Mediana Industria, Altamira, Tamaulipas, México

    María Isabel Arregoitia-Quezada, Ricardo García-Alamilla, Juan Manuel Hernández-Enríquez & José Luis Rivera-Armenta

  2. Centro de Investigación en Materiales Avanzados (CIMAV), Av. Miguel de Cervantes 120, 31109, Chihuahua, Chihuahua, México

    Francisco Paraguay-Delgado

  3. Centro Interdisciplinario de Investigaciones y Estudios sobre Medio Ambiente y Desarrollo del Instituto Politécnico Nacional (CIIEMAD-IPN), 30 de Junio de 1520 S/N, Barrio La Laguna Ticomán, Cd. de México, Distrito Federal, México

    Luz Arcelia Garcia-Serrano

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  1. María Isabel Arregoitia-Quezada
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  2. Ricardo García-Alamilla
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  3. Juan Manuel Hernández-Enríquez
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Correspondence to Ricardo García-Alamilla.

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Arregoitia-Quezada, M.I., García-Alamilla, R., Hernández-Enríquez, J.M. et al. Effect of the method and impregnation time on the surface acidity of zirconia modified with boron. J Sol-Gel Sci Technol 82, 28–39 (2017). https://doi.org/10.1007/s10971-016-4284-9

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  • DOI: https://doi.org/10.1007/s10971-016-4284-9

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