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Preparation and Characterization of Fe-PILCs. Influence of the Synthesis Parameters

Published online by Cambridge University Press:  01 January 2024

José Luis Valverde ,
Amaya Romero ,
Rubí Romero ,
Prado Belén García ,
María Luz Sánchez  and
Isaac Asencio
José Luis Valverde
Affiliation:
Facultad de Ciencias Químicas/Escuela Técnica Agrícola, Departamento de Ingeniería Química, Universidad de Castilla-La Mancha, Campus Universitario s/n, 13071 Ciudad Real, Spain
Amaya Romero*
Affiliation:
Facultad de Ciencias Químicas/Escuela Técnica Agrícola, Departamento de Ingeniería Química, Universidad de Castilla-La Mancha, Campus Universitario s/n, 13071 Ciudad Real, Spain
Rubí Romero
Affiliation:
Facultad de Química, Universidad Autónoma del Estado de México, Paseo Cólon esq. Paseo Tollocan s/n, Toluca, Estado de México, México
Prado Belén García
Affiliation:
Facultad de Ciencias Químicas/Escuela Técnica Agrícola, Departamento de Ingeniería Química, Universidad de Castilla-La Mancha, Campus Universitario s/n, 13071 Ciudad Real, Spain
María Luz Sánchez
Affiliation:
Facultad de Ciencias Químicas/Escuela Técnica Agrícola, Departamento de Ingeniería Química, Universidad de Castilla-La Mancha, Campus Universitario s/n, 13071 Ciudad Real, Spain
Isaac Asencio
Affiliation:
Facultad de Ciencias Químicas/Escuela Técnica Agrícola, Departamento de Ingeniería Química, Universidad de Castilla-La Mancha, Campus Universitario s/n, 13071 Ciudad Real, Spain
*
*E-mail address of corresponding author: amaya.romero@uclm.es
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Abstract

Iron-pillared clays (Fe-PILCs) were synthesized from hydrolyzed FeCl3 solutions added to NaOH solutions using different synthesis conditions. X-ray diffraction, N2 adsorption-desorption, chemical analysis, thermogravimetric analysis, differential thermal analysis, temperature-programmed desorption of ammonia and temperature-programmed reduction were used to characterize the resulting Fe-pillared clays (Fe-PILCs). A higher degree of pillaring was obtained when the Fe content was adjusted to 60 mmoles of Fe/g of clay. It was observed that higher values of this ratio led to worse acidity and textural characteristics, a consequence of the probable formation of Fe oxides that could not only deposit on the surface but also block the pores formed during the pillaring process. Likewise, it was found that the amount of Fe that can be introduced depended on the OH/Fe ratios. Total surface and micropore area decreased and Fe content increased with increasing pillaring solution concentrations. Finally, all pillared samples prepared here were thermally stable at temperatures up to 400°C.

Keywords

AcidityBasal SpacingIronPillared ClaySurface AreaSynthesis
Type
Research Article
Information
Clays and Clay Minerals , Volume 53 , Issue 6 , December 2005 , pp. 613 - 621
Copyright
Copyright © 2005, The Clay Minerals Society

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