Hierarchical Zeolites Prepared Using a Surfactant-Mediated Strategy: ZSM-5 vs. Y as Catalysts for Friedel–Crafts Acylation Reaction

Author:

Martins Angela12ORCID,Amaro Beatriz1,Santos M. Soledade C. S.23,Nunes Nelson12ORCID,Elvas-Leitão Ruben12ORCID,Carvalho Ana P.23

Affiliation:

1. Departamento de Engenharia Química, Instituto Superior de Engenharia de Lisboa, IPL, R. Conselheiro Emídio Navarro, 1, 1959-007 Lisboa, Portugal

2. Centro de Química Estrutural, Faculdade de Ciências, Institute of Molecular Sciences, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal

3. Departamento de Química e Bioquímica, Faculdade de Ciências Universidade de Lisboa, Ed.C8, Campo Grande, 1749-016 Lisboa, Portugal

Abstract

Hierarchical ZSM5 and Y zeolites were prepared through a surfactant-mediated strategy with NH4OH changing the duration of the treatment and the amount of CTAB surfactant and taking as reference multiples of the critical micellar concentration (CMC). The materials were characterized using powder X-ray diffraction, N2 adsorption isotherms at −196 °C, and SEM and TEM microscopy. The catalytic performance was evaluated in Friedel–Crafts acylation of furan with acetic anhydride at 80 °C. The alkaline surfactant-mediated treatment had different effects on the two zeolites. For ZSM5, the CTAB molecular aggregates can hardly diffuse inside the medium-size pores, leading mainly to intercrystalline mesoporosity and increased external surface area, with no positive catalytic impact. On the other hand, for large-pore Y zeolite, the CTAB molecular aggregates can easily diffuse and promote the rearrangement of crystal units around micelles, causing the enlargement of the pores, i.e., intracrystalline porosity. The optimized Y-based sample, treated for 12 h with a CTAB amount 32 times the CMC, shows an increase in product yield and rate constant that was not observed when a higher amount of surfactant was added. The reuse of spent catalysts upon thermal treatment at 400 °C shows a regeneration efficiency around 90%, showing good potentialities for the modified catalysts.

Funder

Fundação para a Ciência e Tecnologia

Publisher

MDPI AG

Subject

Chemistry (miscellaneous),Analytical Chemistry,Organic Chemistry,Physical and Theoretical Chemistry,Molecular Medicine,Drug Discovery,Pharmaceutical Science

Reference33 articles.

1. Sartori, G., and Maggi, R. (2009). Advances in Friedel-Crafts Acylation Reactions: Catalytic and Green Processes, CRC Press.

2. Franck, H.-G., and Stadelhofer, J.W. (1988). Industrial Aromatic Chemistry, Springer. [1st ed.].

3. van Bekkun, H. (2008). Fine Chemicals Trough Heterogeneous Catalysis, Wiley-VCH.

4. Figueiredo, J.L., Pereira, M.-M., and Faria, J. (2008). Catalysis from Theory to Application, Coimbra University Press.

5. Zeolites for Fine Chemicals Production;Clerici;Top. Catal.,2000

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