Y and ZSM-5 Hierarchical Zeolites Prepared Using a Surfactant-Mediated Strategy: Effect of the Treatment Conditions

Author:

Ruggiu Andrea12ORCID,Carvalho Ana Paula34,Rombi Elisabetta12ORCID,Martins Angela35ORCID,Rocha João6,Parpot Pier78ORCID,Neves Isabel C.78ORCID,Cutrufello Maria Giorgia12ORCID

Affiliation:

1. Department of Chemical and Geological Sciences, University of Cagliari, Complesso Universitario di Monserrato, S.S. 554, 09042 Monserrato, CA, Italy

2. National Interuniversity Consortium of Materials Science and Technology (INSTM), Via Giusti 9, 50121 Florence, Italy

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

4. Departamento de Química e Bioquímica, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal

5. Departamento de Engenharia Química, Instituto Superior de Engenharia de Lisboa, Instituto Politécnico de Lisboa, Rua Conselheiro Emídio Navarro, 1959-007 Lisboa, Portugal

6. Departamento de Química and CICECO, Universidade de Aveiro, 3810-193 Aveiro, Portugal

7. CQUM—Centre of Chemistry, Chemistry Department, University of Minho, Campus de Gualtar, 4710-057 Braga, Portugal

8. CEB—Centre of Biological Engineering, University of Minho, Campus de Gualtar, 4710-057 Braga, Portugal

Abstract

Diffusional limitations associated with zeolite microporous systems can be overcome by developing hierarchical zeolites, i.e., materials with a micro- and mesoporous framework. In this work, Y and ZSM-5 zeolites were modified using a surfactant-mediated hydrothermal alkaline method, with NaOH and cetyltrimethylammonium bromide (CTAB). For Y zeolite, after a mild acidic pretreatment, the effect of the NaOH+CTAB treatment time was investigated. For ZSM-5 zeolite, different concentrations of the base and acid solutions were tested in the two-step pretreatment preceding the hydrothermal treatment. The properties of the materials were studied with different physical–chemical techniques. Hierarchical Y zeolites were characterized by 3.3–5 nm pores formed during the alkaline treatment through the structure reconstruction around the surfactant aggregates. The effectiveness of the NaOH+CTAB treatment was highly dependent on the duration. For intermediate treatment times (6–12 h), both smaller and larger mesopores were also obtained. Hierarchical ZSM-5 zeolites showed a disordered mesoporosity, mainly resulting from the pretreatment rather than from the subsequent hydrothermal treatment. High mesoporosity was obtained when the concentration of the pretreating base solution was sufficiently high and that of the acid one was not excessive. Hierarchical materials can be obtained for both zeolite structures, but the pretreatment and treatment conditions must be tailored to the starting zeolite and the desired type of mesoporosity.

Funder

Fundação para a Ciência e a Tecnologia

Publisher

MDPI AG

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