Comprehensive Analysis of the Copper Exchange Implemented in Ammonia and Protonated Forms of Mordenite Using Microwave and Conventional Methods

• Main Authors: Marina G. Shelyapina, Ekaterina A. Krylova, Yurii M. Zhukov, Irina A. Zvereva, Inocente Rodriguez-Iznaga, Vitalii Petranovskii, Sergio Fuentes-Moyado
• Format: Article
• Language: English
• Published: MDPI AG 2019-11-01
• Series: Molecules
• Subjects: mordenite; microwave-assisted ion exchange; xrd; icp-oes; nmr; tga; xps.
• Online Access: https://www.mdpi.com/1420-3049/24/23/4216

This article presents the results of a comprehensive study of copper-exchanged mordenite samples prepared from its ammonia and protonated forms (Si/Al = 10) using two different ion exchange methods: conventional and microwave (MW)-assisted. The protonated H-MOR-10 sample was obtained by calcination of commercial NH₄MOR-10; in this case, a slight degradation of the mordenite framework was observed, but the resulting defects were partially restored after the first ion-exchange procedure of protons for copper ions. The level of copper exchange in the studied materials was found to be limited to 70%. Regardless of the exchange procedure, the replacement of ammonium or proton ions with copper led to a linear increase in the <i>a/b</i> ratio of cell parameters in accordance with an increase in the level of copper exchange, which means that all Cu²⁺ cations are ion-exchangeable and enter the main mordenite channel. Thermal analysis indicated a correlation between the replacement of various ammonium and hydroxyl groups by copper ions during the exchange treatment and their dehydroxylation energy during thermal decomposition. As a conclusion: MW-assisted treatment proved itself as an efficacious method for the synthesis of copper-exchanged mordenites, which not only significantly reduces preparation time but leads to a systematically higher copper exchange level.