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Borate-containing layered double hydroxide composites: synthesis, characterization and application as catalysts in the Beckmann rearrangement reaction of cyclohexanone oxime

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Abstract

Boron-containing CaAl-layered double hydroxides (LDHs) were prepared by milling, as well as the dehydration–rehydration and the anion-exchange methods. The substances obtained were structurally characterized by powder X-ray diffraction measurements, scanning electron microscopy and infrared spectroscopy. Various borate species could be introduced among the layers and/or the outer surface of the CaAl-LDH. The materials were tested as catalysts in the Beckmann rearrangement of cyclohexanone oxime to ε-caprolactam in the liquid phase, at 373 K. Two of them, the samples prepared by dehydration–rehydration and anion exchange, proved to be active, selective and recyclable catalysts, while the one made by the mechanochemical method was practically inactive. The catalytic activity was tied to intercalated and/or surface-bonded triborate and tetraborate species.

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Acknowledgement

This work was supported by the National Science Fund of Hungary through Grant OTKA NKFI 106234. The financial help is highly appreciated.

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Authors and Affiliations

  1. Department of Organic Chemistry, University of Szeged, Dóm tér 8, Szeged, H-6720, Hungary

    Gábor Varga, Szabolcs Muráth, Áron Bajcsi & István Pálinkó

  2. Materials and Solution Structure Research Group, Institute of Chemistry, University of Szeged, Aradi Vértanúk tere 1, Szeged, H-6720, Hungary

    Gábor Varga, Szabolcs Muráth, Áron Bajcsi, Pál Sipos & István Pálinkó

  3. Department of Applied and Environmental Chemistry, University of Szeged, Rerrich Béla tér 1, Szeged, H-6720, Hungary

    Ákos Kukovecz & Zoltán Kónya

  4. MTA-SZTE “Lendület” Porous Nanocomposites Research Group, Rerrich Béla tér 1, Szeged, H-6720, Hungary

    Ákos Kukovecz

  5. MTA-SZTE Reaction Kinetics and Surface Chemistry Research Group, Rerrich Béla tér 1, Szeged, H-6720, Hungary

    Zoltán Kónya

  6. Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, Szeged, H-6720, Hungary

    Pál Sipos

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  1. Gábor Varga
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  2. Szabolcs Muráth
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  3. Áron Bajcsi
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  4. Ákos Kukovecz
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  5. Zoltán Kónya
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  6. Pál Sipos
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  7. István Pálinkó
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Correspondence to István Pálinkó.

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Varga, G., Muráth, S., Bajcsi, Á. et al. Borate-containing layered double hydroxide composites: synthesis, characterization and application as catalysts in the Beckmann rearrangement reaction of cyclohexanone oxime. Reac Kinet Mech Cat 121, 241–254 (2017). https://doi.org/10.1007/s11144-017-1143-9

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  • DOI: https://doi.org/10.1007/s11144-017-1143-9

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