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Copolymerization of transition metal salen complexes and conversion into metal nanoparticles supported on hierarchically porous carbon monoliths: a one pot synthesis

  • Original Paper: Nano- and macroporous materials (aerogels, xerogels, cryogels, etc.)
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Abstract

Described is the synthesis of metal (Ni, Cr, and Mn) doped macro/mesoporous carbon monoliths by co-polymerization of transition metal complexes with resorcinol/formaldehyde and subsequent pyrolysis. Two salen ligands were synthesized via reaction of ethylene diamine (EDA) and 1,6-diaminohexane (DAH) with 2,4-dihydroxybenzaldehyde to give 4,4′-((1E,1′E)-(ethane-1,2-diylbis(azanylylidene))bis(methanylylidene))bis(benzene-1,3-diol) (=E-salen) and 4,4′-((1E,1′E)-(hexane-1,6-diylbis(azanylylidene))bis(methanylylidene))bis(benzene-1,3-diol) (=D-salen). Their metal salen complexes were prepared. All the samples pyrolyzed at 500 °C had macro and mesopores with a specific surface area ranging from 250–500 m2/g. However, the surface area and porosity of the samples decreased dramatically for the metal containing samples pyrolyzed at 800 °C. This is suggested to result from incomplete co-polymerization of the metal salen complexes. The extent of graphitization determined from Raman increased with the pyrolysis temperature. The electrical conductivity was found to increase with the pyrolysis temperature, and followed the trend Ni > Mn > Cr. The M-E-salen containing samples had significantly lower conductivity than their D-salen counterparts.

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Acknowledgements

The technical assistance of Dr. Ken Belmore in the collection and interpretation of the NMR spectra is greatly appreciated. The authors acknowledge the Central Analytical Facility (CAF) at the University of Alabama for support and technical assistance. A seed grant from the CAF at The University of Alabama is acknowledged, the required cost match for which was provided by the Bakker Research Gift fund. TVK acknowledges support from the Research Simulation program of the Office of Research at The University of Alabama.

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  1. Department of Chemistry, The University of Alabama, Tuscaloosa,, AL 35487-0336, USA

    Trupti V. Kotbagi, Kevin H. Shaughnessy, Sefadzi Tay-Agbozo & Martin G. Bakker

  2. Department of Chemical and Biological Engineering, The University of Alabama, Tuscaloosa,, AL 35487-0203, USA

    Christian LeDoux, Hyunseok Cho & John van Zee

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A number of the authors (M.G.B., T.V.K., K.H.S.) have a potential conflict of interest. They are co-inventors of work described in this and prior papers for which the University of Alabama has applied for multiple patents. A granted patent is licensed to a company that M.G.B. and T.V.K. have an ownership interest in.

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This paper is accompanied by Online Resources consisting of: NMR spectra of E-salen and D-Salen ligands, and Ni-E-Salen complex. Tables of fits to XRD, Raman, and Electrical Conductivity and correlations to mesopore volumes. The original Raman spectra and X-Ray diffractograms.

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Kotbagi, T.V., Shaughnessy, K.H., LeDoux, C. et al. Copolymerization of transition metal salen complexes and conversion into metal nanoparticles supported on hierarchically porous carbon monoliths: a one pot synthesis. J Sol-Gel Sci Technol 84, 258–273 (2017). https://doi.org/10.1007/s10971-017-4510-0

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