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Issue 27, 2013
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An alkaline one-pot metathesis reaction to give a [Cu3(BTC)2] MOF at r.t., with free Cu coordination sites and enhanced hydrogen uptake properties

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Abstract

A one-pot metathesis reaction between trimesic acid sodium salt and Cu(NO3)2 to yield [Cu3(BTC)2] (HKUST-1) in moderate to good yields, even at room temperature (r.t.) is presented, herein, for the first time. To determine if the basic nature of the metathesis reaction afforded any new physicochemical properties to HKUST-1, three variables were monitored: a) the energy source either from i) ultrasound (US), ii) stirring at room temperature (SRT) or iii) solvothermal (ST) treatment, b) the reaction solvent and c) the reaction time. The metathesis reaction provided DMF·H2O, EtOH·H2O or MeOH·H2O solvates. The compounds were thoroughly characterized by FTIR, XRD, nitrogen adsorption BET surface areas and TGA/DSC data, which indicated the formation of [Cu3(BTC)2] MOFs in eight out of ten synthetic entries. Low-pressure hydrogen uptake experiments revealed values as high as 2.44 wt% for the [Cu3(BTC)2] EtOH·H2O solvates. The [Cu3(BTC)2] MeOH·H2O and [Cu3(BTC)2] EtOH·H2O solvates possess high surface areas, the latter being the metathesis prepared MOF with the least H2O→Cu coordination according to TGA, DSC and a thermal desorption gas chromatographymass spectrometry (GC-MS) coupled technique. This resulted in a material with less chemisorbed H2O and better H2 adsorption capability.

Graphical abstract: An alkaline one-pot metathesis reaction to give a [Cu3(BTC)2] MOF at r.t., with free Cu coordination sites and enhanced hydrogen uptake properties

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Publication details

The article was received on 11 Feb 2013, accepted on 15 Apr 2013 and first published on 18 Apr 2013


Article type: Paper
DOI: 10.1039/C3RA40726H
Citation: RSC Adv., 2013,3, 10962-10972
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    An alkaline one-pot metathesis reaction to give a [Cu3(BTC)2] MOF at r.t., with free Cu coordination sites and enhanced hydrogen uptake properties

    S. Loera-Serna, L. L. Núñez, J. Flores, R. López-Simeon and H. I. Beltrán, RSC Adv., 2013, 3, 10962
    DOI: 10.1039/C3RA40726H

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