INVESTIGATION ON ELECTROCHEMICAL ROUTE FOR
SYNTHESIS OF METAL (CU AND FE) ORGANIC FRAMEWORKS:
CHARACTERIZATIONS AND ITS CATALYTIC ACTIVITY
R. Senthil Kumar, S. Senthil Kumar and M.Anbu Kulandainathan*
CSIR-Central Electro Chemical Research Institute, Karaikudi, India.
Email: manbu123@yahoo.com
Metal-organic frameworks (MOFs) are very promising systems due to the
virtually unlimited flexibility in their design. The generation of MOFs enables the
tailoring of novel solids with regular porosity from the micro to nanopore scale.
Nowadays several hundred different types of MOF are known. The self assembly of
metal ions, which act as coordination centres, linked together with a variety of
polyatomic organic bridging ligands, results in tailorable nanoporous host materials as
robust solids with high thermal and mechanical stability. These hybrid organic-inorganic
compounds exhibit rather low-dense and relatively robust three-dimensional architectures
delimiting systems of well-defined cavities or tunnels and they offer new potential
applications include molecular magnetism, ionic conductors, sensors, materials for
adsorption applications (gas separation and gas storage, in particular hydrogen storage)
and heterogeneous catalysis. In heterogeneous catalysis, MOFs can exhibit high activity
and selectivity in oxidation, esterification, epoxide ring openings, asymmetric
hydrogenation, etc.
The metal organic framework material Cu3(BTC)2 (BTC = 1,3,5- benzene
tricarboxylate) has been synthesized using different routes: under solvothermal
conditions in an autoclave, under atmospheric pressure and reflux, microwave synthesis,
ultra sonic synthesis, solvent free solid state synthesis and electrochemical synthesis.
Since electrochemical methods are simple and considerably avoid environmental
pollution, many organic compounds are being synthesized by such methods.
In this work, we have synthesized Cu-BTC and Fe-BTC of MOFs by electrolysis
under the condition of 15V D.C potential were applied in the electrolyte solution,
containing methanol with Tetrabutylammoniumtetrafluoroborate (TBATFB) salt at room
temperature. Interestingly, the addition of TBATFB in electrolyte solution, increase the
conductivity of the electrolyte solution and improve the yield of the products. The
synthesized Cu and Fe MOFs were characterized by XRD, XPS, for studied the structure
and electronic properties. The SEM and TEM were used for morphology of the MOFs
and its surface area was determined by BET. Cyclic voltammetric technique was used to
study their surface of electrochemical behavior and its application of electrocatalytic
activity towards CO2 reduction and chemical catalysis of nitrophenols reductions.