Synthesis and characterization of a nanoporous carbon CMK-3 modified with iron for the ODS of DBT.
Date
2017
Journal Title
Journal ISSN
Volume Title
Publisher
Univesidsad Tecnológica Nacional.
Abstract
A nanostructured Carbon CMK-3 modified with Fe by using different sources of Fe, were
used in the oxidative desulfurization (ODS) of dibenzothiophene as a model sulfur
compound.
Ordered mesoporous carbon CMK-3 was synthesized via a two-step impregnation of the
SBA-15 silica mesonanopores with a solution of sucrose using an incipient wetness method.
The sucrose–silica composite was heated at 1173 K for 4 h under nitrogen flow. The silica template was dissolved in 5 wt.% hydrofluoric acid in order to remove the silica. The
template-free carbon product thus obtained was filtered, washed with deionized water and
ethanol and dried.
Fe-CMK-3 was prepared by wetness impregnation using FeCl3.6H2O and FeNO3.9H2O as
different sources of Fe. A solution of FeCl3.6H2O/ FeNO3.9H2O in ethanol was mixed with
the carbon solution at room temperature. The solution was placed in a rotary evaporator to
remove excess of ethanol at about 333 K and 60 rpm. Afterwards, the sample was dried at
373 K for 18 h and was thermally treated in a dynamic inert (N2) atmosphere. The percentage
of Fe has been 2 wt.% with respect to carbon in the final FeCl3-CMK-3 and FeNO3-CMK 3 material.
Porous carbon CMK-3 and the samples modified with Fe were characterized by XRD, FTIR,
XPS, BET, TEM and SEM. These studies indicated that it was possible to obtain a CMK-3
replica successfully from SBA-15, using sucrose as a carbon precursor. Wide angle XRD
pattern of the sample modified with FeCl3.6H2O implies the formation of the magnetite
phase in the silica channels.
The surface areas were 1320 m2/g for the CMK-3 and 1240 m2/g and 609 m2/g for FeCl3-
CMK-3 and FeNO3-CMK-3, respectively. While the nanomaterial area is significantly
smaller with the incorporation of the metal, CMK-3`s characteristic structure is maintained
after the metal is within the host, in agreement with the XRD studies.
The catalytic activity was improved when the nanoporous carbon was modified with Fe. The
sample modified with FeCl3.6H2O was the most active catalyst for ODS of DBT, using
hydrogen peroxide (H2O2) as oxidant and acetonitrile as solvent. 100% of DBT elimination
was attained at a short time in mild conditions.
Description
Keywords
CMK-3, Iron, ODS of DBT
Citation
XXV International Materials Research Congress.
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