The Catalyst Review - September 2015 - 14

EXPERIMENTal

Controlled formation of Nickel Oxide Nanoparticles on Mesoporous
Silica using Molecular Ni4O4 Clusters as Precursors: Enhanced Catalytic
Performance for Dry Reforming of Methane...
Recent efforts aimed at achieving higher conversion rates
for the dry reforming of methane (DRM) have focused
on catalyst design and optimization. Nickel has long been
recognized as an efficient non-noble metal catalyst for the
DRM reaction. However, high and stable conversions can
be reached only if very small Ni particles are dispersed
on a high-surface-area support designed to prevent
deactivation via sintering and/or coking. Herein, the
authors describe the use of small molecular metal-oxo
clusters instead of mononuclear metal salts which act
as single source precursors (SSP), for which all desired
elements of the target material are pre-organized in a
metal organic compound. Specifically, they chose [Ni4O4]
cubane, (Figure 1), which, when attached to the surface of
a high-surface-area support which, after calcination, yields
four Ni atoms in close proximity on the support surface. It
was prepared from Ni(OAc)2 and di-2-pyridinylmethanone
[(C5H4N)2CO, dpk]; dpk is hydrolyzed into the di-2 pyridinylmethanediolato [(C5H4N)2C(OH)2, dpd] ligand in aqueous
solution. Subsequent reduction affords very small clusters
of Ni allowing for increased efficiency in the reforming of
methane.
These workers prepared two series of materials for this
study. The first made use of a mesoporous silica support
(SBA-15) which was impregnated with an aqueous
solution of the Ni4 cubane precursor ("A-Ni4/SBA-15"). For
comparison, the second made use of a conventional nickel
acetate precursor and was used in the same way ("A-Ni/
SBA-15", A=initial wt% of Ni).

figure 1. Schematic illustration of the Ni4/Sba-15 catalyst prepared by
using a ligand-stabilized Ni4 cubane precursor.

Table 1. Characterization and test results of the Ni4/Sba-15 and Ni/
Sba-15 catalysts.

figure 2. Catalysis results based on mole methane converted per mole
nickel per minute.

All samples were first dried at room temperature, then
calcined at 550 ºC for 4h, and finally subjected to an in
situ reducing atmosphere (pure H2) at 500 ºC for 1h before
catalytic tests. After calcination, the actual metal contents
of the samples were determined using inductively coupled
plasma (Table 1). Their catalytic efficiency is shown in
Figure 2. The authors postulate that the Ni4 cubane
precursor seems to combine two advantages by first
allowing the fast formation of small Ni clusters, which are
highly dispersed on the support and quite stable during
the catalytic reaction. Source: Baktash E, Littlewood P,
Pfrommer J, et al. (2015) ChemCatChem 7: 1280-1284.

14

The Catalyst Review

September 2015



The Catalyst Review - September 2015

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The Catalyst Review - September 2015 - Cover 2
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