Paper
Catalysis Science & Technology
the quartz IR cell with CaF2 windows. Spectra were measured
accumulating 30 scans at a resolution of 4 cm−1. A reference
spectrum of the catalyst wafer in He taken at measurement
temperature was subtracted from each spectrum. Prior to the
experiment the disk of Pt/HMFI was heated under H2 flow
(20 cm3 min−1) at 400 °C for 0.5 h, followed by cooling to
40 °C and purging with He. Then, the catalyst was exposed to
a flow of CO (5%)/He (20 cm3 min−1) for 180 s, followed by
purging with He for 600 s. For the IR measurements of pyri-
dine and γVL on metal oxides at 150 °C, the liquid compound
was injected into He flow preheated at 200 °C and was fed to
the IR cell. Then, the IR disk was purged with He for 200 s,
and IR measurement was carried out.
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Catalytic tests
Commercially available organic compounds (from Tokyo
Chemical Industry) were used without further purification.
Typically, Pt/HMFI (0.5 mol% with respect to levulinic acid)
pre-reduced at 400 °C was used as a standard catalyst. After
the pre-reduction, the catalyst in the closed glass tube sealed
with a septum inlet was cooled to room temperature under a
H2 atmosphere. The mixture of levulinic acid (1 mmol, 116.1 mg,
0.102 cm3) and n-dodecane (0.5 mmol, 85.2 mg, 0.114 cm3) as
an internal standard was injected to the pre-reduced catalyst
inside the glass tube through the septum inlet. Then, the
septum was removed under air, and a magnetic stirrer was
put in the tube, followed by inserting the tube inside a stain-
less autoclave with a dead space of 33 cm3. Immediately after
sealing, the reactor was flushed with H2 from a high pressure
gas cylinder and charged with 2 or 8 bar H2 at room tempera-
ture. Then, the reactor was heated at 200 °C under stirring
(400 rpm). Conversion and yields of products were deter-
mined using a GC (Shimadzu GC-14B, N2 as the carrier gas)
equipped with Ultra ALLOY capillary column UA+-5 (Frontier
Laboratories Ltd.) using n-dodecane as an internal standard.
The products were identified using a GC-MS (Shimadzu
GCMS-QP2010, He as the carrier gas) equipped with the same
column as the GC and were compared with commercially pure
products. For the data in Table 4, we carried out three
catalytic tests to show averaged GC yields. For further data,
yield for a single reaction is shown.
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Acknowledgements
This work was supported by a grant-in-aid for Scientific
Research on Innovative Areas “Nano Informatics” (25106010)
from JSPS and a MEXT program “Elements Strategy Initiative
to Form Core Research Center”.
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