ACS Catalysis
. EXPERIMENTAL SECTION
.1. Preparation of Catalysts. We employed the NMIR
Research Article
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ACKNOWLEDGMENTS
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4
This work was supported by the State Key Project of
Fundamental Research for Nanoscience and Nanotechnology
(2011CB932401 and 2011CBA00500), the National Natural
Science Foundation of China (Grants Nos. 20921001 and
strategy in the synthesis of various Rh Ni BNPs. Take the
x
y
synthesis of Rh Ni for example. An aqueous solution of
3
1
RhCl ·3H O (2.25 mL, 0.05 mmol/mL) and nickel(II)
3
2
acetylacetonate (9.6 mg) was mixed with a solution containing
g of ODA, and the resulting mixture was slowly heated to 120
C to form a transparent solution, then injected into 8 g of
ODA at 250 °C with vigorous stirring and aged at 230 °C for
.5 min. Finally, the resulting precipitate was washed several
times with ethanol and dried. The as-obtained Rh Ni BNPs
2
1131004), and China Postdoctoral Science Foundation
2
°
(
2011M500293). W. He gratefully acknowledges financial
support from the Tsinghua−Peking Joint Center for Life
Science and the National Key Basic Research Program of China
1
(
2012CB224802).
3
1
was dispersed in n-hexane for future use. By adjusting the
REFERENCES
amount of metal precursors, other Rh Ni BNPs and Rh NPs
■
x
y
were prepared by the similar procedure mentioned above (for
more details, see Table S1, Supporting Information).
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4
.2. Analysis. TEM observation was performed on a
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010F, JEOL) operated at 200 kV. TEM specimens were
2
prepared via the following procedure: the samples were
dispersed in cyclohexane with the aid of 10 min of ultrasonic
vibration. Then a drop of the solution was transferred onto a
standard holey carbon-covered-copper TEM microgrid. Powder
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2
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(
λ = 1.5406 Å). Energy dispersive spectroscopy (EDS) was
recorded to determine the composition of the obtained
products. The content of NPs was determined by inductively
coupled plasma mass spectrometry (ICP-MS). H NMR was
(
1
(
(
conducted on a JEOL JNM-ECX400 400 MHz instrument. GC
chromatography was performed on a SP-6890 with a FID
detector equipped with a capillary column (SE-54, 30 m × 0.50
μm × 0.53 mm). Parameters were as follows: initial oven
temperature, 60 °C, 3 min; ramp, 15 °C/min; final temper-
ature, 260 °C; final time, 10 min; injector temperature, 260 °C;
detector temperature, 250 °C; injection volume, 1 μL.
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9
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4.3. Typical Procedure for the Hydrogenation of
Nitroarenes. To a solution of substrate (0.5 mmol) in 3 mL of
solvent in a 25 mL round flask, catalyst (containing 0.3 mol %
metal with respect to the substrate) was added, and the reaction
mixture was degassed two times, each time replacing the
vacuum with hydrogen, then stirred at room temperature under
(
(
(
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(
H . When the reaction was over, the catalyst was recovered by
2
centrifugation. The supernatant obtained was analyzed by GC
(
(
and purified by silica gel chromatography using an appropriate
́
1
eluent for H NMR test.
(
́ ́
, P.; Corma, A.; Gonzalez, S.; Illas, F.;
ASSOCIATED CONTENT
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(
(
*
S
Supporting Information
Preparation and characterization of Rh NPs and Rh Ni (x, y =
Phys. Chem. B 1999, 103, 9673.
x
y
1
, 2, 3) BNPs, reaction mechanism studies, and the spectral
(27) Dehm, N. A.; Zhang, X.; Buriak, J. M. Inorg. Chem. 2010, 49,
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Vankelecom, I. F. J.; De Vos, D. E. Appl. Catal., A 2009, 355, 176.
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AUTHOR INFORMATION
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*
Corresponding Author
(
31) Song, S.; Liu, R.; Zhang, Y.; Feng, J.; Liu, D.; Xing, Y.; Zhao, F.;
Zhang, H. Chem.Eur. J. 2010, 16, 6251.
32) Liu, X.; Li, Y.; Lee, J. W.; Hong, C.-Y.; Mou, C.-Y.; Jang, B. W.
L. Appl. Catal., A 2012, 439−440, 8.
33) Wu, Y.; Cai, S.; Wang, D.; He, W.; Li, Y. J. Am. Chem. Soc. 2012,
134, 8975.
(
Notes
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The authors declare no competing financial interest.
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dx.doi.org/10.1021/cs300689w | ACS Catal. 2013, 3, 608−612