Thermal oscillations during the catalytic hydrogenation of nitrobenzene

1989 ◽  
Vol 54 (2) ◽  
pp. 237-242 ◽  
Author(s):  
L. Petrov ◽  
Ch. Vladov ◽  
A. Eliyas ◽  
N. Kirkov ◽  
K. Tenchev ◽  
...  
Author(s):  
R. E. Worsham ◽  
J. E. Mann ◽  
E. G. Richardson

This superconducting microscope, Figure 1, was first operated in May, 1970. The column, which started life as a Siemens Elmiskop I, was modified by removing the objective and intermediate lenses, the specimen chamber, and the complete vacuum system. The large cryostat contains the objective lens and stage. They are attached to the bottom of the 7-liter helium vessel and are surrounded by two vapor-cooled radiation shields.In the initial operational period 5-mm and 2-mm focal length objective lens pole pieces were used giving magnification up to 45000X. Without a stigmator and precision ground pole pieces, a resolution of about 50-100Å was achieved. The boil-off rate of the liquid helium was reduced to 0.2-0.3ℓ/hour after elimination of thermal oscillations in the cryostat. The calculated boil-off was 0.2ℓ/hour. No effect caused by mechanical or electrical instability was found. Both 4.2°K and 1.7-1.9°K operation were routine. Flux pump excitation and control of the lens were quite smooth, simple, and, apparently highly stable. Alignment of the objective lens proved quite awkward, however, with the long-thin epoxy glass posts used for supporting the lens.


2020 ◽  
Author(s):  
hao yin ◽  
Liqing Zheng ◽  
Wei Fang ◽  
Yin-Hung Lai ◽  
Nikolaus Porenta ◽  
...  

<p>Understanding the mechanism of catalytic hydrogenation at the local environment requires chemical and topographic information involving catalytic sites, active hydrogen species and their spatial distribution. Here, tip-enhanced Raman spectroscopy (TERS) was employed to study the catalytic hydrogenation of chloro-nitrobenzenethiol on a well-defined Pd(sub-monolayer)/Au(111) bimetallic catalyst (<i>p</i><sub>H2</sub>=1.5 bar, 298 K), where the surface topography and chemical fingerprint information were simultaneously mapped with nanoscale resolution (≈10 nm). TERS imaging of the surface after catalytic hydrogenation confirms that the reaction occurs beyond the location of Pd sites. The results demonstrate that hydrogen spillover accelerates hydrogenation at the Au sites within 20 nm from the bimetallic Pd/Au boundary. Density functional theory was used to elucidate the thermodynamics of interfacial hydrogen transfer. We demonstrate that TERS as a powerful analytical tool provides a unique approach to spatially investigate the local structure-reactivity relationship in catalysis.</p>


2020 ◽  
Author(s):  
Hao Yin ◽  
Liqing Zheng ◽  
Wei Fang ◽  
Yin-Hung Lai ◽  
Nikolaus Porenta ◽  
...  

<p>Understanding the mechanism of catalytic hydrogenation at the local environment requires chemical and topographic information involving catalytic sites, active hydrogen species and their spatial distribution. Here, tip-enhanced Raman spectroscopy (TERS) was employed to study the catalytic hydrogenation of chloro-nitrobenzenethiol on a well-defined Pd(sub-monolayer)/Au(111) bimetallic catalyst (<i>p</i><sub>H2</sub>=1.5 bar, 298 K), where the surface topography and chemical fingerprint information were simultaneously mapped with nanoscale resolution (≈10 nm). TERS imaging of the surface after catalytic hydrogenation confirms that the reaction occurs beyond the location of Pd sites. The results demonstrate that hydrogen spillover accelerates hydrogenation at the Au sites within 20 nm from the bimetallic Pd/Au boundary. Density functional theory was used to elucidate the thermodynamics of interfacial hydrogen transfer. We demonstrate that TERS as a powerful analytical tool provides a unique approach to spatially investigate the local structure-reactivity relationship in catalysis.</p>


2014 ◽  
Vol 18 (10) ◽  
pp. 1335-1345 ◽  
Author(s):  
Xuecheng Yan ◽  
Han Guo ◽  
Dongjiang Yang ◽  
Shilun Qiu ◽  
Xiangdong Yao

1979 ◽  
Vol 44 (8) ◽  
pp. 2378-2383 ◽  
Author(s):  
Libor Červený ◽  
Radka Junová ◽  
Vlastimil Růžička

Hydrogenation of olefinic substrates in binary and ternary mixtures using 5% Pt on silica gel as the catalyst was studied in normal conditions in the liquid phase with methanol or cyclohexane or in solvent-free systems. The effect of the solvent concentration on the selectivity of hydrogenation of the unsaturated alcohol-olefin binary mixtures was investigated. In ternary systems of unsaturated substrates, the effect of each of the substrates on the selectivity of hydrogenation of the remaining two substances was examined. Another system was found in which a jump change of the hydrogenation selectivity occurred on the vanishing of the fastest reacting substance.


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