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61.
Saleh Al-Sayari Albert F. Carley Stuart H. Taylor Graham J. Hutchings 《Topics in Catalysis》2007,44(1-2):123-128
The preparation of Au/ZnO and Au/Fe2O3 catalysts using two coprecipitation methods is investigated to determine the important factors that control the synthesis
of high activity catalysts for the oxidation of carbon monoxide at ambient temperature. In particular, the factors involved
in the preparation of catalysts that are active without the need for a calcination step are evaluated. The two preparation
methods differ in the manner in which the pH is controlled during the precipitation, either constant pH throughout or variable
pH in which the pH is raised from an initial low value to a defined end point. Non-calcined Au/ZnO catalysts prepared using
both methods are very sensitive to pH and ageing time, and catalysts prepared at a maximum pH = 5 with a short ageing time
(ca. 0–3 h) exhibit high activity. Catalysts prepared at higher pH give lower activity. However, all catalysts require a short
operation period during which the oxidation activity increases. In contrast, the calcined catalysts are not particularly sensitive
to the preparation conditions. Non-calcined Au/Fe2O3 catalysts exhibit high activity when prepared at pH ≥ 5. Calcined Au/Fe2O3 prepared using the controlled pH method retain high activity, whereas calcined catalysts prepared using the variable pH method
are inactive. The study shows the immense sensitivity of the catalyst performance to the preparation methods. It is therefore
not surprising that marked differences in the performance of supported Au catalysts for CO oxidation that are apparent in
the extensive literature on this subject, particularly the effect of calcination, can be expected if the preparation parameters
are not carefully controlled and reported. 相似文献
62.
Graham M. Carter John L. Henshall Robert M. Hooper 《Journal of the American Ceramic Society》1988,71(5):270-C
Indentation creep of yttria- and calcia-fully-stabilized single-crystal zirconia has been observed at room temperature. The Knoop hardnesses decreased by 15% and 12% of their conventional short-time values, respectively, for indentation times of 100000 s. 相似文献
63.
Zoran D. Zujovic Marija R. Gizdavic-Nikolaidis Paul A. Kilmartin Hicham Idriss Sanjaya D. Senanayake Graham A. Bowmaker 《Polymer》2006,47(4):1166-1171
The quantitative investigation of the radical scavenging properties of polyaniline (PANI) upon reaction with excess of the stable DPPH radical (a 4:1 ratio of DPPH to aniline units in the polymer) was carried out using 15N and 13C solid state NMR spectroscopy. During the process the polyaniline was oxidised so that the imine content increased from 45 to 65%. The extent of oxidation measured by NMR was confirmed by N1s XPS analysis. However, within a 30 min reaction time, about 85% of the DPPH radicals were scavenged as monitored by the decay in its EPR signal. This is about 20 times greater than the fraction of DPPH required to oxidize PANI from an imine content of 45-65%. An identification of further redox processes is required to explain the high degree of radical scavenging. At the same time, there was no evidence of significant chemical binding or trapping of DPPH in the PANI structure. 相似文献
64.
Xiaobao Li Richard P. K. Wells Peter B. Wells Graham J. Hutchings 《Catalysis Letters》2003,89(3-4):163-167
The premodification of a 5 wt% Pt/-Al2O3 catalyst with cinchonidine (0.01 and 0.2 g g-1
catalyst) is described and discussed. Premodification is carried out by treating the catalyst with a solution of cinchonidine followed by solvent removal. Catalysts premodified in this way give the same ee and initial rate of reaction for the enantioselective hydrogenation of ethyl pyruvate as those using the standard in situ modification procedure. Investigations of different solvents for premodification and reaction (dichloromethane, ethanol) show that it is the solvent used for the reaction that controls the observed enantioselection. Premodified catalysts also display the initial transient behavior typically observed with in situ modified catalysts in which the ee increases with conversion in the early part of the reaction. Premodified catalysts show an enhanced rate of reaction when ethanol is used as the reaction solvent compared with in situ modified catalysts under the same conditions. Premodification using aerobic conditions gives the best results and premodified catalysts can be stored prior to use for up to a week without loss of catalytic performance. 相似文献
65.
D. König W. H. Weber B. D. Poindexter J. R. McBride G. W. Graham K. Otto 《Catalysis Letters》1994,29(3-4):329-338
Ellipsometry is used to follow the growth of a PdO layer on the surface of a thick Pd-film catalyst during methane oxidation at 500°C. The oxide layer that develops under rich conditions (excess CH4) is quite porous and roughens with time. Little CO is formed during this period, but the CO2 formation rate increases until spontaneous oscillations develop, which correlate with changes in the ellipsometric data. These changes indicate that the porous oxide rapidly converts to a metal-rich state, which has decreased catalytic activity, and then slowly reoxidizes. 相似文献
66.
Nianxue Song Zhengqian Xuan Jonathan K. Bartley Stuart H. Taylor David Chadwick Graham J. Hutchings 《Catalysis Letters》2006,106(3-4):127-131
The use of a periodic flow reactor is described for the oxidation of butane to maleic anhydride to compare the catalytic performance
of vanadium phosphate catalysts operating under aerobic and anaerobic conditions. It is found that for the catalyst prepared
via a standard VPO method, operation in the absence of oxygen leads to a very small enhancement in selectivity when butane
concentrations in the range 0.9–2.9% are used. Operation in the absence of oxygen leads to very small differences in conversion
such that the overall yield is enhanced and this effect is maximised for reactor feeds containing 1.5% butane. However, the
enhancement is negligible when the catalyst is operated at high conversion required for commercial operation, indicating that
reactors operating with continuous flow with aerobic conditions are preferred. Similar experiments are conducted for a catalyst
prepared by the VPD method and, in contrast, this catalyst gives lower butane conversion and maleic anhydride selectivity
when operated in the absence of oxygen. 相似文献
67.
Nianxue Song Colin Rhodes David W. Johnson Graham J. Hutchings 《Catalysis Letters》2005,102(3-4):271-279
Temperature programmed reduction (TPR) and oxidation (TPO) are used extensively in catalyst characterisation. In this paper, we examine the use of TPR/TPO cycles for the characterisation of a range of molybdates and single oxides. In particular we observe that the first cycle differs from that of subsequent analyses, even when the maximum temperature is limited to that used in the catalytic reaction. The effect is independent of heating rates and cooling atmospheres and has been demonstrated using different bed configurations. This observation has significance when these oxides are used in periodic flow reactors that involve many cyclical reduction/oxidation. 相似文献
68.
The degradation kinetics of poly(3‐hydroxybutyrate‐co‐3‐hydroxyhexanoate), a member of the Nodax family of polymers, were investigated using transient constant shear rate and dynamic time sweep rheological tests. The rate of chain scission at several times and temperatures was correlated with viscosity data and verified using molecular weight determination of the degraded samples. The experimental results show that the molecular weight and the viscosity of Nodax decrease with time over the range of temperatures that were studied (155–175°C). The degradation kinetics, which exhibited first‐order behavior, were determined as a function of the flow history and thermal history. An apparent activation energy of 189 ± 5 kJ/mol for thermal degradation was found by modeling variations in the rate with temperature using an Arrhenius law model. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 66–74, 2005 相似文献
69.
Well defined AB block copolymers of polystyrene (PS) and poly(dimethyl siloxane) (PDMS) have been prepared with PS molecular weights in the range 8 800 to 43 600 and PDMS molecular weights in the range 2 400 to 48 000. Provided the PS and PDMS molecular weights have a ratio within the range 0.5 to 4.0, these block copolymers stabilize particles of poly(methyl methacrylate) in n-alkanes. The particle size over the range 0.1 to 0.5 μm may be varied by performing dispersion polymerizations of methyl methacrylate as a function of monomer content of the seed stage and as a function of the concentration, molecular weight and composition of the block copolymer. From silicon analyses of the poly(methyl methacrylate) particles, values of the surface area stabilized per PDMS chain were established. The results indicate complete surface coverage of the particles. 相似文献
70.
Dan I. Enache Dean Barker Jennifer K. Edwards Stuart H. Taylor David W. Knight Albert F. Carley Graham J. Hutchings 《Catalysis Today》2007,122(3-4):407-411
The oxidation of benzyl alcohol with molecular oxygen under solvent-free conditions has been investigated using a range of titania-supported Au–Pd alloy catalysts to examine the effect of the Au–Pd ratio on the conversion and selectivity. The catalysts have been compared at high reaction temperature (160 °C) as well as at 100 °C, to determine the effect on selectivity since at lower reaction temperature the range of by-products that are formed are limited. Under these conditions the 2.5 wt.% Au–2.5 wt.% Pd/TiO2 was found to be the most active catalyst, whereas the Au/TiO2 catalyst demonstrated the highest selectivity to benzaldehyde. Toluene, formed via either a hydrogen transfer process or an oxygen transfer process, was observed as a major by-product under these forcing conditions. 相似文献