Chemisorption hydrogen, catalyst characterization

The effects of tin/palladium ratio, temperatnre, pressnre, and recycling were studied and correlated with catalyst characterization. The catalysts were characterized by chemisorption titrations, in situ X-Ray Diffraction (XRD), and Electron Spectroscopy for Chemical Analysis (ESCA). Chemisorption studies with hydrogen sulfide show lack of adsorption at higher Sn/Pd ratios. Carbon monoxide chemisorption indicates an increase in adsorption with increasing palladium concentration. One form of palladium is transformed to a new phase at 140°C by measurement of in situ variable temperature XRD. ESCA studies of the catalysts show that the presence of tin concentration increases the surface palladium concentration. ESCA data also indicates that recycled catalysts show no palladium sulfide formation at the surface but palladium cyanide is present. 

Hydrogen chemisorption has frequently been used for catalyst characterization. Considerable detailed information is available for hydrogen... 

A MgO-supported W—Pt catalyst has been prepared from IWsPttCOIotNCPh) (i -C5H5)2l (Fig. 70), reduced under a Hs stream at 400 C, and characterized by IR, EXAFS, TEM and chemisorption of Hs, CO, and O2. Activity in toluene hydrogenation at 1 atm and 60 C was more than an order of magnitude less for the bimetallic cluster-derived catalyst, than for a catalyst prepared from the two monometallic precursors. 

W-Rh IWCRht/oCOMCOljD/VCsHO ,) 193, Si02 Hydrogenation of CO and characterization of catalyst (FTIR. CO chemisorption. TPR. EPR) E)9... 

In conclusion, XPS is among the most frequently used techniques in characterizing catalysts. It readily provides the composition of the surface region and also reveals information on both the oxidation state of metals and the electronegativity of any ligands. XPS can also provide insight into the dispersion of particles over supports, vrhich is particularly useful if the more common techniques employed for this purpose, such as electron microscopy or hydrogen chemisorption, can not discriminate between support and active phase. 

Ir catalysts supported on binary oxides of Ti/Si and Nb/Si were prepared and essayed for the hydrogenation of a,P-unsaturated aldehydes reactions. The results of characterization revealed that monolayers of Ti/Si and Nb/Si allow a high metal distribution with a small size crystallite of Ir. The activity test indicates that the catalytic activity of these solids is dependent on the dispersion obtained and acidity of the solids. For molecules with a ring plane such as furfural and ciimamaldehyde, the adsorption mode can iirfluence the obtained products. SMSI effect (evidenced for H2 chemisorption) favors the formation of unsaturated alcohol. 

Highly mesoporous carbon supported Pd catalysts were prepared using sodium formate and hydrogen for the reduction of the catalyst precursors. These catalysts were tested in the enantioselective hydrogenation of isophorone and of 2-benzylidene-l-benzosuberone. The support and the catalysts were characterized by different methods such as nitrogen adsorption, hydrogen chemisorption, SEM, XPS and TPD. 

In any of the schemes presented, hydrogen dissociative adsorption on Pt is possible after Sn addition, as was checked by hydrogen chemisorption. From these results, it is possible to think of a scheme to represent the main reaction pathway during the hydrogenation of a,(3-unsaturated aldehydes. Depending on the catalyst used, such a scheme is shown in Figure 6.12, which summarizes the results from the characterizations and catalytic tests performed in this work [47]. 

Another part of our investigation deals with the effect of heat treatment on the leaching behavior of palladium on activated carbon catalysts. Heat treatment is a known technique to increase the performance of catalysts. (3) Therefore, standard carbon supported palladium catalysts were exposed to different temperatures ranging from 100 to 400 °C under nitrogen. The catalysts were characterized by metal leaching, hydrogenation activity and CO-chemisorption. 

Narayanan, S. and Krishna, K. (1998). Hydrotalcite-supported palladium catalysts Part I preparation, characterization of hydrotalcites and palladium on uncalcined hydrotalcites for CO chemisorption and phenol hydrogenation. Appl. Catal. A 174, 221. 

The prepared catalysts and the chemical compositions measured by atomic absorption, are listed in Table 1. Complementary characterization experiments such as hydrogen chemisorption in a pulse apparatus and temperature-programmed reduction (TPR) were performed using experimental systems and methods described in detail elsewhere [10]. 

The catalysts were characterized by BET surface area measurement, XRD, in-situ CO2 H2 chemisorption measurements, and Temperature Programmed Reduction (TPR). CO2 hydrogenation was carried out in a fixed bed flow reactor made of stainless steel. Prior to the activity studies, the catalysts were reduced in 99.99 % H2 flow at 723K for 12hrs. After this, the reaction gas (H2/CO2 = 3) was introduced into the reactor at 573K at 10 atm. The gas phase effluents were analyzed by on-line GC. 

The in sim characterization of catalysts was earned out in an apparatus which included a quadiupole mass-spectrometer and a gas chromatograph for TPO and H2 chemisorption measurements. In situ coking was performed by injecting a mixture of He and n-hexane vapor over the reduced catalysts at 500 C, In TPO experiments, ihe coked sample was heated at a rate of 8 C/min in a stream of 2 voL% O2 + 98% He. The amount of CO2 produced was recorded. The chemisorption of H2 was carried out in the same appanitus by a flow method after reduction or caking. The flow rate of carrier gas (Ar) was maintained at 25 ml/min and the volume of H2 injected was 0.062 ml/pulse. Since the partial piessiire of H2 was very low in this system, the hydrogenation of coke was never observed. Isobaric H2 chemisorption measurements with fresh catalysts were carried out in a static adsorption apparatus. Dehydrogenation of n-butane was carried out in a flow micro-rcactor in H2 atmosphere at LHSV = 3 h-l and H2/HC=1. Reaction products were... 

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