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NH4Y and NH4LaY-type zeolite catalysts were prepared by cyclic ion-exchange of a synthetic Linde Y-zeolite. The release of ammonia and water were followed by evolved gas analysis (automatic thermogastitrimetric equipment) as well as with a continuous selective water detector.

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Abstract  

The surface properties of gallium oxide and tin dioxide supported on alumina or titania have been studied by adsorption microcalorimetry. The differential heats of adsorption of various pollutant adsorbates such as sulfur dioxide, nitrogen monoxide, nitrogen dioxide and also ammonia were measured on these catalytic surfaces. NH3, SO2, NO2 are strongly adsorbed while NO is only physisorbed. The supported Ga2O3 samples show a slight decrease in acidity as probed by ammonia adsorption, compared to alumina or titania. The addition of SnO2 decreases the number of strong acid sites but creates a few weak and medium strength acid sites on alumina and does not modify the acidity of titania. In all cases, the basicity, probed by SO2 adsorption, is very strongly affected by the deposition of Ga2O3 or SnO2. The differential heats of NO2 adsorption remain nearly constant on all samples. The heats of adsorption are discussed as a function of the coverage and of the amount of guest oxide.

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Abstract  

In order to explore the influence of CeO2 on the structure and surface characteristics of molybdena, an investigation was undertaken by using N2 adsorption (BET method), thermal analysis and in-situ diffuse reflectance infrared (DRIFT) techniques. In this work, the Mo/CeO2 and Ce-Mo/Al2O3 samples were prepared by impregnation and co-precipitation methods with high Mo loadings. Combining the results one may notice that the presence of ceria led to the increase of polymerized surface Mo species so as to forming Mo-O-Ce linkages besides the formation of coupled O=Mo=O bonds indicative of polymeric MoO3. From thermal analysis, it can be inferred that Mo/Al2O3 is the thermally most stable material in the temperature range used in the experiment (up to 900°C), whereas Ce-Mo/Al2O3 and Mo/CeO2 samples undergo morphological modifications above 700°C resulting in lattice defects, which motivate the mobility of Mo and Ce ions and thus enhance the possibility of interaction between them. Additionally, their activity towards CO adsorption needs reduced ceria and molybdena containing coordinatively unsaturated sites (CUS), oxygen vacancies and hydroxyl groups to form various carbonate species.

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Investigation of RuO2-IrO2-SnO2 thin film evolution

A thermoanalytical and spectroscopic study

Journal of Thermal Analysis and Calorimetry
Authors: Elizabet Horváth, J. Kristóf, L. Vázquez-Gómez, Á. Rédey, and V. Vágvölgyi

Abstract  

The thermal evolution process of RuO2–IrO2–SnO2 mixed oxide thin films of varying noble metal contents has been investigated under in situ conditions by thermogravimetry-mass spectrometry (TG-MS), infrared emission spectroscopy (IR) and cyclic voltammetry (CV). The gel-like films prepared from aqueous solutions of the precursor compounds RuOHCl3, H2IrCl6 and Sn(OH)2(CH3COO)2–xClx on titanium metal support were heated in an atmosphere containing 20% O2 and 80% Ar up to 600C. Chlorine evolution takes place in a single step between 320 and 500C accompanied with the decomposition of the acetate ligand. The decomposition of surface species formed like carbonyls, carboxylates and carbonates occurs in two stages between 200 and 500C. The temperature of chlorine evolution and that of the final film formation increases with the increase of the iridium content in the films. The anodic peak charge shows a maximum value at 18% iridium content.

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Abstract  

The thermal behaviour of halloysite fully expanded with hydrazine-hydrate has been investigated in nitrogen atmosphere under dynamic heating and at a constant, pre-set decomposition rate of 0.15 mg min-1. Under controlled-rate thermal analysis (CRTA) conditions it was possible to resolve the closely overlapping decomposition stages and to distinguish between adsorbed and bonded reagent. Three types of bonded reagent could be identified. The loosely bonded reagent amounting to 0.20 mol hydrazine-hydrate per mol inner surface hydroxyl is connected to the internal and external surfaces of the expanded mineral and is present as a space filler between the sheets of the delaminated mineral. The strongly bonded (intercalated) hydrazine-hydrate is connected to the kaolinite inner surface OH groups by the formation of hydrogen bonds. Based on the thermoanalytical results two different types of bonded reagent could be distinguished in the complex. Type 1 reagent (approx. 0.06 mol hydrazine-hydrate/mol inner surface OH) is liberated between 77 and 103C. Type 2 reagent is lost between 103 and 227C, corresponding to a quantity of 0.36 mol hydrazine/mol inner surface OH. When heating the complex to 77C under CRTA conditions a new reflection appears in the XRD pattern with a d-value of 9.6 , in addition to the 10.2 Ĺ reflection. This new reflection disappears in contact with moist air and the complex re-expands to the original d-value of 10.2 in a few h. The appearance of the 9.6 reflection is interpreted as the expansion of kaolinite with hydrazine alone, while the 10.2 one is due to expansion with hydrazine-hydrate. FTIR (DRIFT) spectroscopic results showed that the treated mineral after intercalation/deintercalation and heat treatment to 300C is slightly more ordered than the original (untreated) clay.

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Reaction Kinetics, Mechanisms and Catalysis
Authors: Viorel Chihaia, Karl Sohlberg, M. Scurtu, C. Hornoiu, M. Caldararu, C. Munteanu, G. Postole, N. I. Ionescu, T. Yuzhakova, and A. Redey

Abstract

The surface dynamics of SnO2/γ-Al2O3 catalysts with different tin dioxide loadings (3 and 20 wt%) prepared by the impregnation method were investigated by using in situ electrical/dielectric measurements. The samples were characterized by BET, inductively coupled plasma atomic emission spectroscopy and X-ray diffraction methods. The propylene oxidation reaction, in the temperature range of 30–400 °C, was used to identify the catalytic activity of SnO2 based catalysts. Results are discussed on the bases of the electrical changes accompanying variation of the active phase content. The conductance/capacitance of supported samples evidenced the reciprocal influence of the support and of the guest oxide.

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