Edgardo L. Sham

Identification and quantification of the interaction mechanisms between the cationic surfactant HDTMA-Br and montmorillonite

Several detailed studies have been done on the characterization of organoclays and the type of structures developed when they interact with alkylammonium molecules. Few published contributions exist, however, on the distribution of surfactant within the organoclays and the mechanism by which they are intercalated. Also, although X-ray photoelectron spectroscopy (XPS) is a suitable technique for the study of the surface characteristics of organoclays, very few such XPS studies have been carried out. With the aim of contributing to a better understanding of the intercalation process, a series of organoclays was synthesized using a montmorillonite and the cationic surfactant hexadecyltrimethylammonium bromide (HDTMABr), with an increasing surfactant load of between 0.2 and 4.0 times the cation exchange capacity of the starting clay. By means of XPS, zeta potential, and thermal analysis techniques, distinguishing the strongly interacting fraction from the weakly interacting fraction of the adsorbed surfactant molecules was possible. Adsorption isotherms of each of these processes were constructed and then adjusted using the Langmuir and Dubinin-Radusquevich adsorption models. Three types of interaction between the surfactant and the clay were identified and described qualitatively and quantitatively. Two of these interactions, strong and weak, involved the hexadecyltrimethylammonium cation (HDTMA+). The third was a weak interaction involving the ion pair HDTMA+Br−. The results of this study may be useful for the comprehensive design of organoclays with specific physicochemical properties according to the application for which they are destined.

Nitrogen dopedTiO2photoactive in visible light

In this research TiO2 modified with nitrogen has been prepared. The synthesis method used was sol gel from the hydrolysis of titanium tetrabutoxide with urea solution, combined with a low temperature treatment at atmospheric pressure. The theoretical mole ratio N/Ti was equal to 0.5 and the theoretical mole ratio HNO3/TiO2 was equal to 0.5. The solid obtained was calcined at different temperatures in static air with high heating rate and residence time of 1 hour. The samples were characterized by X-ray diffraction, FTIR Raman and diffuse reflectance spectroscopy, thermodifferential and thermogravimetric analysis and specific surface area. All calcined solids exhibit absorption in the visible range. The Raman spectroscopy and X-ray diffraction revealed for all the heat treatments, the presence of crystalline phases corresponding to anatase and brookite polymorphism. The photocatalytic activity of the catalysts was tested in degradation of an artificial dye under visible light, yielding the best results for the sample treated at 250°C. Our results allow to say that this behaviour is due to the absorption of visible light, good efficiency for the adsorption of the dye and presence of two crystalline phases that decreases the recombination of photogenerated electrons and holes. The synthesis technique used allows obtaining solids with textural and attractive photocatalytic properties.

Characterization of hexadecyltrimethylammonium-organoclay and its individual components by thermal techniques

The properties of the materials determine their potential applications. The aim of this article is to study the properties of the organoclays using simple and rapid technologies. Organoclays with different surfactant loadings (SL) were synthesized using an Argentine bentonite with a high content of montmorillonite (Bent) and hexadecyltrimethylammonium bromide as cationic surfactant. The samples were characterized using thermal techniques. The results revealed that the hydrophilicity of the organoclays decreases with increasing SL until the SL reaches 0.8 times the cation exchange capacity of the clay; and remains constant at a higher surfactant load. The stability of organoclays was inversely proportional to the SL of each sample. The layers showed a stabilization of approximately 40

V2O5-SiO2 Catalyst Prepared by the sol–gel Process in the Oxidative Dehydrogenation of n-butane

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Sol–gel synthesis of V2O5–SiO2 catalyst in the oxidative dehydrogenation of n-butane

∘C for their structural transformation temperature, caused by the presence of the surfactant. In addition, at a SL <1.0 the surfactant presented a ‘liquid-like’ structure in the interlayer space, whereas at a SL >1.0 the structure was ‘solid-like’.

Adsorption of nisin on raw montmorillonite

TiO2 organoclays are potential adsorbents for aqueous pollutants and subsequently they could favour the photocatalysis of them. For this reason, the study of their surface and textural characteristics is important for the improvement of those processes. In this work TiO2 pillared organoclays were studied. The surfactant (hexadecyltrimethilammonium bromide) was introduced post-pillaring or during the pillaring process. The effect of the use of different acids of hydrolysis and different surfactants ratios was investigated. The clays were characterized by thermogravimetric analysis, infrared spectroscopy and nitrogen sorptometry. It was found that the highest adsorption capacity post-pillaring of the surfactant is near to 0.5 times the CEC of the original pillared clay, independently of the amount of surfactant offered. An increment in the amount of the surfactant introduced only increased the ratio adsorbed as ionic pair. In these samples the CEC measured after the adsorption was between 0.26 and 0.47 times the original CEC. It was observed a decrease in the total pore volume and the BET surface for every sample. The surface hydrophobicity of the samples with post-pillaring adsorption was higher than in those with co-adsorption. In conclusion, it was demonstrated that the incorporation of surfactant modifies the surface and textural properties of the material in different extent in accordance with the incorporation stage and the amount of surfactant used.

OXIDATIVE DEHYDROGENATION OF PROPANE AND n-BUTANE OVER ALUMINA SUPPORTED VANADIUM CATALYSTS

Vanadium silicate gels (V2O5-SiO2) were prepared by the sol–gel method by hydrolysis of vanadium acetilacetonate and silicon alkoxide. The changes in the vanadium species and its interaction with SiO2 network upon heat treatment at various temperatures was studied by means of XRD, XPS and IR. The catalytic behavior for the oxidative dehydrogenation of n-butane was studied. It was found that hydration degree of gel derived catalyst strongly influenced its catalytic activity.