Síntese e caracterização de CuNb2O6 e CuNbC através de reação sólido- sólido e gás- sólido a baixa temperatura

The refractory metal carbides have proven important in the development of engineering materials due to their properties such as high hardness, high melting point, high thermal conductivity and high chemical stability. The niobium carbide presents these characteristics. The compounds of niobium impregnated with copper also have excellent dielectric and magnetic properties, and furthermore, the Cu doping increases the catalytic activity in the oxidation processes of hydrogen. This study aimed to the synthesis of nanostructured materials CuNbC and niobium and copper oxide from precursor tris(oxalate) oxiniobate ammonium hydrate through gas-solid and solid-solid reaction, respectively. Both reactions were carried out at low temperature (1000°C) and short reaction time (2 hours). The niobium carbide was produced with 5 % and 11% of copper, and the niobium oxide with 5% of copper. The materials were characterized by X-Ray Diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), X-Ray Fluorescence Spectroscopy (XRF), infrared spectroscopy (IR), thermogravimetric (TG) and differential thermal analysis (DTA , BET and particle size Laser. From the XRD analysis and Rietveld refinement of CuNbC with S = 1.23, we observed the formation of niobium carbide and metallic copper with cubic structure. For the synthesis of mixed oxide made of niobium and copper, the formation of two distinct phases was observed: CuNb2O6 and Nb2O5, although the latter was present in small amounts

Avaliação cinética e potencial do Nb2O5 obtido a partir de um complexo de nióbio para formação do oleato de metila através da reação de esterificação do ácido oleico

Among the heterogeneous catalysts materials made from niobium show up as an alternative to meet the demand of catalysts for biodiesel production. This study aims to evaluate the potential of a heterogeneous catalyst derived from a complex of niobium in the reaction of methyl esterification of oleic acid. The catalyst was synthesized after calcination at different temperatures of a niobium complex ((NH4)3[NbO(C2O4)3].H2O) generating a niobium oxide nanostructure with a different commercial niobium oxide used to synthesize the complex. The commercial niobium oxide, the complex niobium and niobium catalyst were characterized by thermogravimetry (TG and DTA), surface area analysis (BET), scanning electron microscopy (SEM) and X-ray diffraction (XRD), showing the catalyst has researched morphological and crystallographic indicating a catalytic potential higher than that of commercial niobium oxide characteristics. Factorial with central composite design point, with three factors (calcination temperature, molar ratio of alcohol/oleic acid and mass percentage of catalyst) was performed. Noting that the optimal experimental point was given by the complex calcination temperature of 600°C, a molar ratio alcohol/oleic acid of 3.007/1 and the catalyst mass percentage of 7.998%, with a conversion of 22.44% oleic acid in methyl oleate to 60 min of reaction. We performed a composite linear and quadratic regression to determine an optimal statistical point of the reaction, the temperature of calcination of the complex at 450°C, the molar ratio of alcohol/oleic acid 3.3408/1 and mass percentage of catalyst of 7.6833% . Kinetic modeling to estimate parameters for heterogeneous catalysis it set well the experimental results with a final conversion of 85.01% with 42.38% of catalyst and without catalyst at 240 min reaction was performed. Allowing to evaluate the catalyst catalytic studied has the potential to be used in biodiesel production

Síntese e caracterização de niobiosilicatos para produção de biocombustível

The mesoporous materials has been an special attention, among them was discovered in the 1990´s the mesoporous molecular sieve of SBA-15 type. The good features of the SBA- 15 makes this material very promising in catalysis, however, due to the absence of native active sites, it has low catalytic activity. In this way, different metals and oxides have been included in this molecular sieve as a means of introducing active sites and increase its catalytic activity. Among the oxides that are being researched, there is the niobium oxide, which presents strong acid sites and exists in abundance. Brazil is the largest producer of the mineral. On the other hand, the production of biofuels has been desired, but it requires the development of new catalysts for this purpose. The aim of this work was to develop silicate of niobium by impregnation and by new synthesis method for application in the cracking of moringa oil. The methodology consisted of inserting the niobium oxide either by postsynthesis process using wet impregnation and direct insertion. For direct insert a new method was developed for pH adjustment, being tested different pH, and the pH 2.2 was used different ratios of Si/Nb. The materials were characterized by different techniques such as: XRD, N2 adsorption, SEM, EDS, UV-visible, TG/DTG, DSC, TEM, acidity by thermodesorption of n-butilamine and FTIR. After this part of the catalysts developed by the two methods were tested in the thermocatalytic cracking of moringa oil, being used a simple distillation. All silicates of Niobium obtained showed a highly ordered structure, having high specific areas, good distribution of pore diameters, beyond present a morphology in the form of fibers. In the catalysts after synthesis was observed that the niobium inserted has so as octahedrally and tetrahedrally coordinated, demonstrating that there were also oxides formed on the external surface of SBA-15. The materials obtained in the direct synthesis are only tetrahedrally coordinated. The new synthesis method of pH adjusting by using the buffer solution for it, proved to be very efficient for the production of such materials, because the materials obtained showed characteristics and structures similar to the molecular sieve of SBA-15 type. Among the pH tested the material that presented better characteristics was synthesized at pH 2.2. The application of these materials in catalytic cracking showed a higher formation of organic liquids when compared to thermal cracking, in addition to significantly reducing the acidity and residues formed, demonstrating that the use of silicates of Niobium increases both the conversion and the selectivity of the products.

Síntese e caracterização de CuNb2O6 e CuNbC através de reação sólido- sólido e gás- sólido a baixa temperatura

The refractory metal carbides have proven important in the development of engineering materials due to their properties such as high hardness, high melting point, high thermal conductivity and high chemical stability. The niobium carbide presents these characteristics. The compounds of niobium impregnated with copper also have excellent dielectric and magnetic properties, and furthermore, the Cu doping increases the catalytic activity in the oxidation processes of hydrogen. This study aimed to the synthesis of nanostructured materials CuNbC and niobium and copper oxide from precursor tris(oxalate) oxiniobate ammonium hydrate through gas-solid and solid-solid reaction, respectively. Both reactions were carried out at low temperature (1000°C) and short reaction time (2 hours). The niobium carbide was produced with 5 % and 11% of copper, and the niobium oxide with 5% of copper. The materials were characterized by X-Ray Diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), X-Ray Fluorescence Spectroscopy (XRF), infrared spectroscopy (IR), thermogravimetric (TG) and differential thermal analysis (DTA , BET and particle size Laser. From the XRD analysis and Rietveld refinement of CuNbC with S = 1.23, we observed the formation of niobium carbide and metallic copper with cubic structure. For the synthesis of mixed oxide made of niobium and copper, the formation of two distinct phases was observed: CuNb2O6 and Nb2O5, although the latter was present in small amounts