Obtenção e caracterização físico-química de blendas poliméricas, baseadas em POE e PMMA, dopadas com dióxido de titânio

The study of polymer blends has been an alternative method in the search field of new materials for obtaining materials with improved properties. In this work blends of poly(methyl methacrylate) (PMMA) and poly(ethylene oxide) (PEO) doped with titanium dioxide (TiO2) were studied. The PEO is a polymer semicrystalline structure varying between, 70 and 84% crystallinity, while the PMMA exhibits behavior amorphous in their structure. The use of TiO2 is related to corrosion-resistant of titanium as well as good heat transfer and other characteristics. The study of these polymer blends doped TiO2 gives the properties junction organic (polymer) and inorganic (oxide) which leads to modification of the properties of the resultant material. The blends were doped TiO2 (POE/PMMA/TiO2) in different proportions of the PMMA with the PEO and TiO2 fixed. The ratios were: 90/10/0,1; 85/15/0, 1; 80/20/0,1, 75/25/0,1 and 70/30/0,1. The resulting material was obtained in powder form and being characterized by Fourier Transformed Infrared (FTIR) Spectroscopy, Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Electrochemical Impedance Spectroscopy (EIS). The infrared spectra (IR) for the blends in different ratios showed a band at 1744 cm-1, characteristic of the C=O stretching, which increases in intensity with increasing PMMA composition, while in the spectrum of pure PEO this band is absent. This may suggest that the interaction is occurring between the polymers. In the micrographs of the blends also observed change in their surfaces with variation of the composition of PMMA, contributing to the change of the electrical properties of the material. The EIS data showed that the material exhibited conductivity of the order of 10-6 S.cm-1. The blend in the ratio B2(85/15/0, 1) showed better conductivity, σ = 1.56 x 10-6 S.cm-1. It was observed that the diffusion coefficient for the blends, B5(70/30/0, 1) was the largest, 1.07 x 10-6 m2.s-1. The XRD data showing that, with the variation in the composition of the PMMA blend crystallinity of the material is decreased reaching a minimum B3(80/20/0,1), and then increases again. Thermal analysis suggests that blends made from the material obtained can be applied at room temperature

Obtenção e caracterização do sistema compósito alginato de sódio-dióxido de titânio em formas de pó e de membrana

The alginates are copolymers of 1→4-linked β-D-mannuronic acid (M) and α-Lguluronic acid (G) residues that are arranjed in a block structure along a linear chain. Titanium dioxide, TiO2, is a ceramic material and can exist in three distinct crystallography forms: anatase, brookite and rutile. composites of organic and inorganic materials have better properties than the components alone. Thus, this study aims to synthesize, characterize and analyze the composite NaAlg-TiO2 in the form of powder and film. The synthesis of composite powders was performed using the sol-gel process and obtain the composite film was performed using the slow evaporation process, then the composites were analyzed by infrared spectroscopy, fluorescence x ray, thermal analysis, attenuated total reflection (ATR), x ray diffraction and impedance spectroscopy. The X ray diffraction patterns of composite powders show that with increasing calcination temperature, there were no complete transition of rutile-anatase crystalline phase, since at all temperatures studied (300, 500, 700, 900 and 1100ºC) were observed peaks of anatase phase. Thermal analysis shows that at 400°C caused the decomposition of sodium alginate in sodium carbonate and above 600°C, we observe an exothermic peak related to the decomposition of sodium carbonate and in the presence of titanium dioxide becomes sodium titanate. The XRD results confirm the formation of sodium carbonate at 700ºC and the formation sodium titanate in the temperature range 900-1100ºC. The sodium titanate influenced the electrical properties of the material, because with increasing temperature there was a decrease in conductivity, probably due to the creation of Ti vacancies, since the sodium can induce the reduction of surface Ti4+ ions into Ti3+ species. The infrared spectra of the composites in the form of powder and film showed a small shift in the bands compared to the spectrum of pure alginate, indicating that these shifts, even small ones, have evidence of miscibility between the polymer and ceramic material

Síntese pelo método pechini e caracterização da zircônia dopada com cério e neodímio

In this study five compositions were synthesized zirconia doped with cerium and neodymium ions in the system Ce10-xNdx Zr90O2 with 0,5 ≤ x ≤ 4,0 using the Pechini method. The powders were characterized by thermogravimetric analysis, differential thermal analysis, infrared spectroscopy and X-ray diffraction, with application of Rietveld refinement of the calcination temperatures of 350ºC/3h and 30 minutes at 900ºC/3h. All compositions stabilized with a mixture of cubic and tetragonal phase zirconia. The samples were pressed into bars and sintered at 1500°C/3h and 1500°C/6h, being characterized by Xray diffraction, with application of the Rietveld refinement, density and porosity using Archimedes method, scanning electron microscopy and resistance the three point bending. It has been observed the increase in strength with increasing sintering temperature for the compositions x = 2,0 and x = 4,0. For x = 2,0 the main phase was the cubic with 92,56% with crystallite size of 0,56 μm, density and porosity of 96,82% from 1,36%. For x = 4,0 was a mixture of cubic and tetragonal phase with 21% and 37,98%, respectively. The crystallite size was 54,21 nm and 49,64 nm with a density porosity of 97,45% and 1,32% respectively. In the analysis of the fracture surface was observed a greater amount of grain fracture intragranular type, which contribute to increase the mechanical strength of the ceramic. Increased addition of the neodymium ion in the crystal lattice of the zirconium showed a nearly linear behavior with increasing mechanical strength of the zirconia ceramic. Was obtained a bending resistance of 537 ± 38 MPa for the composition x = 2,0 predominantly attributed to cubic phase with 92,56%

Síntese hidrotérmica e caracterização estrutural de titanatos nanotubulares para aplicação na captura do dióxido de carbono

Nanostructured materials have been spreading successfully over past years due its size and unusual properties, resulting in an exponential growth of research activities devoted to nanoscience and nanotechnology, which has stimulated the search for different methods to control main properties of nanomaterials and make them suitable for applications with high added value. In the late 90 s an alternative and low cost method was proposed from alkaline hydrothermal synthesis of nanotubes. Based on this context, the objective of this work was to prepare different materials based on TiO2 anatase using hydrothermal synthesis method proposed by Kasuga and submit them to an acid wash treatment, in order to check the structural behavior of final samples. They were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), adsorption/desorption of N2, thermal analysis (TG/DTA) and various spectroscopic methods such as absorption spectroscopy in the infrared (FT-IR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). All the information of characterizations confirmed the complete conversion of anatase TiO2 in nanotubes titanates (TTNT). Observing the influence of acid washing treatment in titanates structure, it was concluded that the nanotubes are formed during heat treatment, the sample which was not subjected to this process also achieved a complete phase transformation, as showed in crystallography and morphology results, however the surface area of them practically doubled after the acid washing. By spectroscopy was performed a discussion about chemical composition of these titanates, obtaining relevant results. Finally, it was observed that the products obtained in this work are potential materials for various applications in adsorption, catalysis and photocatalysis, showing great promise in CO2 capture

Preparo e caracterização de membranas de quitosana modificadas com poli (ácido acrílico)

The aim of this study was to generate an asymmetric biocompactible and biodegradable chitosan membrane modified by the contact with a poly(acrylic acid) solution at one of its sides at room temperature and 60◦C. The pure chitosan membrane, as well as the ones treated with poly(acrylic acid) were characterized by infrared spectroscopy (FTIRATR) at angles of 39◦, 45◦ and 60◦ , swelling capacity in water, thermal analysis (TG/DTG), scanning electronic microscopy (SEM) and permeation experiments using metronidazole at 0,1% and 0,2% as a model drug. The results confirmed the presence of ionic interaction between chitosan and poly(acrylic acid) by means of a polyelectrolyte complex (PEC) formation. They also showed that such interactions were more effective at 60◦C since this temperature is above the chitosan glass transition temperature wich makes the diffusion of poly(acrylic acid) easier, and that the two treated membranes were asymmetrics, more thermically stable and less permeable in relation to metronidazole than the pure chitosan membrane

Síntese e caracterização da ferrita de MnZn obtida pelo método dos citratos precursores

It was synthesized MnZn ferrite with general formulae Mn1-xZnxFe2O4 (mol%), 0,3 ≤ x ≤ 0,7 by using the citrate precursor method. The precursors decomposition was studied by thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) of powder calcined at 350ºC/3,5h. X-ray diffraction pattern (XRD) of samples was done from 350 to 1200ºC/2h using various atmospheres. The power calcined at 350ºC/3,5h formed spinel phase. It is necessary atmosphere control to avoid secondary phase such as hematite. From 900 to 1200ºC was obtained 90,66 and 100% of MnZn spinel ferrite phase, respectively. Analysis by dispersive energy scanning (EDS) at 350ºC shows high Mn and Zn dispersion, indicating that the diffusion process was homogeneous. Semi-quantitative analysis by EDS verified that despite the atmosphere control during calcinations at high temperatures (< 800ºC) occurred ZnO evaporation causing stoichiometric deviation. Vibrating sample magnetometer (VSM) measures show soft ferrite material characteristics with Hc from 6,5 x 10-3 to 11,1 x 10-2 T. Saturation magnetization (Ms) and initial permeability (µi) of MnZn spinel phase obtained, respectively, from 14,3 to 83,8 Am2/kg and 14,1 to 62,7 (Am2/kg)T

Síntese, caracterização e estudo fotofísico de complexos de 4,4- diaminoestilbeno-2,2-dissulfonato com íons lantanídeos

This is a work involving fundamental studies of chemistry where the synthesis and structural characterization, as well as a possible future application of these new compounds as luminescent sensors or sunscreen agents, complexes with 4,4 diaminostilbene-2,2-disulfonic (DSD) and trivalent lanthanide ions La3+, Nd3+, Eu3+, Gd3+ and Yb3+, were synthesized in the ratio of 3 mmol: 1 mmol (DSD: lanthanides). The complexes obtained with these ions were present in powder form and were characterized by complexometric titration with EDTA CHN Elemental analysis, molecular absorption spectroscopy in the ultraviolet region, the absorption spectroscopy in the infrared, thermal analysis (TG / DTG), Nuclear Magnetic Resonance - NMR 1H and Luminescence Spectroscopy. The complexometric titration and CHN analysis, confirmed the TG / DTG which suggest that these complexes have the following general chemical formulas: [La2(C14H12S2O6N2)2(H2O)2Cl2].7H2O,[Nd2(C14H12S2O6N2)2(H2O)2Cl2].6H2O,[Eu2(C14 H12S2O6N2)2(H2O)2Cl2].7H2O,[Gd2(C14H12S2O6N2)2(H2O)2Cl2].4H2O e [Yb2(C14H12S2O6N2)2(H2O)2].6H2O. The disappearance of the bands in the infrared spectrum at 2921 cm-1 and 2623 cm-1 and the displacement of the bands in the spectra of the amine complex indicate that the lanthanide ion is coordinated to the oxygen atoms and the sulfonate groups of the nitrogens amines, suggesting the formation of the dimer. The disappearance of the signal and the displacement signal SO3H amines in the 1H NMR spectrum of this complex are also indicative coordination and dimer formation. The Thermogravimetry indicates that the DSD is thermally stable in the range of 40º to 385°C and their complexes with lanthanide ions exhibit weight loss between 4 and 5 stages. The Uv-visible spectra indicated that the DSD and complexes exhibit cis isomers. The analysis of luminescence indicates that the complexes do not exhibit emission in the region of the lanthanides but an intense emission part of the binder. This is related to the triplet states of the ligand, which are in the lowest energy state emitting lanthanide ions, and also the formation of the dimer that suppress the luminescence of ion Eu3+. The formation of dimer was also confirmed by calculating the europium complex structure using the model Hamiltonian PM6 and Sparkle

Desenvolvimento de metodologia capaz de detectar e quantificar misturas de corantes em sucos artificiais em pó

Foi desenvolvido um método para detectar e quantificar misturas de corantes em sucos artificiais em pó fabricados no Brasil, de diferentes marcas e sabores. Foram estudados 6 corantes artificiais: amarelo tartrazina, amarelo crepúsculo, vermelho ponceau 4R, vermelho bordeaux S, vermelho 40 e azul brilhante presentes de forma unitária ou em misturas nos sucos com sabores laranja, tangerina, maracujá, abacaxi, limão e uva. A identificação dos corantes nas amostras foi feita através da comparação com os espectros dos padrões, utilizando-se a análise por infravermelho médio e pelos respectivos valores de absorção máxima nos comprimentos de onda relativos aos padrões e valores de referência na literatura. Também foram estudados os perfis de decomposição térmica por termogravimetria, termogravimetria derivada e calorimetria diferencial exploratória dos corantes e dos sucos em pó, sendo determinados os teores de umidade, de matéria orgânica e de cinzas. O teor de umidade encontrado não ultrapassou 4% para todas as amostras de suco analisadas. Com relação ao teor de matéria orgânica obteve-se para 57% dos sucos analisados um teor médio de 51,3% e para 43% das outras amostras obteve-se uma média de 67,2 %. Os resultados obtidos para o teor de cinzas indicaram que 29% das amostras apresentaram um teor de 26,7% para esse parâmetro enquanto 71% das amostras apresentaram um teor de cinzas de 46,4%. Os resultados obtidos por análise térmica mostraram-se adequados considerando-se que para obter os resultados pelo método tradicional há um investimento maior de tempo, de pessoal envolvido e de material, além da proteção ao meio ambiente. Para a análise por espectroscopia de absorção molecular foi proposta uma equação simplificada para a determinação de cada corante na mistura utilizando-se a lei de Beer. Para validação, empregou-se a espectroscopia de absorção molecular no visível, onde foi investigada a influência dos interferentes (TiO2 e açúcar) presentes nas amostras de sucos, os testes de fotodegradação e a avaliação do efeito do pH. Para quantificação tomou-se como referência 512 amostras sintéticas contendo um e dois corantes (1,5625 a 25,000 mg L-1) para obtenção das curvas analíticas que foram aplicadas à análise dos sucos em pó. Os resultados indicaram que o teor máximo do amarelo crepúsculo foi encontrado nos sucos com os sabores laranja, tangerina e manga que correspondeu a 25,6% da ingestão diária aceitável (para ser ultrapassada corresponderia a ingestão de 4 copos). O teor máximo encontrado para o amarelo tartrazina nos sucos foi para o sabor maracujá que correspondeu a 8,5% da ingestão diária aceitável, (para ser alcançado corresponderia a ingestão de 12 copos). O método proposto foi testado e validado com sucesso para amostras de sucos em pó sendo de simples execução e de rapidez na obtenção dos resultados

Desenvolvimento de catalisadores bifuncionais de óxido de zircônio modificado por óxidos de tungstênio e molibdênio contendo platina para a reação de isomerização de n-parafinas

Bifunctional catalysts based on zircon oxide modified by tungsten (W = 10, 15 and 20 %) and by molybdenum oxide (Mo= 10, 15 e 20 %) containg platinum (Pt = 1%) were prepared by the polymeric precursor method. For comparison, catalysts the tungsten base was also prepared by the impregnation method. After calcinations at 600, 700 and 800 ºC, the catalysts were characterized by X-ray diffraction, fourier-transform infrared spectroscopy, thermogravimetric and differential thermal analysis, nitrogen adsorption and scanning electron microscopy. The profile of metals reduction was determined by temperature programmed reduction. The synthesized catalysts were tested in n-heptane isomerization. X-ray diffractogram of the Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts revealed the presence of tetragonal ZrO2 and platinum metallic phases in all calcined samples. Diffraction peaks due WO3 and ZrO2 monoclinic also were observed in some samples of the Pt/WOx-ZrO2 catalysts. In the Pt/MoOx-ZrO2 catalysts also were observed diffraction peaks due ZrO2 monoclinic and Zr(MoO4)2 oxide. These phases contained on Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts varied in accordance with the W or Mo loading and in accordance with the calcination temperature. The infrared spectra showed absorption bands due O-W-O and W=O bonds in the Pt/WOx-ZrO2 catalysts and due O-Mo-O, Mo=O and Mo-O bonds in the Pt/MoOx-ZrO2 catalysts. Specific surface area for Pt/WOx-ZrO2 catalysts varied from 30-160 m2 g-1 and for the Pt/MoOx-ZrO2 catalysts varied from 10-120 m2 g-1. The metals loading (W or Mo) and the calcination temperature influence directly in the specific surface area of the samples. The reduction profile of Pt/WOx-ZrO2 catalysts showed two peaks at lower temperatures, which are attributed to platinum reduction. The reduction of WOx species was evidenced by two reduction peak at high temperatures. In the case of Pt/MoOx-ZrO2 catalysts, the reduction profile showed three reduction events, which are attributed to reduction of MoOx species deposited on the support and in some samples one of the peak is related to the reduction of Zr(MoO4)2 oxide. Pt/WOx-ZrO2 catalysts were active in the n-heptane isomerization with high selectivity to 3-methyl-hexane, 2,3- dimethyl-pentane, 2-methyl-hexane among other branched hydrocarbons. The Pt/MoOx-ZrO2 catalysts practically didn't present activity for the n-heptane isomerization, generating mainly products originating from the catalytic cracking

Caracterização físico-química da mucilagem de inhame liofilizada

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Characterization of native and oxidized starches of two varieties of Peruvian carrot (Arracacia xanthorrhiza, B.) from two production areas of Paraná state, Brazil

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influence of the Al content on the phase transformations in Cu-Al-Ag alloys

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Synthesis, characterization and thermal behaviour of heavy trivalent lanthanide malonates

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Thermoanalytical study of the complexes of 4-dimetilaminocinnamylidenepiruvate with manganese (II), cobalt (II), nickel (II), cupper (II), zinc (II) and lead (II), in the solid state

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Synthesis, characterization and thermal behaviour of solid state compounds of 2-chlorobenzylidenepyruvate with trivalent aluminium, gallium, indium and scandium metals

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)