Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Influência do uso de combustíveis alternativos na síntese por combustão via microondas para a produção de materiais cerâmicos com estrutura espinélio

The development and study of detectors sensitive to flammable combustible and toxic gases at low cost is a crucial technology challenge to enable marketable versions to the market in general. Solid state sensors are attractive for commercial purposes by the strength and lifetime, because it isn t consumed in the reaction with the gas. In parallel, the use of synthesis techniques more viable for the applicability on an industrial scale are more attractive to produce commercial products. In this context ceramics with spinel structure were obtained by microwave-assisted combustion for application to flammable fuel gas detectors. Additionally, alternatives organic-reducers were employed to study the influence of those in the synthesis process and the differences in performance and properties of the powders obtained. The organic- reducers were characterized by Thermogravimetry (TG) and Derivative Thermogravimetry (DTG). After synthesis, the samples were heat treated and characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), analysis by specific area by BET Method and Scanning Electron Microscopy (SEM). Quantification of phases and structural parameters were carried through Rietveld method. The methodology was effective to obtain Ni-Mn mixed oxides. The fuels influenced in obtaining spinel phase and morphology of the samples, however samples calcined at 950 °C there is just the spinel phase in the material regardless of the organic-reducer. Therefore, differences in performance are expected in technological applications when sample equal in phase but with different morphologies are tested

Síntese do Poli (ácido láctico) por policondensação direta utilizando um planejamento fatorial

The environmental impact caused by the disposal of non-biodegradable polymer packaging on the environment, as well as the high price and scarcity of oil, caused increase of searches in the area of biodegradable polymers from renewable resources were developed. The poly (lactic acid) (PLA) is a promising polymer in the market, with a large availability of raw material for the production of its monomer, as well as good processability. The aimed of this study was synthesis PLA by direct polycondesation of lactic acid, using the tool of experimental design (DOE) (central composite rotatable design (CCRD)) to optimize the conditions of synthesis. The polymer obtained was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), viscosimetric analysis, differential scanning calorimeter (DSC) and size exclusion chromatography (SEC). The results confirmed the formation of a poly (lactic acid) semicrystalline in the syntheses performed. Through the central composite rotatable design was possible to optimize the crystallization temperature (Tc) and crystallinity degree (Xc). The crystallization temperature maximum was found for percentage of catalyst around the central point (0,3 (%W)) and values of time ranging from the central point (6h) to the upper level (+1) (8h). The crystallization temperature maximum was found for the total synthesis time of 4h (-1) and percentage of catalyst 0,1(W%) (-1). The results of size exclusion chromatography (SEC) showed higher molecular weights to 0,3 (W%) percent of catalyst and total time synthesis of 3,2h

Membranas de quitosana micro e macroporosas : preparo, caracterização e estudos de permeabilidade

Two methodologies were proposed to obtain micro and macroporous chitosan membranes, using two different porogenic agents. The methodologies proved to be effective in control the porosity as well as the pore size. Thus, microporous membranes were obtained through the physical blend of chitosan and polyethylene oxide (PEO) on an 80:20 (m/m) ratio, respectively, followed by the partial PEO solubilization in water at 80 ◦C. Macroporous chitosan membranes with asymmetric morphology were obtained using SiO2 as the porogenic agent. In this case, chiotsan-silica ratios used were 1:1, 1:3 and 1:5 (m/m). Membranes characterization were carried out by SEM (scanning electronic microscopy), X-ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR), Thermal analysis (TG, DTG , DSC and DMTA). Permeability studies were performed using two model drugs: sodium sulfamerazine and sulfametoxipyridazine. By transmission FTIR it was possible to confirm the complete removal of SiO2. The SEM images confirmed the porous formation for both micro and macroporous membranes and also determined their respective sizes. By thermal analysis it was possible to show differences related with water sorption capacity as well as thermal stability for both membranes. DTG and DSC allowed evidencing the PEO presence on microporous membranes. The absorbance x time curves obtained on permeability tests for micro and macroporous membranes showed a linear behavior for both drugs in all range of concentration used. It was also observed, through P versus C curves, an increase in permeability of macroporous membranes according to the increase in porosity and also a decrease on P with increase in drug concentration. The influences of the drug molecular structure, as well as test temperatures were also evaluated

Síntese e caracterização de membranas zeolíticas tipo mfi e aplicação em separação de aromáticos

The synthesis of MFI-type zeolite membranes was carried by the process in situ or hydrothermal crystallization. We studied the homogenization time of the room temperature and gel filtration just before the crystallization step performed out in an oven, thus obtaining a more uniform zeolite film. The powder synthesized zeolite (structure type MFI, Silicalite) was characterized by several complementary techniques such as Xray diffraction (XRD), scanning electron microscopy (SEM), thermal analysis, temperature programmed desorption (TPD), Fourier Transform infrared spectroscopy (FTIR) and textural analysis by nitrogen adsorption (specific surface area). For the purpose of evaluating the quality of the layer supported on the ceramic support, N2 permeation tests were carried starting from room temperature to 600 °C, where values were observed values more appropriate permeation from 200 °C. With the data obtained, it was made into a graph of temperature versus permeation function, the curve of surface diffusion was found. For scanning electron microscopy, we observed the formation of homogeneous crystals and the zeolite film showed no fissures or cracks, indicating that the process of synthesis and subsequent treatments not damaged the zeolite layer on the support. Carried permeation studies were found values ranging from 3.64x10-6 to 3.78x10-6, 4.71x10-6 to 5.02x10-6, to pressures 20 and 25 psi, respectively. And the mixture xylenes/N2 values were between 5.39x10-6 to 5.67x10-6 and 8.13x10-6 to 8.36x10-6, also for pressures of 20 and 25 psi. The values found for the separation factor were 15.22 at 400 °C in the first experiment and 1.64 for the second experiment at a temperature of 150 °C. It is concluded that the Silicalite membrane was successfully synthesized and that it is effective in the separation of binary mixtures of xylenes

Confecção e caracterização físico-química de filmes compósitos autossustentáveis NaAlg-TiO2-WO3

A new self-sustainable film was prepared through the sol-gel modified method, previously employed in our research group; sodium alginate was used as the polymer matrix, along with plasticizer glycerol, doped with titanium dioxide (TiO2) and tungsten trioxide (WO3). By varying WO3 concentration (0,8, 1,6, 2,4 and 3,2 μmol) and keeping TiO2 concentration constant (059 mmol), it was possible to study the contribution of these oxides on the obtained films morphological and electrical properties. Self-sustainable films have analyzed by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XDR), Scanning Electron Microscope (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and Electrochemical Impedance Spectroscopy (EIS). By the IR specters, it was possible identify the TiO2, and posteriorly WO3, addition has provided dislocation of alginate characteristics bands to smaller vibrations frequencies indicating an electrostatic interaction between the oxides and the polymer matrix. Diffractograms show predominance of the amorphous phase in the films. SEM, along with EDX, analysis revealed self-sustainable films showed surface with no cracks and relative dispersion of the oxides throughout the polymer matrix. From Impedance analysis, it was observe increasing WO3 concentration to 2,4 μmol provided a reduction of films resistive properties and consequent improvement of conductive properties

Encapsulação de nanopartículas de magnetita em matriz de poli(metacrilato de metilacoácido metacrílico) por processo de polimerização em miniemulsão

Magnetic particles are systems with potential use in drug delivery systems, ferrofluids, and effluent treatment. In many situations, such as in biomedical applications, it is necessary to cover magnetic particles with an organic material, as polymers. In this work, magnetic particles were obtained through covering magnetite particles with poly(methyl methacrylate‐comethacrylic acid) via miniemulsion polymerization process. The resultant materials were characterized X‐ray diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), zeta potential (��) measurements and vibrating sample magnetometry (VSM). XRD results showed magnetite as the predominant cristalline phase in all samples and that cristallites had nanometric dimensions. Thermogravimetric analysis revealed an increase in polymer thermal stability as a result of magnetite encapsulation. TGA results showed also that the encapsulation efficiency was directly related to nanoparticles s hidrofobicity degree. VSM measurements showed that magnetic polymeric particles were superparamagnetic, so that they may be potentially used for magnetic (bio)separation

Síntese de catalisadores nanoporosos na ausência total e parcial de direcionadores orgânicos para pirólise catalítica de óleos pesados e intermediários

The processing of heavy oil produced in Brazil is an emergency action and a strategic plan to obtain self-sufficiency and economic surpluses. Seen in these terms, it is indispensable to invest in research to obtain new catalysts for obtaining light fraction of hydrocarbons from heavy fractions of petroleum. This dissertation for the degree of Doctor of Philosophy reports the materials preparation that combine the high catalytic activity of zeolites with the greater accessibility of the mesoporosity, more particularly the HZSM-5/MCM-41 hybrid, done by synthesis processes with less environmental impact than conventional ones. Innovative methodologies were developed for the synthesis of micro-mesoporous hybrid material by dual templating mechanism and from crystalline zeolitic aluminosilicate in the absence of organic template. The synthesis of hybrid with pore bimodal distribution took place from one-single organic directing agent aimed to eliminate the use of organic templates, acids of any kind or organic solvents like templating agent of crystalline zeolitic aluminosilicate together with temperature-programmed microwave-assisted, making the experimental procedures of preparation most practical and easy, with good reproducibility and low cost. The study about crystalline zeolitic aluminosilicate in the absence of organic template, especially MFI type, is based on use of H2O and Na+ cation playing a structural directing role in place of an organic template. Advanced characterization techniques such as X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Highresolution Transmission Electron Microscopy (HRTEM), Adsorption of N2 and CO2, kinetic studies by Thermogravimetric Analysis (TGA) and Pyrolysis coupled to Gas Chromatography/Mass Spectrometry (Pyrolysis-GC/MS) were employed in order to evaluate the synthesized materials. Achieve the proposed objectives, has made available a set of new methodologies for the synthesis of zeolite and hybrid micro-mesoporous material, these suitable for catalytic pyrolysis of heavy oils aimed at producing light fraction

Tratamento de argila montmorilonítica para a produção de nanocompósitos poliméricos com retardo de propagação de chama

Compared to conventional composites, polymer matrix nanocomposites typically exhibit enhanced properties at a significantly lower filler volume fraction. Studies published in the literature indicate t hat the addition of nanosilicate s can increase the resistance to flame propagation in polymers. In this work, a treatment of montmorillonite (MMT) nano clay and the effect of its ad dition o n flame propagation characteristics of vinyl ester were studied. The resea rch was conducted in two stages. The first stage focused on the purification and activation of the MMT clay collected from a natural deposit to improve compatibility with the polymer matrix . Clay modification with sodium acetate was also studied to improve particle dispersion in the polymer. The second step was focused on the effect of the addition of the treated clay on nanocomposites ’ properties. Nanocomposites with clay con tents of 1, 2, 4 wt. % were processed. T he techniques for the characterization of the clay included X - ray fluorescence (XRF), X - r ay d iffraction (XRD), thermogravimetric a nalysis (TGA), d ifferential scanning c alorimetry (DSC) , s urface area (BET) and Fourier transform infrared spectroscopy (FTIR). For t he characterization of the nanocomposites , the techniques used were thermogravimetric a nalysis (TGA) , differential scanning c alorimetry (DSC), Fourier transform infrared spectroscopy (FTIR) , scanning electron mi croscopy (SEM), transmission electron m icroscopy (TEM), and the determination of tensile strength, modulus of elasticity and resistance to flame propagation. According to the results, the purification and activation treatment with freeze - drying used in thi s work for the montmorillonite clay was efficient to promote compatibility and dispersion in the polymer matrix as evidenced by the characterization of the nanocomposite s . It was also observed that the clay modifica tion using sodium acetate did not produce any significant effect to improve compatibilization of the clay with the polymer. The addition of the treated MMT resulted in a reduction of up to 53% in the polymer flame propagation speed and did not affect the mechanical tensile strength and modulus o f elas ticity of the polymer, indicating compatibility between the clay and polymer. The effectiveness in reducing flame propagation speed peaked for nanocomposites with 2 wt. % clay, indicating that this is the optimum clay concentration for this property. T he clay treatment used in this work enables the production of vinylester matrix nanocomposites with flame - retardancy properties .

Utilização da cinza da casca de arroz em cimentação de poços de petróleo

Pozzolanic materials such as rice husk ash are widely used to substitute part of cement, because they react with calcium hydroxide (CH) producing calcium silicate hydrate (C-S-H), which aggregate better physical, chemical and mechanical properties to the cement slurry. The usage of rice husk biomass ash from agribusiness in addition to or partially replacing cement is a noble purpose and a good way of sustainable development which currently is an obsession around the world. The ashes utilized in this study were characterized by: scanning electron microscopy technique (SEM), Fourier transform infrared spectroscopy (FTIR), Energy-dispersive X-ray spectroscopy (EDX) and BET method. The pozzolanic activity of RHA and WRHA in cement slurries was evaluated by: thermal-gravimetric technique and derivative thermogravimetry (TGA/DTG), X-ray diffraction (XRD) and Compressive Strength. The slurries formulated with additions of 10% and 20% of RHA and WRHA were cured for 28 days at 58 °C. The results of thermal analysis demonstrated that a 20% WRHA addition caused a reduction of approximately 73% of Portlandite (calcium hydroxide – CH) phase related to standard slurry (STD). The XRD scans also demonstrated the reduction of the Portlandite peaks’ intensity for each slurry compared with STD slurry. The RHA and WRHA react chemically with Portlandite producing calcium silicate hydrate (C-S-H), confirming their effect as a pozzolanic agent. The WRHA presented the best results as a pozzolanic material.

Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Influência do uso de combustíveis alternativos na síntese por combustão via microondas para a produção de materiais cerâmicos com estrutura espinélio

The development and study of detectors sensitive to flammable combustible and toxic gases at low cost is a crucial technology challenge to enable marketable versions to the market in general. Solid state sensors are attractive for commercial purposes by the strength and lifetime, because it isn t consumed in the reaction with the gas. In parallel, the use of synthesis techniques more viable for the applicability on an industrial scale are more attractive to produce commercial products. In this context ceramics with spinel structure were obtained by microwave-assisted combustion for application to flammable fuel gas detectors. Additionally, alternatives organic-reducers were employed to study the influence of those in the synthesis process and the differences in performance and properties of the powders obtained. The organic- reducers were characterized by Thermogravimetry (TG) and Derivative Thermogravimetry (DTG). After synthesis, the samples were heat treated and characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), analysis by specific area by BET Method and Scanning Electron Microscopy (SEM). Quantification of phases and structural parameters were carried through Rietveld method. The methodology was effective to obtain Ni-Mn mixed oxides. The fuels influenced in obtaining spinel phase and morphology of the samples, however samples calcined at 950 °C there is just the spinel phase in the material regardless of the organic-reducer. Therefore, differences in performance are expected in technological applications when sample equal in phase but with different morphologies are tested

Síntese do Poli (ácido láctico) por policondensação direta utilizando um planejamento fatorial

The environmental impact caused by the disposal of non-biodegradable polymer packaging on the environment, as well as the high price and scarcity of oil, caused increase of searches in the area of biodegradable polymers from renewable resources were developed. The poly (lactic acid) (PLA) is a promising polymer in the market, with a large availability of raw material for the production of its monomer, as well as good processability. The aimed of this study was synthesis PLA by direct polycondesation of lactic acid, using the tool of experimental design (DOE) (central composite rotatable design (CCRD)) to optimize the conditions of synthesis. The polymer obtained was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), viscosimetric analysis, differential scanning calorimeter (DSC) and size exclusion chromatography (SEC). The results confirmed the formation of a poly (lactic acid) semicrystalline in the syntheses performed. Through the central composite rotatable design was possible to optimize the crystallization temperature (Tc) and crystallinity degree (Xc). The crystallization temperature maximum was found for percentage of catalyst around the central point (0,3 (%W)) and values of time ranging from the central point (6h) to the upper level (+1) (8h). The crystallization temperature maximum was found for the total synthesis time of 4h (-1) and percentage of catalyst 0,1(W%) (-1). The results of size exclusion chromatography (SEC) showed higher molecular weights to 0,3 (W%) percent of catalyst and total time synthesis of 3,2h

Síntese e caracterização de tungstatos de cério e estrôncio para fins catalíticos

The main goal of this work was to produce nanosized ceramic materials of the family of the tungstates (tungstates of cerium and strontium), and test them for their catalytic activity in processes involving the transformation of methane (CH4). The methodology used for the synthesis of the ceramic powders involved the complexation combining EDTA-citrate. The materials characterization was performed using simple and differential thermogravimetry, x-ray diffraction, transmission electron microscopy, and energy dispersive spectroscopy (EDS). The microstructure analysis was performed using the refinement by the Rietveld method, and the crystallite size and distribution of the materials was elucidate by the Scherrer and Williamson-Hall methods. The conditions of the synthesis process for the three envisaged materials (SrWO4, SrWO4 using tungsten oxide concentrate as raw material, and Ce2(WO4)3) were adjusted to obtain a single phase crystalline material. The catalytic tests were carried out in the presence of methane and synthetic air, which is composed of 21% O2 and 79% N2. The analysis of the conversion of the reaction was done with the aid of an fourier transform infrared device (FTIR). The analysis showed that, structurally, the SrWO4 produced using raw materials of high and poor purity (99% and 92%, respectively) are similar. The ideal parameters of calcination, in the tested range, are temperature of 1000 °C and time of calcination 5 hours. For the Ce2(WO4)3, the ideal calcination time and are temperature 15 hours and 1000°C, respectively. The Williamson-Hall method provided two different distributions for the crystallite size of each material, whose values ranged between the nanometer and micrometer scales. According to method of Scherrer, all materials produced were composed of nanometric crystallites. The analyses of transmission electron microscopy confirmed the results obtained from the Williamson- Hall method for the crystallite size. The EDS showed an atomic composition for the metals in the SrWO4 that was different of the theoretical composition. With respect to the catalytic tests, all materials were found to be catalytically active, but the reaction process should be further studied and optimized.

Avaliação da poatencialidade da perlita natural e expandida na adsorção de metais

The contamination by metal ions has been occurring for decades through the introduction of liquid effluent not treated, mainly from industrial activities, rivers and lakes, affecting water quality. For that the effluent can be disposed in water bodies, environmental standards require that they be adequately addressed, so that the concentration of metals does not exceed the limits of standard conditions of release in the receptor. Several methods for wastewater treatment have been reported in the literature, but many of them are high cost and low efficiency. The adsorption process has been used as effective for removal of metal ions. This paper presents studies to evaluate the potential of perlite as an adsorbent for removing metals in model solution. Perlite, in its natural form (NP) and expanded (EP), was characterized by X-ray fluorescence, X-ray diffraction, surface area analysis using nitrogen adsorption (BET method), scanning electron microscopy and Fourier transform infrared spectroscopy. The physical characteristic and chemical composition of the material presented were appropriate for the study of adsorption. Adsorption experiments by the method of finite bath for model solutions of metal ions Cr3+, Cu2+, Mn2+ and Ni2+ were carried out in order to study the effect of pH, mass of the adsorbent and the contact time on removal of ions in solution. The results showed that perlite has good adsorption capacity. The NP has higher adsorption capacity (mg g-1) than the EP. According to the values of the constant of Langmuir qm (mg g-1), the maximum capacity of the monolayer was obtained and in terms of proportion of mass, we found the following order experimental adsorption: Cr3+ (2.194 mg g- 1) > Ni2+ (0.585 mg g-1) > Mn2+ (0.515 mg g-1) > Cu2+ (0.513 mg g-1) and Cr3+ (1.934 mg g-1)> Ni2+ (0.514 mg g-1) > Cu2+ (0.421 mg g-1) > Mn2+ (0.364 mg g-1) on the NP and EP, respectively. The experimental data were best fitted the Langmuir model compared to Freundlich for Cu2+, Mn2+ and Ni2+. However, for the Cr3+, both models fit the experimental data