Síntese e caracterização do líquido iônico tetrafluoroborato de 1-metil-3-(2,6-(S)-dimetiloct-2-eno)-imidazol como eletrólito para produção de hidrogênio via eletrólise da água

Ionic liquids (ILs) are organic compounds liquid at room temperature, good electrical conductors, with the potential to form as a means for electrolyte on electrolysis of water, in which the electrodes would not be subjected to such extreme conditions demanding chemistry [1]. This paper describes the synthesis, characterization and study of the feasibility of ionic liquid ionic liquid 1-methyl-3(2,6-(S)-dimethyloct-2-ene)-imidazole tetrafluoroborate (MDI-BF4) as electrolyte to produce hydrogen through electrolysis of water. The MDI-BF4 synthesized was characterized by thermal methods of analysis (Thermogravimetric Analysis - TG and Differential Scanning Calorimetry - DSC), mid-infrared spectroscopy with Fourier transform by method of attenuated total reflectance (FTIR-ATR), nuclear magnetic resonance spectroscopy of hydrogen (NMR 1H) and cyclic voltammetry (CV). Where thermal methods were used to calculate the yield of the synthesis of MDI-BF4 which was 88.84%, characterized infrared spectroscopy functional groups of the compound and the binding B-F 1053 cm-1; the NMR 1H analyzed and compared with literature data defines the structure of MDI-BF4 and the current density achieved by MDI-BF4 in the voltammogram shows that the LI can conduct electrical current indicating that the MDI-BF4 is a good electrolyte, and that their behavior does not change with the increasing concentration of water

Pirólise rápida catalítica do capim elefante utilizando materiais mesoporosos e óxidos metálicos para deoxigenação em bio-óleo

The fast pyrolysis of lignocellulosic biomass is a thermochemical conversion process for production energy which have been very atratactive due to energetic use of its products: gas (CO, CO2, H2, CH4, etc.), liquid (bio-oil) and charcoal. The bio-oil is the main product of fast pyrolysis, and its final composition and characteristics is intrinsically related to quality of biomass (ash disposal, moisture, content of cellulose, hemicellulose and lignin) and efficiency removal of oxygen compounds that cause undesirable features such as increased viscosity, instability, corrosiveness and low calorific value. The oxygenates are originated in the conventional process of biomass pyrolysis, where the use of solid catalysts allows minimization of these products by improving the bio-oil quality. The present study aims to evaluate the products of catalytic pyrolysis of elephant grass (Pennisetum purpureum Schum) using solid catalysts as tungsten oxides, supported or not in mesoporous materials like MCM-41, derived silica from rice husk ash, aimed to reduce oxygenates produced in pyrolysis. The biomasss treatment by washing with heated water (CEL) or washing with acid solution (CELix) and application of tungsten catalysts on vapors from the pyrolysis process was designed to improve the pyrolysis products quality. Conventional and catalytic pyrolysis of biomass was performed in a micro-pyrolyzer, Py-5200, coupled to GC/MS. The synthesized catalysts were characterized by X ray diffraction, infrared spectroscopy, X ray fluorescence, temperature programmed reduction and thermogravimetric analysis. Kinetic studies applying the Flynn and Wall model were performed in order to evaluate the apparent activation energy of holoceluloce thermal decomposition on samples elephant grass (CE, CEL and CELix). The results show the effectiveness of the treatment process, reducing the ash content, and were also observed decrease in the apparent activation energy of these samples. The catalytic pyrolysis process converted most of the oxygenate componds in aromatics such as benzene, toluene, ethylbenzene, etc

Degradacao termica e catalitica da borra oleosa de Petroleo com materiais nanoestruturados al-mcm-41 e AL-SBA-15

Aiming to reduce and reuse waste oil from oily sludge generated in large volumes by the oil industry, types of nanostructured materials Al-MCM-41 and Al-SBA-15, with ratios of Si / Al = 50, were synthesized , and calcined solids used as catalysts in the degradation of oily sludge thermocatalytic oil from oilfield Canto do Amaro, in the state of Rio Grande do Norte. Samples of nanostructured materials were characterized by thermogravimetric analysis (TG / DTG), X-ray diffraction (XRD), scanning electron microscopy (SEM), absorption spectroscopy in the infrared Fourier transform (FT-IR) and adsorption nitrogen (BET). The characterization showed that the synthesized materials resulted in a catalyst nanostructure, and ordered pore diameter and surface area according to existing literature. The oily sludge sample was characterized by determining the API gravity and sulfur content and SARA analysis (saturates, aromatics, resins and asphaltenes). The results showed a material equivalent to the average oil with API gravity of 26.1, a low sulfur content and considerable amount of resins and asphaltenes, presented above in the literature. The thermal and catalytic degradation of the oily sludge oil was performed from room temperature to 870 ° C in the ratios of heating of 5, 10 and 20 ° C min-1. The curves generated by TG / DTG showed a more accelerated degradation of oily sludge when it introduced the nanostructured materials. These results were confirmed by activation energy calculated by the method of Flynn-Wall, in the presence of catalysts reduced energy, in particular in the range of cracking, showing the process efficiency, mainly for extraction of lightweight materials of composition of oily sludge, such as diesel and gasoline

Avaliação da argila atapulgita para potencial uso como excipiente farmacêutico em formas sólidas

Clays are natural materials that have great potential for use as excipients for solid dosage forms. Palygorskite is a type of clay that has hydrophilic properties as well as a large surface area, which could contribute to the dissolution of drugs. Thus, the present study aims to evaluate the use of palygorskite clay, from Piaui (Northeast region of Brazil), as a pharmaceutical excipient for solid dosage forms, using rifampicin and isoniazid as the model drugs. The former is a poorly soluble drug often associated with isoniazid for tuberculosis treatment. Palygorskite was characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and specific surface area (BET). The rheological and technological properties of palygorskite were determined and compared to those of talc, magnesium stearate and Aersosil 200. Mixtures between drugs and palygorskite were analyzed by differential scanning calorimetry (DSC), thermogravimetric analysis (TG) combined with thermal analysis (DTA) and Fourier Transform Infrared Spectroscopy (FT-IR), where the results were compared with those of the individual compounds. In addition, dissolution studies of solid dispersions and capsules containing the drugs, mixed with either palygorskite or a mixture of talc and magnesium stearate, were performed. The results showed that palygorskite has small particles with a high surface area. Its rheological characteristics were better than those of others commonly used glidants and lubricants. There was no interaction between palygorskite and the drugs (rifampicin and isoniazid). Among the dispersions studied, the mixture with palygorskite (5%) showed the highest drug dissolution when compared to other excipients. The dissolution of the rifampicin capsules containing palygosrkite was faster in higher concentrations. However, these differences were statistically different only in the first minutes of the dissolution experiment. The dissolution profile of isoniazid was also statistically different on the initial part of the experiment. The formulations prepared with isoniazid and palygorskite showed higher drug dissolution, but it was in descending order of concentration. According to these results, the palygorskite clay used in this study has great potential for application as an excipient for solid dosage forms

Enhancement of thermal stability, strength and extensibility of lipid-based polyurethanes with cellulose-based nanofibers

Cellulose was extracted from lignocellulosic fibers and nanocrystalline cellulose (NC) prepared by alkali treatment of the fiber, steam explosion of the mercerized fiber, bleaching of the steam exploded fiber and finally acid treatment by 5% oxalic acid followed again by steam explosion. The average length and diameter of the NC were between 200-250 nm and 4-5 nm, respectively, in a monodisperse distribution. Different concentrations of the NC (0.1, 0.5, 1.0, 1.5, 2.0 and 2.5% by weight) were dispersed non-covalently into a completely bio-based thermoplastic polyurethane (TPU) derived entirely from oleic acid. The physical properties of the TPU nanocomposites were assessed by Fourier Transform Infra-Red spectroscopy (FTIR), Thermo-Gravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), X-Ray Diffraction (XRD), Dynamic Mechanical Analysis (DMA) and Mechanical Properties Analysis. The nanocomposites demonstrated enhanced stress and elongation at break and improved thermal stability compared to the neat TPU. The best results were obtained with 0.5% of NC in the TPU. The elongation at break of this sample was improved from 178% to 269% and its stress at break from 29.3 to 40.5 MPa. In this and all other samples the glass transition temperature, melting temperature and crystallization behavior were essentially unaffected. This finding suggests a potential method of increasing the strength and the elongation at break of typically brittle and weak lipid-based TPUs without alteration of the other physico-chemical properties of the polymer. (C) 2012 Elsevier Ltd. All rights reserved.

Obtenção de cerâmicas à base de tricálcio fosfatos utilizando óxido de magnésio como aditivo

The tricalcium phosphate ceramics has been widely investigated in the last years due its bioresorbable behavior. The limiting factor of the application of these materials as temporary implants is its low strength resistance. The tricalcium phosphate presents an allotropic transformation β→α around 1250 ºC that degrades its resistance. Some studies have been developed in order to densify this material at this temperature range. The objective of this work is to study the influence of the addition of magnesium oxide (MgO) in the sintering of β-TCP. The processing route was uniaxial hot pressing and its objective was to obtain dense samples. The samples were physically characterized through density and porosity measurements. The thermal behavior was studied through dilatometric, thermal differential and thermogravimetric analysis. The mechanical properties were characterized by three point flexure test and Vickers microhardness measurements, analyzed of the microstructure. The addition of magnesium oxide doesn t cause an improvement of the mechanical strength in relation to material without additive.

Obtenção de cerâmicas à base de tricálcio fosfatos utilizando óxido de manganês como aditivo

The calcium phosphate ceramics have been very investigated as material for bone implants. The tricalcium phosphate (β-TCP) had a great potential for application in temporary implants like a resorbable bioceramic. This material presents a limitation in its sintering temperature due to occurrence of the allotropic transformation β → α at temperatures around 1200°C, not allowing the attainment of dense ceramic bodies. This transformation also causes cracks, what diminishes the mechanical strength, limiting its use to applications of low mechanical requests. This work studies the influence of the addition of manganese oxide in the sintering of β-TCP. Two processing routes were investigated. The first was the powder metallurgy conventional process. The test bodies (samples) were pressed and sintering at temperatures of 1200 and 1250°C. The second route was uniaxial hot pressing and its objective was to obtain samples with high relative density. The samples were physically characterized through density and porosity measurements. The thermal behavior was studied through dilatometric, thermal differential and thermogravimetric analysis. The mechanical properties were characterized by three point flexure test and Vickers microhardness measurements. The microstructure was analyzed by scanning electron microscopy. The addition of manganese oxide caused an improvement of the mechanical strength in relation to the material without additive and promoting the stabilization of β-TCP to greater temperatures

Desenvolvimento e caracterização de nanocompósito de resina epóxi com nanopartículas de sílica para revestimento de dutos para transporte de petróleo

The use of polymer based coatings is a promising approach to reduce the corrosion problem in carbon steel pipes used for the transport of oil and gas in the oil industry. However, conventional polymer coatings offer limited properties, which often cannot meet design requirements for this type of application, particularly in regard to use temperature and wear resistance. Polymer nanocomposites are known to exhibit superior properties and, therefore, offer great potential for this type of application. Nevertheless, the degree of enhancement of a particular property is greatly dependent upon the matrix/nanoparticle material system used, the matrix/nanoparticle interfacial bonding and also the state of dispersion of the nanoparticle in the polymer matrix. The objective of the present research is to develop and characterize polymer based nanocomposites to be used as coatings in metallic pipelines for the transportation of oil and natural gas. Epoxy/SiO2 nanocomposites with nanoparticle contents of 2, 4, and 8 wt % were processed using a high-energy mill. Modifications of the SiO2 nanoparticles‟ surfaces with two different silane agents were carried out and their effect on the material properties were investigated. The state of dispersion of the materials processed was studied using Scanning and Transmission Electron Microscopy (SEM and TEM) micrographs. Thermogravimetric analysis (TG) were also conducted to determine the thermal stability of the nanocomposites. In addition, the processed nanocomposites were characterized by dynamic mechanical analysis (DMA) to investigate the effect of nanoparticles content and silane treatment on the viscoelastic properties and on the glass transition temperature. Finally, wear tests of the pin-on-disc type were carried out to determine the effects of the nanoparticles and the silane treatments studied. According to the results, the addition of SiO2 nanoparticles treated with silane increased the thermal stability, the storage modulus and Tg of the epoxy resin and decreased wear rate. This confirms that the interaction between the nanoparticles and the polymer chains plays a critical role on the properties of the nanocomposites

Estudo do aproveitamento de resíduo de gesso como carga para compósito com matriz de resina expansiva de mamona

In the execution of civil engineering works, either by wasting during the coating of wall or demolition of gypsum walls, the generation of the gypsum waste involves serious environmental concerns. These concerns are increased by the high demand of this raw material in the sector and by the difficulties of proper disposal byproduct generated. In the search for alternatives to minimize this problem, many research works are being conducted, giving emphasis in using gypsum waste as fillers in composites materials in order to improve the acoustic, thermal and mechanical performances. Through empirical testing, it was observed that the crystallization water contained in the residue (CaSO4.2H2O) could act like primary agent in the expanding of the polyurethane foam. Considering that polyurethane produced from vegetable oils are biodegradable synthetic polymers and that are admittedly to represent an alternative to petrochemical synthetic polyurethane, this research consist an analysis of the thermal behavior of a composite whose matrix obtained from a resin derived from the expansive castor oil seed, with loads of 4%, 8%, 12% and 16% of gypsum waste replacing to the polyol prepolymer blend. Contributors to this analysis: a characterization of the raw material through analysis of spectroscopy by Fourier transform infrared (FTIR), chemical analysis by X-Ray Fluorescence (XRF) and mineralogical analysis by X Ray Diffraction (XRD), complemented by thermo gravimetric analysis (TGA). In order to evaluate the thermo physical properties and thermal behavior of the composites manufactured in die closed with expansion contained, were also carried tests to determine the percentage of open pore volume using a gas pycnometer, scanning electronic microscopy (SEM), in addition to testing of flammability and the resistance to contact with hot surfaces. Through the analysis of the results, it appears that it is possible to produce a new material, which few changes in their thermo physical properties and thermal performance, promotes significant changes and attractive to the environment

Análise do comportamento mecânico de espumas cerâmicas a base de alumina obtidas pelo método da réplica

Ceramics with porous cellular structure, called ceramic foams, have a potential use in several applications, such as: thermal insulation, catalyst supports, filters, and others. Among these techniques to obtain porous ceramics the replication method is an important process. This method consists of impregnation of a sponge (usually polymer) with ceramic slurry, followed by a heat treatment, which will happen the decomposition of organic material and sintering the ceramic material, resulting in a ceramic structure which is a replica of impregnated sponge. Knowledge of the mechanical properties of these ceramics is important for these materials can be used commercially. Gibson and Ashby developed a mathematical model to describe the mechanical behavior of cellular solids. This model wasn´t for describing the ceramics behavior produced by the replica method, because it doesn´t consider the defects from this type of processing. In this study were researched mechanical behavior of porous alumina ceramics obtained by the replica method and proposed modifications to the model of Gibson and Ashby to accommodate this material. The polymer sponge used in processing was characterized by thermogravimetric analysis and scanning electron microscopy. The materials obtained after sintering were characterized by mechanical strength tests on 4-point bending and compression, density and porosity and by scanning electron microscopy. From these results it was evaluated the mechanical strength behavior compared to Gibson and Ashby model for solid cellular structure and was proposed a correction of this model through a factor related to struts integrity degree, which consider fissures present in the structure of these materials besides defects geometry within the struts

Estudo de formulação de massa para aplicação em placas cerâmicas

The sector of civil construction is strongly related to the red ceramic industry. This sector uses clay as raw material for manufacturing of various products such as ceramic plates. In this study, two types of clay called clay 1 and clay 2 were collected on deposit in Ielmo Marinho city (RN) and then characterized by thermogravimetric analysis (TG/DTG), differential thermal analysis (DTA), X-ray diffraction (XRD), X-ray fluorescence (XRF), rational analysis and particle size distribution and dilatometric analyses. Ceramic plates were manufactured by uniaxial pressing and by extrusion. The plates obtained by pressing were produced from the four formulations called 1, 2, 3 and 4, which presented, respectively, the following proportions by mass: 66.5% clay 1 and 33.5% clay 2, 50% clay 1 and 50% clay 2, 33.5% clay 1 and 66.5% clay 2, 25% clay 1 and 75% clay 2. After firing at 850, 950 and 1050 °C with heating rate of 10 °C/min and soaking time of 30 minutes, the following technological properties were determined: linear firing shrinkage, water absorption, apparent porosity, apparent specific mass and tensile strength (3 points). The formulation containing 25% clay 1 produced plates with most satisfactory results of water absorption and mechanical resistance, because of that it was chosen for manufacturing plates by extrusion. A single firing cycle was established for these plates, which took place as follow: heating rate of 2 °C/min up to 600 ºC with soaking time of 60 minutes, followed by heating using the same rate up to 1050 ºC with soaking time of 30 minutes. After this cycle, the same technological properties investigated in the plates obtained by pressing were determined. The results indicate (according to NRB 13818/1997) that the plates obtained by pressing from the mixture containing 25 wt% clay 1, after firing at 1050 °C, reach the specifications for semi-porous coating (BIIb). On the other hand, the plates obtained by extrusion were classified as semi-stoneware (group AIIa)

Avaliação do comportamento tribológico de compósitos poliéster/fibra de vidro utilizando resíduos de poliéster/fibra de vidro e carbonato de cálcio como carga

The use of composite materials and alternative is being increased every day, as it becomes more widespread awareness that the use of renewable and not harmful to the environment is part of a new environmentally friendly model. Since its waste (primarily fiberglass) can not be easily recycled by the difficulty that still exists in this process, since they have two phases mixed, a polymeric matrix thermoset difficult to recycle because it is infusible and phase of fiber reinforcements. Thermoset matrix composites like Polyester + fiberglass pose a threat due to excessive discharge. Aiming to minimize this problem, aimed to reuse the composite Polyester + fiber glass, through the wastes obtained by the grinding of knifes and balls. These residues were incorporated into the new composite Polyester/Fiberglass for hot compression mold and compared tribological to composites with filler CaCO3, generally used as filler, targeting a partial replacement of CaCO3 by such waste. The composites were characterized by thermal analysis (TGA, DSC and DMA), by the surface integrity (roughness determination, contact angle and surface energy), mechanical properties (hardness) and tribological tests (wear and coefficient of dynamic friction) in order to evaluate the effect of loads and characterize these materials for applications that can take, in the tribological point of view since waste Polyester + fiberglass has great potential for replacement of CaCO3

Estudo da viabilidade técnica do uso das argilas da região do agreste potiguar para produção de peças cerâmicas: caracterização e formulação

In recent decades, ceramic products have become indispensable to the technological development of humanity, occupying important positions in scientific production and consequently in industrial production. One area of the economy that continues to absorb large amounts of the products of this sector is Construction. Among the branches of the ceramic industry, there are the red ceramic industry which is traditionally the basis of that economic sector. Among the reasons for which the red ceramic industry became popular in the country, and specifically in Rio Grande do Norte, is the abundance of this raw material, easily found throughout the national territory. However, it appears that the red ceramic industry has deficiencies in technology and skilled labor, resulting in the production of ceramic goods with low added value. Among the factors that determine the quality of the ceramic products red has the proper formulation of the ceramic mass, the conformation and the firing temperature. Thus, the overall goal of this work is to study the mineralogical and technological properties, two clays from the region of the Wasteland Potiguar industrial ceramist. Therefore, the raw materials were characterized by analysis of Xray diffraction (XRD) analysis, X-ray fluorescence (XRF), particle size analysis (FA), scanning electron microscopy (SEM), optical microscopy (OM ), plasticity index (PI), thermal gravimetric analysis (TGA) and differential thermal analysis (DTA). The technological properties of the material were analyzed by water absorption tests (AA%) porosity (% PA), the linear shrinkage (RT%), apparent density (MEA), loss on ignition (PF%) and flexural strength three points (TRF)

Otimização do tempo e temperatura no processamento da gipsita oriunda dos cristalizadores da produção de sal para obter gesso de uso na construção civil

During the process of the salt production, the first the salt crystals formed are disposed of as industrial waste. This waste is formed basically by gypsum, composed of calcium sulfate dihydrate (CaSO4.2H2O), known as carago cru or malacacheta . After be submitted the process of calcination to produce gypsum (CaSO4.0,5H2O), can be made possible its application in cement industry. This work aims to optimize the time and temperature for the process of calcination of the gypsum (carago) for get beta plaster according to the specifications of the norms of civil construction. The experiments involved the chemical and mineralogical characterization of the gypsum (carago) from the crystallizers, and of the plaster that is produced in the salt industry located in Mossoró, through the following techniques: x-ray diffraction (XRD), x-ray fluorescence (FRX), thermogravimetric analysis (TG/DTG) and scanning electron microscopy (SEM) with EDS. For optimization of time and temperature of the process of calcination was used the planning three factorial with levels with response surfaces of compressive mechanical tests and setting time, according norms NBR-13207: Plasters for civil construction and x-ray diffraction of plasters (carago) beta obtained in calcination. The STATISTICA software 7.0 was used for the calculations to relate the experimental data for a statistical model. The process for optimization of calcination of gypsum (carago) occurred in the temperature range from 120° C to 160° C and the time in the range of 90 to 210 minutes in the oven at atmospheric pressure, it was found that with the increase of values of temperature of 160° C and time calcination of 210 minutes to get the results of tests of resistance to compression with values above 10 MPa which conform to the standard required (> 8.40) and that the X-ray diffractograms the predominance of the phase of hemidrato beta, getting a beta plaster of good quality and which is in accordance with the norms in force, giving a by-product of the salt industry employability in civil construction

Dependence of the electrical conductivity and elastomeric properties on sample preparation of blends of polyaniline and natural rubber

Blend films (free-standing) containing 20% in volume of polyaniline (PANI) in 80% of natural rubber (NR) were fabricated by casting in three different ways: (1) adding PANI-EB (emeraldine base) dissolved in N-methyl-2-pyrrolidone (NMP) to the latex (NRL), (2) adding PANI-EB dissolved in in-cresol to NR dissolved in xylol (NRD), (3) overlaying the surface of a pure NR cast film with a PANI layer grown by in situ polymerization (NRO). All the films were immersed into HCl solution to achieve the primary doping (protonation) of PANI before the characterization. The main goal here was to investigate the elastomeric and electrical conductivity properties for each blend, which may be applied as pressure and deformation sensors in the future. The characterization was carried out by optical microscopy, dc conductivity, vibrational spectroscopy (infrared absorption and Raman scattering), thermogravimetry analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMTA), and tensile stress-strain curves. The results suggest that the NRL blend is the most suitable in terms of mechanical and electrical properties required for applications in pressure and deformation sensors: a gain of conductivity without losing the elastomeric property of the rubber. (c) 2005 Wiley Periodicals, Inc.