Formulação e caracterização de matérias-primas para revestimento cerâmico Semi-Poroso com adição de chamote de telhas

The ceramics industry in Piauí is nowadays with 55 industries where 11 are in Teresina which is the mainstream of the state, producing 55 million shingles; in which 10 % is of this production is wasted being sometimes thrown on the margins of rivers, roads and highways provoking an environmental degradation. The main goal of this work is to verify the potential of producing semi porous ceramic using grog of shingles, on the first part of this work bodies-of-proof were produced from a basic formula of an industry, doping it with 5 %, 10 %, 15 % and 20 % in mass and in the second part of this work some bodies-of-proof were produced from a formula where one raw material was substituted by 50 % of grog and another substituting it all by grog, bodies-of-proof made of a basic formula previously announced was used for experiment control.The grog and the raw materials were characterized by: particle size analysis , thermal differential analysis, X ray diffraction , X ray fluorescence, an thermal gravimetric analysis and rational analyses. The bodies-of-proof were sintetisized in an industrial oven obeying the normal cycle adopted by an industry, with peak temperatures of 1135 oC and a fast burning cycle of 25 minutes having as energetic fuel liquefied petroleum gas . The pieces that were obtained by this were submersed in rehearsed physics of: water absorption of, apparent specific mass, apparent porosity, lineal retraction, rupture tension to the flexural and dilatometry; mineralogical analysis for X ray diffraction; and microstructural for electronic microscope of sweeping. For all the formulas with addition of grog, superior priorities to the requested by the requirements for semi porous and for the formula to F2-2,5 superior priorities to standard formulas which justifies the incorporation of the shingles in mass for the semi porous ceramic

Obtenção e caracterização de nanopartículas de argilominerais

Natural nanoclays are of great interest particularly for the production of polymer-based nanocomposites. In this work, kaolinite clays from two natural deposits in the State of the Rio Grande do Norte and Paraiba were purified with thermal treatment and chemical treatments, and characterized. Front to the gotten data, had been proposals methodologies for elimination or reduction of coarse particle texts, oxide of iron and organic substance. These methodologies had consisted of the combination of operations with thermal treatments, carried through in electric oven, and acid chemical attacks with and hydrogen peroxide. The Analyzers Thermogravimetric was used to examine the thermal stability of the nanoclays. The analysis indicated weight losses at temperatures under 110 ºC and over the temperature range of 350 to 550 ºC. Based on the thermal analysis data, the samples were submitted to a thermal treatment at 500 °C, for 8 h, to remove organic components. The X-ray diffraction patterns indicated that thermal treatment under 500 °C affect the basic structure of kaolinite. The BET surface area measurements ranged from 32 to 38 m2/g for clay samples with thermal treatment and from 36 to 53 m2/g for chemically treated samples. Thus, although the thermal treatment increased the surface area, through the removal of organic components, the effect was not significant and chemical treatment is more efficient, not affect the basic structure of kaolinite, to improve particle dispersion. SEM analysis confirms that the clay is agglomerated forming micron-size particles

Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

Sinterização de Ce1-XEuXO2-(X/2) para aplicação como eletrólito sólido em células a combustível de temperaturas intermediárias

Given the environmental concern over global warming that occurs mainly by emission of CO2 from the combustion of petroleum, coal and natural gas research focused on alternative and clean energy generation has been intensified. Among these, the highlight the solid oxide fuel cell intermediate temperature (IT-SOFC). For application as electrolyte of the devices doped based CeO2 with rare earth ions (TR+ 3) have been quite promising because they have good ionic conductivity and operate at relatively low temperatures (500-800 ° C). In this work, studied the Ce1-xEuxO2-δ (x = 0,1, 0,2 and 0,3), solid solutions synthesized by the polymeric precursor method to be used as solid electrolyte. It was also studied the processing steps of these powders (milling, compaction and two step sintering) in order to obtain dense sintered pellets with reduced grain size and homogeneous microstructure. For this, the powders were characterized by thermal analysis, X-ray diffraction, particle size distribution and scanning electrons microscopy, since the sintered samples were characterized by dilatometry, scanning electrons microscopy, density and grain size measurements. By x-ray diffraction, it was verified the formation of the solid solution for all compositions. Crystallites in the nanometric scale were found for both sintering routes but the two step sintering presented significant reduction in the average grain size

Caracterização de atapulgita visando aplicação para reforço de materiais poloméricos

The clay mineral attapulgite is a group of hormitas, which has its structures formed by microchannels, which give superior technological properties classified the industrial clays, clays of this group has a very versatile range of applications, ranging from the drilling fluid for wells oil has applications in the pharmaceutical industry. Such properties can be improved by activating acid and / or thermal activation. The attapulgite when activated can improve by up to 5-8 times some of its properties. The clay was characterized by X-ray diffraction, fluorescence, thermogravimetric analysis, differential thermal analysis, scanning electron microscopy and transmission electron microscopy before and after chemical activation. It can be seen through the results the efficiency of chemical treatment, which modified the clay without damaging its structure, as well as production of polymer matrix composites with particles dispersed atapugita

Síntese e caracterização de catalisadores nanométricos de LaSrNiO4 para aplicação em dessulfurização de tiofeno

The mixed metal oxides constitute an important class of catalytic materials widely investigated in different fields of applications. Studies of rare earth nickelates have been carried by several researchers in order to investigate the structural stability afforded by oxide formed and the existence of catalytic properties at room temperature. So, this study aims synthesize the nanosized catalyst of nickelate of lanthanum doped with strontium (La(1-x)SrxNiO4-d; x = 0,2 and 0,3), through the Pechini method and your characterization for subsequent application in the desulfurization of thiophene reaction. The precursor solutions were calcined at 300ºC/2h for pyrolysis of polyester and later calcinations occurred at temperatures of 500 - 1000°C. The resulting powders were characterized by thermogravimetric analysis (TG / DTG), surface area for adsorption of N2 by BET method, X-ray diffraction (XRD), scanning electron microscopy (HR_SEM) and spectrometry dispersive energy (EDS). The results of XRD had show that the perovskites obtained consist of two phases (LSN and NiO) and from 700ºC have crystalline structure. The results of SEM evidenced the obtainment of nanometric powders. The results of BET show that the powders have surface area within the range used in catalysis (5-50m2/g). The characterization of active sites was performed by reaction of desulfurization of thiophene at room temperature and 200ºC, the relation F/W equal to 0,7 mol h-1mcat -1. The products of the reaction were separated by gas chromatography and identified by the selective detection PFPD sulfur. All samples had presented conversion above 95%

Degradação do PMMA através da reação despolimerização uitlizando catalisadores de óxidos mistos

In this work, mixed oxides were synthesized by two methods: polymeric precursor and gel-combustion. The oxides, Niquelate of Lanthanum, Cobaltate of Lanthanum and Cuprate of Lanthanum were synthesized by the polymeric precursor method, and treated at 300 º C for 2 hours, calcined at 800 º C for 6h in air atmosphere. In gel-combustion method were produced and oxides using urea and citric acid as fuel, forming for each fuel the following oxides Ferrate of Lanthanum, Cobaltato of Lanthanum and Ferrato of Cobalt and Lanthanum, which were submitted to the combustion process assisted by microwave power maximum of 10min. The samples were characterized by: thermogravimetric analysis, X-ray diffraction; fisisorção of N2 (BET method) and scanning electron microscopy. The reactions catalytic of depolymerization of poly (methyl methacrylate), were performed in a reactor of silica, with catalytic and heating system equipped with a data acquisition system and the gas chromatograph. For the catalysts synthesized using the polymeric precursor method, the cuprate of lanthanum was best for the depolymerization of the recycled polymer, obtaining 100% conversion in less time 554 (min), and the pure polymer, was the Niquelate of Lanthanum, with 100% conversion in less time 314 (min). By gel-combustion method using urea as fuel which was the best result obtained Ferrate of Lanthanum for the pure polymer with 100% conversion in less time 657 (min), and the recycled polymer was Cobaltate of Lanthanum with 100 % conversion in less time 779 (min). And using citric acid to obtain the best result for the pure polymer, was Ferrate of Lanthanum with 100% conversion in less time 821 (min and) for the recycled polymer, was Ferrate of Lanthanum with 98.28% conversion in less time 635 (min)

Estudo da adição do resíduo proveniente da extração de minério de ferro em argilas do Rio Grande do Norte

The mining industry is responsible for the generation of waste from their natural process of extraction. The mining impacts in urban areas are of special importance due to the high urban occupation, which are exacerbated due to the proximity of the mined areas and populated areas. Some solutions to wastedisposal have the potential to significantly reduce the environmental risks and liabilities, but represent higher costs in the stages of deployment and operation. The addition of mining waste as raw material in the development of commercial products reduces the environmental impacts, transforming the waste into a positive element in the generation of employment and income. This thesis studies the incorporation of waste iron ore in two clays, one from the ceramic industry of the City of Natal and the other from the ceramic industry of the Seridó Region, both in the State of Rio Grande do Norte, Brazil. Percentages of iron ore waste of 5%, 10% , 15%, 20%, 25% and 30% were used in the tested ceramic matrix. The two clays and the iron ore waste used as part of this investigation were characterized by X-ray diffraction tests, X-ray fluorescence tests, differential thermal analysis, thermogravimetric analysis and dilatometric analysis. The samples were sintered under temperatures of 850 °C, 950 °C and 1050°C at a heating rate of 5 °C/min with isotherms of two hours. The following tests were performed with the samples: linear shrinkage, water absorption, apparent porosity, apparent density, mass loss in fire and bending resistance in order to obtain their physical and mechanical properties. An amount of 5% of waste iron ore in the matrix clay at a temperature of 850 0C resulted in na increase of about 65% in the tensile strength of the clay samples from the Natal ceramic industry. A linear shrinkage of only 0.12% was observed for the samples, which indicates that the physical properties of the final product were not influenced by the addition of the waste

O efeito do tratamento da atapulgita no desenvolvimento de compósito com o polietileno reciclado

The study aimed at the treatment of attapulgite for the development and characterization of composite recycled low density polyethylene - PEBD_rec embedded with natural attapulgite - ATP_NAT, sifted - ATP_PN and attapulgite treated with sulfuric acid - ATP_TR in different compositions (1, 3 and 5%) and compared with the PEBD_rec. The atapulgitas, natural, screened and treated, were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size analysis, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and determining the area specific surface (BET). The composites were characterized by thermogravimetry (TG), differential scanning calorimetry (DSC), Xray diffraction (XRD), torque rheometry, scanning electron microscopy (SEM) and traction. The composite PEBD_rec / ATP (natural, sieved and treated) were produced by mixing in the molten state in a single screw extruder matrix wire with subsequent reprocessing matrix tape. It was found that the screening of attapulgite not reduce the quantity of quartz and the acid treatment completely extracted dolomite aggregate impurities of the channels attapulgite, and increase their surface area. The addition of attapulgite in PEBD_rec acts as a catalyst, reducing the thermal stability of the polymer. The increased concentration of attapulgite, increases resistance and reduces the elongation at break and modulus of elasticity of the composite PEBD_rec / attapulgite

Obtenção de uma porcelana dielétrica a partir de matérias-primas do Rio Grande do Norte

The dielectric porcelain is usually obtained by mixing various raw materials proportions and is used in the production of electronic equipment for various applications, from capacitors of high and low Power to insulators for low, medium, high and extra high voltage, which are used in distribution lines and transmission of electricity.This work was directed to the s tudy of technological properties of technic porcelain, made from raw materials extracted from pegmatites found in the regions of Seridó and the Alto Oeste of Rio Grande do Norte, which are made of kaolin, quartz and feldspar, abundant and high quality in these regions. The technic ceramics were obtained by mixing in appropriate levels, kaolin, feldspar, quartz and clay, the last item from a pottery in the city of Sao Gonçalo do Amarante, Rio Grande do Norte. During the development the following characterizations correlated to raw materials were made: laser particle sizing, x-ray diffraction, DTA and TG. The compositions studied were formed by uniaxial pressing at a pressure of 50 MPa and sintered at temperatures ranging from 1150 to 1350ºC and levels (times) of sintering between 30, 60, 90 and 120 minutes. The characterization of the samples were taken from the analysis of weight loss, linear shrinkage, porosity, stoneware curve, bulk density, flexural strength of three points, SEM and X-ray diffraction, TMA, Dielectric and cross Resistivity. The studied materials can be employed in producing the objects used in electrical engineering such as: insulators for low, medium and high-voltage electrical systems, command devices, bushing insulation for transformers, power capacitors, spark plugs, receptacles for fluorescent and incandescent light bulbs and others

Mesoestruturas porosas a partir de materiais naturais

The MCM-41 mesoporous synthesis was done using rice hulls ash and chrysotile as natural alternative silica sources. For the using of these sources, chemical and thermic treatments were done in both materials. After chemical and thermic treatments, these materials were employed on the MCM-41 mesoctructures synthesis. The natural materials treated and employed in the synthesis were characterized by several techniques such as X-ray diffraction, N2 adsorption and desorption, scanning electronic microscopy and thermogravimetric analysis. MCM-41 standart samples synthetized with aerosil 200 commercial sílica were used to evaluation. The formed material from rice hulls ash showed values from BET specific area about 468 m².g-1, N2 adsorption and desorption isotherms and loss mass similar to reference materials. The silica from chrysotile calcined and leached was employed to mesoporous materials synthesis. The BET specific area showed values about 700 m².g-1, N2 adsorption and desorption isotherms type IV and loss mass similar to mesoporous materials. The formed material from calcined and leached chrysotile, without calcination, applied to phenol remotion carried high performance liquid chromatography and evaluated with organophilic clays with different treatments. By the characterization techniques were proved that mesoporous materials with lesser order that reference samples. The material formed from rice hulls ash without the calcination step achieved better adsorption results than organophilic clays

Síntese de catalisadores do tipo LaNixFe1-xO3 como precursores catalíticos para reação oxidação parcial do metano

Nickel-bases catalysts have been used in several reform reactions, such as in the partial oxidation of methane to obtain H2 or syngas (H2 + CO). High levels of conversion are usually obtained using this family of catalysts, however, their deactivation resulting from carbon deposition still remains a challenge. Different approaches have been tested aiming at minimizing this difficulty, including the production of perovskites and related structures using modern synthesis methods capable of producing low cost materials with controlled microstructural characteristics at industrial scale. To establish grounds for comparison, in the present study LaNixFe1-xO3 (x=0, 0.3 or 0.7) perovskites were prepared following the Pechini method and by microwave assisted self-combustion. All samples were sub sequently calcined at 900 °C to obtain the target phase. The resulting ceramic powders were characterized by thermogravimetric analysis, infrared spectroscopy, X ray diffraction, specific area and temperature programmed reduction tests. Calcined samples were also used in the partial oxidation reaction of methane to evaluate the level of conversion, selectivity and carbon deposition. The results showed that the calcined samples were crystalline and the target phase was formed regardless of the synthesis method. According to results obtained by Rietveld refinement, we observed the formation of 70.0% of LaNi0.3Fe0.7O3 and 30.0% of La2O3 for samples LN3F7-900- P, LN3F7-900-M and 41,6% of LaNi0.7Fe0.3O3, 30.7% of La2NiO4 and 27.7% of La2O3 for samples LN7F3-900-P and LN7F3-900-M.Temperature-programmed profiles of the LaNiO3 sample revealed the presence of a peak around 510 °C, whereas the LaFeO3 sample depicted a peak above 1000°C. The highest l evel of methane conversion was obtained for LaNiO3 synthesized by the Pechini method. Overall, catalysts prepared by the Pechini method depicted better conversion levels compared to those produced by microwave assisted self-combustion

Preparação de óxidos mistos de níquel e zinco nanoparticulados a partir de combustíveis alternativos

The field of "Materials Chemistry" has been developing in recent years and there has been a great increase of interest in the synthesis and chemical and physical properties of new inorganic solids. New routes of synthesis and synthesis modified has been developed with the aim not only to optimize the processes in laboratory scale, but also on an industrial scale, and make them acceptable by current environmental legislation. The phenomenology of current solid state chemistry properties coupled with the high temperature superconductivity, ferromagnetism, porosity molecular and colors are evidence affected by the synthesis method, which in turn can influence the technological application of these materials. From this understanding, mixed oxides of nickel and zinc nanoparticulate were synthesized by microwave-assisted combustion route using three specific types of organic fuels employing the weight ratios 1:1/2 and 1:1 of cation metallic/fuel, in order to investigate the influence of such proportions to obtain the solids. The new fuels were chosen to replace, for example, urea or glycine that are the fuels most commonly preferred in this kind of synthesis. The powders without heat treatment were studied by Thermogravimetric analysis (TGA), X-Ray Diffraction (XRD) and then calcined at 900°C. After heat treatment, the samples were characterized by analysis of X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The modified synthesis route porposed was effective for obtaining powders. Both the alternative fuels chosen as the different weight ratios employed, influenced in the morphology and obtaining oxides

Síntese, aplicação e avaliação do efeito do teor de fósforo da celulose fosfatada em argamassa de alvenaria com aditivo comercial a base de hidroxi-etil-metil celulose (HEMC)

Generally, cellulose ethers improves mortar properties such as water retention, workability and setting time, along with adherence to the substrate. However, a major disadvantage of the addition of cellulose ethers in mortars is the delay in hydration of the cement. In this paper a cellulose phosphate (Cp) was synthesized water soluble and has been evaluated the effect of their incorporation into mortar based on Portland cement. Cellulose phosphate obtained was characterized by spectrophotometry Fourier transform infrared (FTIR), X-ray diffraction (XRD), elemental analysis and scanning electron microscopy (SEM). Mortar compositions were formulated with varying phosphorus content in cellulose and cellulose phosphate concentrations, when used in partial or total replacement of the commercial additive based hydroxyethyl methyl cellulose (HEMC). The mortars formulated with additives were prepared and characterized by: testing in the fresh state (consistency index, water retention, bulk density and air content incorporated) and in the hardened state (absorption by capillarity, density, flexural and compression strength). In mixtures the proportion of sand:cement of 1:5 (v / v) and factor a / c = 1.31 and water were held constant. Overall, the results showed that the celluloses phosphates employed in mortars added acted significantly when partially substituting the commercial additive. With regard to consistency index, water retention and bulk density in the fresh state and absorption by capillarity and bulk density apparent in the hardened state, showed no appreciable differences as compared to the commercial additive. The incorporated air content in the fresh state reduced markedly, but did not affect other properties. The mortars with cellulose phosphate, partially replacing the commercial additive showed an improvement of the properties of flexural strength and compressive strength

Caracterização microestrutural e elétrica de La(FexNi1-x)O3 sintetizado pelo método da gelatina

The present work deals with the synthesis of materials with perovskite structure with the intention of using them as cathodes in fuel cells SOFC type. The perovskite type materials were obtained by chemical synthesis method, using gelatin as the substituent of citric acid and ethylene glycol, and polymerizing acting as chelating agent. The materials were characterized by X-ray diffraction, thermal analysis, spectroscopy Fourier transform infrared, scanning electron microscopy with EDS, surface area determination by the BET method and Term Reduction Program, TPR. The compounds were also characterized by electrical conductivity for the purpose of observing the possible application of this material as a cathode for fuel cells, solid oxide SOFC. The method using gelatin and polymerizing chelating agent for the preparation of materials with the perovskite structure allows the synthesis of crystalline materials and homogeneous. The results demonstrate that the route adopted to obtain materials were effective. The distorted perovskite structure have obtained the type orthorhombic and rhombohedral; important for fuel cell cathodes. The presentation material properties required of a candidate cathode materials for fuel cells. XRD analysis contacted by the distortion of the structures of the synthesized materials. The analyzes show that the electrical conductivity obtained materials have the potential to act as a cell to the cathode of solid oxide fuel, allowing to infer an order of values for the electrical conductivities of perovskites where LaFeO3 < LaNiO3 < LaNi0,5Fe0,5O3. It can be concluded that the activity of these perovskites is due to the presence of structural defects generated that depend on the method of synthesis and the subsequent heat treatment