Estudo do perfil térmico de fornos do tipo "caipira" utilizados pelo setor de cerâmica vermelha em parelhas na região Seridó-RN

The present study aimed to characterize the thermal profile of wood fired oven used by the red ceramic industry in Parelhas, in the Seridó region/RN, aiming to propose structural interventions that can contribute to increasing productivity and product quality, optimize wood consumption and mitigate existing losses during the burning process. The study was conducted at Cerâmica Esperança in the city of Parelhas -RN, Brazil, during the period from August 2012 to September 2013. Four treatments were performed with three replicates, ie, with, a total of 12 experimental units (burnings). In the first stage 4 treatments were performed with three replicates, totaling 12 experimental units (firings). In the second stage 2 treatments were performed with three replications, totaling 6 experimental units (firings). The physical characteristics of the wood were analyzed using standard NBR 11941 and NBR 7190 for basic density and moisture, respectively. The clay was used as a reference parameter for distinguishing treatments. For both the analysis and characterization was carried out using techniques of fluorescence X (XRF) rays, X-ray diffraction (XRD) analysis, particle size analysis (FA). In the first and second stages were monitored: the time during the firing process, the amount of wood used at each firing, the number of parts enfornadas for subsequent determination of the percentages of losses, but also product quality. To characterize the thermal profile of the oven, we measured the temperature at 15 points scored in the surface charge put into the oven. Measurements were taken every 30 minutes from preheat until the end of burning, using a pyrometer laser sight sighting from preheating until the end of burning. In the second step 12 metal cylinders distributed on the oven walls, and the cylinder end walls 8 of the furnace 2 and rollers on each side walls are installed equidistant to 17 cm from the soil and the surface 30 of the wall are installed. The cylinders distributed on the front were placed 50 cm above the furnace, and the base of the oven 20 cm distant from the ground. 10 also thermocouples were installed, and five thermocouples distributed 1.77 cm above the combustion chambers, and one thermocouple on each side, and three thermocouples in front of the oven. We carried out the measurements of the temperatures every 1 hour during the burning two hours in cooling the cylinders with a pyrometer and thermocouples for dattaloger. These were fixed with depth of 30 cm from the wall. After statistical analysis it was found that: the thermal profile of the furnace surface and at different heights was heterogeneous; and the ranges of density and moisture content of wood are within recommended for use as an energy source standards. We conclude that even at low temperatures reached during firing there was a significant production of good quality products, this is due to high concentrations of iron oxide and potassium oxide found in clay, which lowers the melting point of the piece. The average burn time for each step varied 650-2100 minutes wood consumption was on average 20 m3, product quality was on average 16% of first quality, 70% second, third and 5% to 10% loss . The distance between the wire and the surface of the oven was a significant parameter for all treatments, but with different variations, meaning that the wire should not be so generic and unique form, used as a criterion for completion of the burn process. The central part of the furnace was the area that reached higher temperature, and in a unified manner, with the highest concentration of top quality products. The ideal temperature curve, which provided the highest quality of ceramic products was achieved in the central part of the furnace

Avaliação do comportamento termoanalítico e oxidativo do biodiesel de mamona

In this work biodiesel was gotten through the transesterification reaction using the oil of castor as source of triglycerides and using the methylic route for obtaining of esters. For the characterization of biodiesel and its mixtures with mineral diesel oil, physical chemical parameters and several analytical techniques had been used, as well as: gas chromatography (GC), nuclear magnetic resonance of proton (1H NMR), infrared spectroscopy (IR) and thermal analysis. The chromatography confirmed the complete reaction of esters in biodiesel presenting a 97,08% conversion. The 1H - NMR presented singlet in 3,6 ppm corresponding to the hydrogen of the group ester RCOO CH3. The infrared presented a strong band in 1741 cm-1 referring to stretching C=O of ester and an average band in 1175 cm-1 referring C O deformation. With the data of thermal analysis it was possible to observe the thermal and oxidative stability of the samples changing the atmospheres of synthetic air and nitrogen, where stages of the thermal decomposition had been verified and had been attributed to the volatilization and/or decomposition of the triacylglycerides. The thermal degradation of the samples was carried through 150 and 210°C during 1, 12, 24 and 48 hours and was observed change in the thermogravimetric profile, therefore an increase in the number of stages of the thermal decomposition also occurred indicating characteristic intermediate composites of polymerization, being this confirmed through the rheological study that presented brusque increase of viscosity. The kinetic study showed that the activation energy has the following order: biodiesel > mineral diesel oil > mixtures biodiesel/diesel

Synthesis and characterization of hybrids derived from vermiculite chloropropyl and aliphatic diamines

ALVES, Ana Paula de Melo et al. Synthesis and characterization of hybrids derived from vermiculite chloropropyl and aliphatic diamines. Journal of Thermal Analysis and Calorimetry, v.87, n. 3, p.771–774, 2007.

Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Estudo de massa cerâmica triaxial visando à otimização do ciclo de queima da indústria de cerâmica estrutural

Over recent years the structural ceramics industry in Brazil has found a very favorable market for growth. However, difficulties related to productivity and product quality are partially inhibiting this possible growth. An alternative for trying to solve these problems and, thus, provide the pottery industry the feasibility of full development, is the substitution of firewood used in the burning process by natural gas. In order to contribute to this process of technological innovation, this paper studies the effect of co-use of ceramic phyllite and kaolin waste on the properties of a clay matrix, verifying the possible benefits that these raw materials can give to the final product, as well as the possibility of such materials to reduce the heat load necessary to obtain products with equal or superior quality. The study was divided into two steps: characterization of materials and study of formulations. Two clays, a phyllite and a residue of kaolin were characterized by the following techniques: laser granulometry, plasticity index by Atterberg limits, X-ray fluorescence, X-ray diffraction, mineralogical composition by Rietveld, thermogravimetric and differential thermal analysis. To study the formulations, specifically for evaluation of technological properties of the parts, was performed an experimental model that combined planning involving a mixture of three components (standard mass x phyllite x kaolin waste) and a 23 factorial design with central point associated with thermal processing parameters. The experiment was performed with restricted strip-plot randomization. In total, 13 compositional points were investigated within the following constraints: phyllite ≤ 20% by weight, kaolin waste ≤ 40% by weight, and standard mass ≥ 60% by weight. The thermal parameters were used at the following levels: 750 and 950 °C to the firing temperature, 5 and 15 °C/min at the heating rate, 15 and 45min to the baseline. The results showed that the introduction of phyllite and/or kaolin waste in ceramic body produced a number of benefits in properties of the final product, such as: decreased absorption of water, apparent porosity and linear retraction at burn; besides the increase in apparent specific mass and mechanical properties of parts. The best results were obtained in the compositional points where the sum of the levels of kaolin waste and phyllite was maximal (40% by weight), as well as conditions which were used in firing temperatures of 950 °C. Regarding the prospect of savings in heat energy required to form the desired microstructure, the phyllite and the residue of kaolin, for having small particle sizes and constitutions mineralogical phases with the presence of fluxes, contributed to the optimization of the firing cycle.

Síntese e caracterização de TaC e óxido misto de tântalo e cobre nanoestruturados a partir do precursor oxálico de tântalo através de reações gás-sólido e sólido-sólido a baixa temperatura

The research and development of nanostructured materials have been growing significantly in the last years. These materials have properties that were significantly modified as compared to conventional materials due to the extremely small dimensions of the crystallites. The tantalum carbide (TaC) is an extremely hard material that has high hardness, high melting point, high chemical stability, good resistance to chemical attack and thermal shock and excellent resistance to oxidation and corrosion. The Compounds of Tantalum impregnated with copper also have excellent dielectric and magnetic properties. Therefore, this study aimed to obtain TaC and mixed tantalum oxide and nanostructured copper from the precursor of tris (oxalate) hydrate ammonium oxitantalato, through gas-solid reaction and solid-solid respectively at low temperature (1000 ° C) and short reaction time. The materials obtained were characterized by X-ray diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), Spectroscopy X-Ray Fluorescence (XRF), infrared spectroscopy (IR), thermogravimetric (TG), thermal analysis (DTA) and BET. Through the XRD analyses and the Reitiveld refinement of the TaC with S = 1.1584, we observed the formation of pure tantalum carbide and cubic structure with average crystallite size on the order of 12.5 nanometers. From the synthesis made of mixed oxide of tantalum and copper were formed two distinct phases: CuTa10O26 and Ta2O5, although the latter has been formed in lesser amounts

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

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

Análise comparativa entre as propriedades do gesso obtido de rejeito da produção de sal e gesso comerciais

The environmental impacts, caused by the solid residues generation, are an often quoted concern nowadays. Some of these residues, which are originated from different human activities, can be fully reused, reducing the effects of the poor waste management on the environment. During the salt production process, the first formed crystals are discarded as industrial waste. This is mainly made of gypsum that is a calcium sulfate dihydrate (CaSO4.2H2O). The gypsum in question may go through a calcination process due to the plaster (CaSO4.0,5H2O) production and then the application on the cement industry. Considering the necessity of development and application for these industrial wastes, this paper aims to analyze the plaster, called Salgesso, from the gypsum that was generated during the salt production, and its use viability on the civil construction industry in order to create environmental and economical benefits. For characterization, the following experiments were performed: X-ray Fluorescence (XRF), X-ray Diffraction (XRD), thermal analysis (TG/DTG) and Scanning Electron Microscopy (SEM) with EDS. The following tests were also performed to obtain the mechanical characteristics: Thinness Modulus, Unit Mass, Setting Time and Compressive Resistance. Three commercial plasters used on civil construction were taken as references. All of these tests were performed according to the current standards. It was noticed that although there were some conflicting findings between the salt and commercial plasters in all of the studied properties, the Salgesso has its values within the standard limits. However, there is the possibility to improve them by doing a more effective calcination process. Three commercial plasters, used in construction, were used as reference material. All tests were performed according to standards in force. It was observed that although some tests present conflicting findings between the salt and gypsum plasters commercial properties in all of the studied Salgesso have values within the limits imposed by the standard, but can be improved simply by calcination process more effective

Caracterização térmica (TG/DTG, DTA, DSC, DSC-fotovisual) de Hormônios bioidênticos (estriol estradiol)

Bioidentical hormones are defined as compounds that have exactly the same chemical and molecular structure as hormones that are produced in the human body. It is believed that the use of hormones may be safer and more effective than the non-bioidentical hormones, because binding to receptors in the organism would be similar to the endogenous hormone. Bioidentical estrogens have been used in menopausal women, as an alternative to traditional hormone replacement therapy. Thermal data of these hormones are scarce in literature. Thermal analysis comprises a group of techniques that allows evaluating the physical-chemistry properties of a drug, while the drug is subjected to a controlled temperature programming. The thermal techniques are used in pharmaceutical studies for characterization of drugs, purity determination, polymorphism identification, compatibility and evaluation of stability. This study aims to characterize the bioidentical hormones estradiol and estriol through thermal techniques TG/DTG, DTA, DSC, DSC-photovisual. By the TG curves analysis was possible to calculated kinetic parameters for the samples. The kinetic data showed that there is good correlation in the different models used. For both estradiol and estriol, was found zero order reaction, which enabled the construction of the vapor pressure curves. Data from DTA and DSC curves of melting point and purity are the same of literature, showed relation with DSC-photovisual results. The analysis DTA curves showed the fusion event had the best linearity for both hormones. In the evaluation of possible degradation products, the analysis of the infrared shows no degradation products in the solid state

Avaliação do processo industrial da cerâmica vermelha na região do Seridó - RN

Particularly in Braziland in Rio Grande do Norte, companies manufacturing red ceramic, play an important role as agents of development to study the region Seridó- RN, specific place for carrying out the research. It is observed in this region a concentration of red ceramic industries of small size, which, despite its importance in the ceramic, they are unable to enjoy or use the new forms of administrative management and technological advances designed and offered by universities, centers of research and projects of governments, remained almost entirely outside the progress and modernization, technological and administrative. These companies still have outdated technology, and management processes, providing quality problems and standardization of end products. Upon these conditions are the companies going through crisis and struggling to survive alone and without assistance. The region of Seridó-RN, lets make a detailed case study of red ceramic companies in the region proposed from the existing theoretical and actual lifting of the condition of the product manufacturing red ceramic, allowing through this overview of the implementation of collect samples of raw materials, allowing the study of each ceramic industry that contributed to the participation of the research, which was determined parameters such as: analysis of the physical, chemical and technological properties of raw materials, characterization of the processes used, raising the technological resources considering equipment, machinery, supplies, raw materials and facilities available and its organization by type of products from companies involved in this study. The methodology consists of the following steps: collection of raw material, crushing and screening, characterization of raw materials (liquid limit, chemical analysis, mineralogical analysis, differential thermal analysis, sieve analysis), mixing, forming, cutting, drying and burning of ceramic bodies and bodies of evidence. The results showed that it was clay with distinct characteristics with respect to plasticity. With respect to the different compositions of mixtures of ceramic masses, we conclude that the ceramic properties showed a direct proportionality with increasing fraction of the clay not plastic. However, the compositions of the masses studied proved to be the most appropriate for the types of simulated clay for use in ceramics. Adopted in the ceramic processing made it possible to obtain products the resulted in consistent properties, and in some cases even exceeding the requirements of technical studies and standard-Brazilian clays to obtain ceramic products such as tiles, bricks and tiles to floor. Based on the discussions from the results obtained in the various processing steps of this work, one can draw conclusions according to the physico-chemical and mineralogical properties of raw materials, the properties of ceramic products burned and analysis. This work may be used by other researchers, private companies and governmental organizations, undergraduate students and graduate, can develop studies and future research to: develop projects to modify the furnaces; mapping projects develop and rationalize the exploitation of raw materials ;promoting reforestation and forest management; develop reduction projects and recovery of waste; develop training projects in manpower sector, and develop security projects, improving the conditions of work in the area pottery

Uso do pó da palha de carnaúba em compósitos de quitosana

In this work a biodegradable composite using the carnauba straw s powder as reinforcement on chitosan matrix polymeric were manufactured. Firstly, were carried out the chemistry characterization of the carnauba straw s powder before and after treatments with NaOH and hexane. Goering and Van Soest method (1970), flotation test, moisture absorption, FTIR, TG/DTG, DSC and SEM have also being carried out. Composites were developed with variations in granulometry and in powder concentrations. They were characterized by TG/DTG, SEM and mechanicals properties. The results of chemical composition showed that the carnauba straw s powder is composed of 41% of cellulose; 28,9% of hemicellulose and 14% of lignin.The flotation test have indicated that the chemical treatment with NaOH decreased the powder s hidrophilicity.The thermal analysis showed increased of thermal stability of material after treatments. The results of FTIR and SEM revealed the removal of soluble materials from the powder (hemicelluloses and lignin), the material became rougher and clean. The composites obtained showed that the mechanicals properties of the composites were decreased in respect at chitosan films, and the composites with the powder at 150 Mesh showed less variation in the modulus values. The speed test of 10 mm/min showed the better reproducibility of the results and is in agreement to the standard ASTM D638. The SEM analysis of fracture showed the low adhesion between the fiber/matrix. The increase of volume of powder in the composite caused a decrease in values of stress and strain for the samples with untreated powder and treated with hexane. The composite with 50% of the powder s treated in NaOH didn t have significant variation in the values of stress and strain as compared with the composites with 10% of the powder, showing that the increase in the volume of fiber didn t affect the stress and strain of the composite. Thereby, it is concluded that the manufacture of polymeric composites of chitosan using carnauba straw s powder can be done, without need for pre-treatment of reinforcement, become the couple of carnauba straw s powder-chitosan a good alternative for biodegradable composites

Síntese e caracterização de carreadores de oxigênio para combustão com recirculação química obtidos via reação de combustão assistida por microondas

Perovskites oxides win importance by its properties and commercials applications, they have a high thermal stability, have conductive properties, electrical, catalytic, electro catalytic, optical and magnetic, and are thermally stable. Because of these properties, are being widely studied as carriers of oxygen in the process of power generation with CO2 capture. In this work, the base carrier system La1-xMexNiO3 (Me = Ca and Sr) were synthesized by the method via the combustion reaction assisted by microwave. were synthesized from the combustion reaction method by microwave process. This method control the synthesi`s conditions to obtain materials with specific characteristics. The carriers calcined at 800 ° C/2h were analyzed by thermal analysis (TG-DTA), to verify its thermal stability, X-ray diffraction (XRD) to verify the phase formation, with subsequent refinement by the Rietveld method, to quantify the percentage of phases formed, the surface area by BET method was determined, scanning electron microscopy (SEM) was obtained to evaluate the material morphology and temperature programmed reduction (TPR) was done to observe the metallic phase of the nickel. After all proposed characterization and analysis of their results can be inferred to these oxides, key features so that they can be applied as carriers for combustion reactions in chemical cycles. The final products showed perovskite-type structures K2NiF4 (main) and ABO3.

Complexos metálicos de cobalto, níquel e cobre com a Pirazina-2-carboxamida e 4- hidrazida ácida piridincarboxílica: síntese e caracterização

This work involved the synthesis, characterization and proposing the molecular structure of coordination compounds involving ligands pyrazine-2-carboxamide (PZA) and 4- hydrazide acidic pyridine carboxylic (INH) and metals of the first transition series (M = Co2+, Ni2+ and Cu2+). For the characterization of the compounds used were analytical techniques such as infrared absorption spectroscopy average (FT-IR) molar conductivity measurements, CHN elemental analysis, EDTA Complexometric, measurement of melting point, X-ray diffraction by powder method, Thermogravimetry (TG) and Differential Thermal Analysis (DTA) and Simultaneous Differential Scanning Calorimetry (DSC). The absorption spectra in the infrared region suggested that the ligand coordination to the metal center occurs through the carbonyl oxygen atom and nitrogen alpha pyrazine ring to those complexes formed with PZA. For INH complexes with metal-ligand coordination is through the carbonyl oxygen and nitrogen of the terminal hydrazide grouping. The conductivity measurements of the complexes in aqueous solution they suggest to all behavior of the type 1:2 electrolytes, and conduct of non-electrolytes in acetonitrile. The results obtained by CHN elemental analysis and EDTA Complexometric allowed to infer the stoichiometry of the compounds synthesized. For all of the complexes obtained was possible to record the melting points, neither of which melted near the melting temperature of the free ligands. The X-ray diffraction showed that the complexes of pyrazinamide exhibited diffraction lines, suggesting that these compounds are crystalline, while compounds of isoniazid, with the exception of cobalt, exhibited diffraction lines, indicating that they are crystalline. The results from the TG-DTA and DSC allowed information regarding the dehydration and thermal decomposition of these complexes

Síntese e caracterização de óxidos de zinco e de magnésio suportados em A1SBA-15 para produção de biodiesel

To overcome the challenge of meeting growing energy demand in a sustainable way, biodiesel has shown very promising as alternative energy can replace fossil fuels, even partially. Industrially, the biodiesel is produced by homogeneous transesterification reaction of vegetable oils in the presence of basic species used as catalysts. However, this process is the need for purification of the esters obtained and the removal of glycerin formed after the reaction. This context, the alternative catalysts have that can improve the process of biodiesel production, aiming to reduce costs and facilitate its production. In this study, the AlSBA-15 support with Si / Al ratio = 50 was synthesized, as like as the heterogeneous catalysts of zinc oxide and magnesium supported on mesoporous AlSBA-15 silica, in the concentrations of 5, 10, 15 and 30 %, relative to the support. The textural properties and structural characterization of catalysts and supports were determined by techniques: X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) coupled to the chemical analyzer, adsorption / desorption of N2, thermal analysis (TG / DTG), absorption spectroscopy in the infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). Characterization results indicated that the support AlSBA-15 retained the hexagonal ordered after the incorporation of zinc oxide and magnesium oxide in the holder. For heterogeneous catalysts, ZnO-AlSBA-15, that was observed the presence of zinc oxide nanoparticles dispersed in the surface and interior channels of the mesoporous and microporous support. The catalytic activity was evaluated by the transesterification reaction of sunflower oil via methylic route, and some reaction parameters were optimized with the most active catalyst in biodiesel production by sunflower oil. For the series of heterogeneous catalysts, the sample with 30 % ZnO supported on AlSBA-15 showed a better conversion of triglyceride to methyl esters, about 95.41 % of reaction conditions: temperature 175 °C, with molar ratio of 42:1, stirring at 200 rpm and under a pressure of 14 bar for 6 h. The catalyst MgO-AlSBA-15 showed no catalytic activity in the studied reactions

Trissoralen um medicamento de baixa dosagem: estudos termoanalíticos da compatibilidade do fármaco-excipientes e determinação de parâmetros de qualidade para cápsulas magistrais

The trioxsalen (Tri) is a low-dose drug used in the treatment of psoriasis and other skin diseases. The aim of the study was applying the thermal analysis and complementary techniques for characterization, evaluation of the trioxsalen stability and components of manipulated pharmaceutical formulations. The thermal behavior of the Tri by TG/DTG-DTA in dynamic atmosphere of synthetic air and nitrogen showed the same profile with a melting peak followed by a volatilization-related event. From the curves TG / DTG is observed a single stage of mass loss. By heating the drug in the stove at temperatures of 80, 240 and 260 °C, it had no change in chemical structure through the techniques of XRD, HPLC, MIR, OM and SEM. From the non-isothermal and isothermal TG kinetic studies was possible to calculate the activation energy and reaction order for the Tri. The drug showed good thermal stability. Studies on drug-excipient compatibility showed interaction of trissoralen with sodium lauryl sulfate 1:1. There was no interaction with aerosol, pregelatinized starch, sodium starch glycolate, cellulose, croscarmellose sodium, magnesium stearate, lactose and mannitol.The characterization of three trioxsalen formulations at concentrations of 2.5, 5, 7.5, 10, 12.5 and 15 mg was performed by DSC, TG / DTG, XRD, NIR and MIR. The PCA classification method based on spectral data from the NIR and MIR of trissoralen formulations allows successful differentiation into three groups. The formulation 3 was the one that best showed analytical profile with the following composition of aerosil excipients, pre-gelatinized starch and cellulose. The activation energy of the volatilization process of the drug was determined in binary mixtures and formulation 3 through fitting and isoconversional methods. The binary mixture with sodium starch glycolate and lactose showed differences in kinetic parameters compared to the drug isolated. The thermoanalytical techniques (DSC and TG / DTG) were shown to be promising methodologies for quantifying trioxsalen obtained by the linearity, selectivity, no use solvents, without sample preparation, speed and practicality.