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 de pigmento cerâmico ferrita de cobalto utilizando planejamento experimental

Synthetic inorganic pigments are the most widely used in ceramic applications because they have excellent chemical and thermal stability and also, in general, a lower toxicity to man and to the environment. In the present work, the ceramic black pigment CoFe2O4 was synthesized by the polymerization Complex method (MPC) in order to form a material with good chemical homogeneity. Aiming to optimize the process of getting the pigment through the MPC was used a fractional factorial design 2(5-2), with resolution III. The factors studied in mathematical models were: citric acid concentration, the pyrolysis time, temperature, time and rate of calcination. The response surfaces using the software statistica 7.0. The powders were characterized by thermal analysis (TG/DSC), x-ray diffraction (XRD), scanning electron microscopy (SEM) and spectroscopy in the UV-visible. Based on the results, there was the formation of phase cobalt ferrite (CoFe2O4) with spinel structure. The color of the pigments obtained showed dark shades, from black to gray. The model chosen was appropriate since proved to be adjusted and predictive. Planning also showed that all factors were significant, with a confidence level of 95%

Estudos comparativos do ciclo de regeneração de diferentes tipos de silicoaluminofosfatos

Different types of heterogeneous catalysts of the silicoaluminophosphate type, (SAPO-5, SAPO-11, SAPO-31, SAPO-34 and SAPO-41), molecular sieves with a: AFI, AEL, ATO, CHA and AFO structure, respectively, were synthesized through the hydrothermal method. Using sources such as hydrated alumina (pseudobohemita), phosphoric acid, silica gel, water, as well as, different types of organic structural templates, such as: cetyltrimethylammonium bromide (CTMABr), di-isopropylamine (DIPA), di-n- propylamine (DNPA) and tetraethylammonium hydroxide (TEOS), for the respective samples. During the preparation of the silicoaluminophosphates, the crystallization process of the samples occurred at a temperature of approximately 200 ° C, ranging through periods of 18-72 h, when it was possible to obtain pure phases for the SAPOs. The materials were furthermore washed with deionized water, dried and calcined to remove the molecules of the templates. Subsequently the samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), absorption spectroscopy in the infrared region (FT-IR), specific surface area and thermal analysis via TG/DTG. The acidic properties were determined using adsorption of n-butylamine followed by programmed termodessorption. These methods revealed that the SAPO samples showed a typically weak to moderate acidity. However, a small amount of strong acid sites was also detected. The deactivation of the catalysts was conducted by artificially coking the samples, followed by n-hexane cracking reactions in a fixed bed with a continuous flow micro-reactor coupled on line to a gas chromatograph. The main products obtained were: ethane, propane, isobutene, n-butane, n-pentane and isopentane. The Vyazovkin (model-free) kinetics method was used to determine the catalysts regeneration and removal of the coke

Estudo da adição de resíduo de scheelita em matriz cerâmica: formulação, propriedades físicas e microestrutura

Extractivism mineral is considered an activity highly degrading, due to the large volume of material that he moves in the form of ore and residues. The vast majority of mining companies do not show any technology or economically viable application that will allow the recycling of mineral residue, these being launched in areas receiving located the "open skies" degrade the environment. In Rio Grande do Norte to the production of ceramic red restricts their activities to the production of products such as: solid bricks, ceramic blocks, tiles, among others. Seeking to unite experiences and technical information that favor sustainable development, with important benefits to the construction sector and civil society in general, the present work studies the incorporation of the residue of scheelite in ceramic matrix kaolinitic, coming from the municipality of Boa Saúde - RN, in percentage of 5 %, 10 %, 20 %, 30% 40% and 50 %, by evaluating its microstructure, physical properties and formulation. The raw materials were characterized through the trials of X ray fluorescence, Diffraction of X rays, Differential Thermal Analysis and Termogravimetric Analysis. The samples were formed and fired at temperatures of 850o, 900o, 1000o, 1050o, 1100o, 1150o and 1200 oC, with isotherm of 1 hour and heating rate of 10 oC/min. Assays were performed technological of loss to fire, Water Absorption, Apparent Porosity, Apparent Density, Mass Loss in Fire and Bending Resistance; in addition to the Scanning Electron Microscopy, analyzing their physical and mechanical properties. The use of residue of scheelite in ceramic mass kaolinitic provided a final product with technological properties that meet the technical standards for the production of bricks and roofing tiles, with the percentage of 20% of waste that showed the best results

Síntese e caracterização de ferrita ni-zn pelo método dos precursores poliméricos calcinada por energia de microondas

Magnetic ceramics have been widely investigated, especially with respect to intrinsic and extrinsic characteristics of these materials. Among the magnetic ceramic materials of technological interest, there are the ferrites. On the other hand, the thermal treatment of ceramic materials by microwave energy has offered various advantages such as: optimization of production processes, high heat control, low consumption of time and energy among others. In this work were synthesized powders of Ni-Zn ferrite with compositions Ni1- xZnxFe2O4 (0.25 ≤ x ≤ 0.75 mols) by the polymeric precursor route in two heat treatment conditions, conventional oven and microwave energy at 500, 650, 800 and 950°C and its structural, and morphological imaging. The materials were characterized by thermal analysis (TG/ DSC), X-ray diffraction (XRD), absorption spectroscopy in the infrared (FTIR), scanning electron microscopy (SEM), X-ray spectroscopy and energy dispersive (EDS) and vibrating sample magnetometry (VSM). The results of X-ray diffraction confirmed the formation of ferrite with spinel-type cubic structure. The extrinsic characteristics of the powders obtained by microwave calcination and influence significantly the magnetic behavior of ferrites, showing particles ferrimagnéticas characterized as soft magnetic materials (soft), is of great technological interest. The results obtained led the potential application of microwave energy for calcining powders of Ni-Zn ferrite

Estudo da potencialidade da incorporação de resíduo de granito e da queima da casca do café em cerâmica vermelha

The industrial production of ornamental rocks and the burning of coffee husk generate waste that is discarded into the environment. However, with the study of the incorporation of these residues in ceramic products, may be found an alternative to reducing environmental impacts and detrimental effects on human health caused by its indiscriminate disposal of waste in nature. Thus, this work aimed to study the addition of ashes of the coffee husk and granite residue in matrix of red ceramic. The raw materials were dry milled and sieved to mesh 100. To characterize the raw materials were carried out analyzes of X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size analysis (PSA), differential thermal analysis (DTA) and thermogravimetric analysis (TG). Six formulations were prepared where the clay content was kept constant (70%wt) and ashes contents and granite residue varied from 10, 15, 20 and 30%. Dilatometrics analyzes were performed at four selected formulations, containing them: 100% clay (A100); 70% clay and 30% ashes (A70C30); 70% clay and 30% granite residue (A70G30); and 70% clay, 15% granite residue and 15% ashes (A70G15C15). The samples were prepared by uniaxial compaction with pressure of 25 MPa, and fired at temperatures of 800°C, 850ºC, 900ºC, 950ºC, 1000ºC and 1100°C. Assays were performed to determine the linear shrinkage of burning (LSB), water absorption (WA), apparent porosity (AP), density (D) and tensile bending. Also were performed analyzes of X-ray diffraction (XRD) and scanning electron microscopy (SEM) of the samples fired. The formulations incorporating granite residue and/or ashes reached the required limits of water absorption according to NBR 15270-1 and NBR 15310 and tensile bending according to classical literature (SANTOS, 1989) necessary for the production of tiles and ceramic block for masonry sealing

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

Formulação de bloco intertravado cerâmico com adição de resíduos urbanos e industriais

The production of waste from urban and industrial activities is one of the factors of environmental contamination and has aroused attention of the scientific community, in the sense of its reuse. On the other hand, the city of Salvador/Ba, with approximately 262 channels, responsible for storm water runoff, produces every year, by the intervention of cleaning and clearing channels, a significant volume of sediments (dredged mud), and thus an appropriate methodology for their final destination. This study aims to assess the influence of incorporation of these tailings in arrays of clay for production of interlocked block ceramic, also known as ceramic paver. All the raw materials from the metropolitan region of Salvador (RMS) were characterized by x-ray fluorescence, x-ray diffraction, thermal analysis (TG and TDA), particle size analysis and dilatometry. With the use of statistical experimental planning technique, ternary diagram was defined in the study region and the analyzed formulations. The specimens were prepared with dimensions of 60x20x5mm³, by uniaxial pressing of 30 MPa and after sintering at temperatures of 900°, 1000º and 1100ºC the technological properties were evaluated: linear shrinkage, water absorption, apparent porosity, apparent specifies mass, flexural rupture and module. For the uniaxial compression strength used cylindrical probe body with Ø 50 mm. The standard mass (MP) was prepared with 90% by weight of clay and 10% by weight of Channel sediment (SCP), not being verified significant variations in the properties of the final product. With the incorporation of 10% by weight of manganese residue (PFM) and 10% by weight of the Ceramic waste (RCB) in the mass default, in addition to adjusting the plasticity due to less waste clay content, provided increased linear firing shrinkage, due the significant concentration of K2O, forming liquid phase at low temperature, contributing to decreased porosity and mechanical resistance, being 92,5 MPa maximum compressive strength verified. After extract test leachate and soluble, the piece containing 10% of the PFM, was classified as non-hazardous and inert material according to NBR10004/04 ABNT. The results showed the feasibility on using waste, SCP, RCB and PFM clay mass, at temperatures above 900ºC, paver ceramic production, according to the specifications of the technical standards, so that to exceed the 10% of the PFM, it becomes imperative to conduct studies of environmental impacts

Propriedade fotoluminescente da ZrO2: Tb+3, Eu+3, Tm+3 obtida pelo método de polimerização de complexos

Recent studies are investigating a new class of inorganic materials which arise as a promising option for high performance applications in the field of photoluminescence. Highlight for rare earth (TR +3 ) doped, which have a high luminous efficiency, long decay time and being able to emit radiation in the visible range, specific to each element. In this study, we synthesized ZrO2: Tb +3 , Eu +3 , Tm +3 nanoparticles complex polymerization method (CPM). We investigated the influences caused by the heat treatment temperature and the content of dopants in zirconia photoluminescent behavior. The particles were calcined at temperature of 400, 500 and 600 ° C for two hours and ranged in concentration of dopants 1, 2, 4 and 8 mol% TR +3 . The samples were characterized by thermal analysis, X-ray diffraction, photoluminescence of measurements and uv-visible of spectroscopies. The results of X-ray diffraction confirmed the formation of the tetragonal and cubic phases in accordance with the content of dopants. The photoluminescence spectra show emission in the region corresponding simultaneous to blue (450 nm), green (550 nm) and red (615 nm). According to the results, ZrO2 particles co-doped with rare earth ions is a promising material white emission with a potential application in the field of photoluminescence

Efeito da adição de fibras da palma do licuri (syagrus coronata) no comportamento físico e mecânico de compósitos de matriz cimentícia

This research was motivated by the requirement of asbestos s replacement in building systems and the need to generate jobs and income in the country side of the state of Bahia, Brazil. The project aimed at using fibers from licuri leaves (syagrus coronata), an abundant palm in the region, to produce composites appropriate for the sustainable production of cement fibre reinforced products in small plants. The composites were produced in laboratory using Portland cement CP-II-F32, sand, water, licuri palm fiber contents of 1.0, 1.5 and 2.0% by weight of binder (two different fiber length) and metakaolin. The latter was chosen as an additional binder for its efficiency to reduce the alkalinity of cementitious matrixes therefore preventing the degradation of vegetable fibers. The characterization of the composite components was carried out by sieving and laser particle size analyses, thermal analysis, fluorescence and X-ray diffraction. The composites performance was evaluated by 3- point-bending tests, compressive strength, ultrasound module of elasticity, free and restrained shrinkage, water capillarity absorption and apparent specific gravity. It has been found that the addition of fibers increased the time to onset of cracking over 200.00% and a 25% reduction in cracks opening in the restrained shrinkage test. The capillary absorption reduced about 25% when compared to fiber-free composites. It was also observed with regard to flexural strength, compressive strength and specific gravity, that the addiction of fibers did not affect the composite performance presenting similar results for compounds with and without fibers. In general it can be stated that the reinforced composite fibers of palm licuri presents physical and mechanical characteristics which enable them to be used in the intended proposals of this research

Rejeito de xisto como adsorvente para remoção de fenol em águas produzidas na indústria de petróleo

Produced water is the main effluent linked to the activity of extraction of oil and their caring management is necessary due to the large volume involved, to ensure to minimize the negative impacts of discharges of these waters in the environment. This study aimed to analyze the use of retorted shale, which is a reject from the pyrolysis of pirobituminous shale, as adsorbent for the removal of phenols in produced water. The material was characterized by different techniques (grain sized analysis, thermal analysis, BET, FRX, FT-IR, XRD and SEM), showing the heterogeneity in their composition, showing its potential for the removal of varied compounds, as well as the phenols and their derivatives. For the analysis of the efficiency of the oil shale for the adsorption process, assays of adsorption balance were carried through, and also kinetic studies and dynamics adsorption, in the ETE of the UTPF of Petrobras, in Guamaré-RN. The balance assays shown a bigger conformity with the model of Langmuir and the kinetic model more adjusted to describe the adsorption of phenols in retorted shale was of pseudo-second order. The retorted shale presented a low capacity of adsorption of phenols (1,3mg/g), when related to others conventional adsorbents, however it is enough to the removal of these composites in concentrations presented in the produced water of the UTPF of Guamaré. The assays of dynamics adsorption in field had shown that the concentration of phenol in the effluent was null until reaching its rupture (58 hours). The results showed the possibility of use of the reject for removal of phenols in the final operations of the treatment process, removing as well, satisfactorily, the color and turbidity of the produced water, with more than 90% of removal

Avaliação térmica dos resíduos da destilação atmosférica das blendas - biodiesel/diesel

The worldwide concern regarding the use of sustainable energy and preserving the environment are determining factors in the search for resources and alternative sources of energy and therefore fuel less aggressive nature. In response to these difficulties Biodiesel has emerged as a good solution because it is produced from renewable sources, produces burns cleaner and is easily reproducible. This work was synthesized with biodiesel oil, sunflower via homogeneous catalysis in the presence of KOH, with and without the use of BHT and subsequently added to the blends BX (a proportion of biodiesel X = 5, 10, 15 and 20 %). Atmospheric distillation of the analysis, performed in blends with and without BHT were collected residue generated by each sample and performed a study heat from the thermogravimetric analysis at a heating rate of 10 °C*min-1, nitrogen atmosphere and heating to 600 °C. According to the specifications of Resolution N 7/2008 for biodiesel, it was found that the synthesized material was in accordance with the specifications. For blends showed that the samples are in accordance with the Resolution of ANP N 42/2009. From the TG / DTG curves of the samples of biodiesel, blends and waste can be seen that these show a single loss of thermal decomposition concerning constituents present in each sample. The blends without BHT with ratios of 5%, 10% and 15% biodiesel showed a lower amount of waste (1,07%; 1,09% e 1,10%) to mineral diesel (1,15%). Therefore, it is concluded that the addition of biodiesel with diesel mineral can improve some physico-chemical parameters, but also, depending on the added amount, decreasing the amount of waste generated. This fact is of great importance because the carbonaceous residue can cause problems in mechanical equipment and parts for vehicles, causing more frequent maintenance, and this is not desirable

Obtenção de álcool alílico (PROP-2-EN-1-OL) a partir da glicerina derivada do biodiesel de óleo de mamona

In this work, biodiesel was produced from castor oil that was a byproduct glycerin. The molar ratio between oil and alcohol, as well as the use of (KOH) catalyst to provide the chemical reaction is based on literature. The best results were obtained using 1 mol of castor oil (260g) to 3 moles of methyl alcohol (138g), using 1.0% KOH as catalyst at a temperature of 260 ° C and shaken at 120 rpm. The oil used was commercially available, the process involves the reaction of transesterification of a vegetable oil with methyl alcohol. The product of this reaction is an ester, biodiesel being the main product and the glycerin by-product which has undergone treatment for use as raw material for the production of allyl alcohol. The great advantage of the use of glycerin to obtain allyl alcohol is that its use eliminates the large amount of waste of the biodiesel and various forms of insult to the environment. The reactions for the formation of allyl alcohol was conducted from formic acid and glycerin in a ratio 1/1, at a temperature of 260oC in a heater blanket, being sprayed by a spiral condenser for a period of 2 hours and the product obtained contains mostly the allylic alcohol .. The monitoring of reactions was performed by UV-Visible Spectrophotometer: FTIR Fourier transform, the analysis showed that these changes occur spectrometer indicating the formation of the product allylic alcohol (prop-2-en-1-ol) in the presence of water, This alcohol was appointed Alcohol GL. The absorption bands confirms that the reaction was observed in (υ C = C) 1470 -1600 cm -1 and (υ CO), 3610-3670 attributed to C = C groups and OH respectively. The thermal analysis was carried out in a thermogravimetric analyzer SDT Q600, where the mass and temperature are displayed against time, that allows checking the approximate rate of heating. The innovative methodology developed in the laboratory (LABTAM, UFRN), was able to treat the glycerine produced by transesterification of castor oil and used as raw material for production of allyl alcohol, with a yield of 80%, of alcohol, the same is of great importance in the manufacture of polymers, pharmaceuticals, organic compounds, herbicides, pesticides and other chemicals