Incorporação de resíduo de perfuração em matriz cerâmica: estabilização por solidificação

One of the waste generated during the drilling of oil wells are gravel which are impregnated of drilling fluid. This residue consists of highly toxic chemicals, including toxic metals. This study suggests an alternative process to the treatment of this waste, by incorporating it the form of raw material in the ceramic matrix , and by solidification and stabilize the metals present, Aluminum (Al), Iron (Fe), Manganese (Mn) and Zinc (Zn). The raw materials were characterized by the techniques of X ray fluorescence (FRX), X ray diffraction (DRX), laser granulometry (GL), thermogravimetry (TG) and differential thermal analysis (ADT). To evaluate the percentage of gravel effect the environmental and technological properties were obtained from formulations containing 0, 10 and 20 % by weight of gravel in the ceramic matrix. After sintering at temperatures 1080, 1120 and 1160 °C, the samples were tested for water absorption, the linear shrinkage firing, voltage of rupture and solubility. The results obtained showed that the stabilization by solidification, is a viable alternative to safe disposal of waste drilling. Ceramics products can be used in the manufacture of solid bricks

Estudo da estabilidade térmica de adoçantes naturais e artificiais

Sweeteners provide a pleasant sensation of sweetness that helps the sensory quality of the human diet, can be divided into natural sweeteners such as fructose, galactose, glucose, lactose and sucrose, and articial sweeteners such as aspartame, cyclamate and saccharin. This work aimed to study the thermal stability of natural and artificial sweeteners in atmospheres of nitrogen and syntetic air using thermogravimetry (TG), derivative thermogravimetry (DTG), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). Among the natural sweeteners analyzed showed higher thermal stability for the lactose and sucrose, which showed initial decomposition temperatures near 220 ° C, taking advantage of the lactose has a higher melting point (213 ° C) compared to sucrose (191 ° C). The lower thermal stability was observed for fructose, it has the lowest melting point (122 °C) and the lower initial decomposition temperature (170 °C). Of the artificial sweeteners studied showed higher thermal stability for sodium saccharin, which had the highest melting point (364 ° C) as well as the largest initial decomposition temperature (466 ° C under nitrogen and 435 ° C in air). The lower thermal stability was observed for aspartame, which showed lower initial decomposition temperature (158 ° C under nitrogen and 170 ° C under air). For commercial sweeteners showed higher thermal stability for the sweeteners L and C, which showed initial temperature of thermal decomposition near 220 ° C and melting points near 215 ° C. The lower thermal stability was observed for the sweetener P, which showed initial decomposition temperature at 160 ° C and melting point of 130 °C. Sweeteners B, D, E, I, J, N and O had low thermal stability, with the initial temperature of decomposition starts near 160 °C, probably due to the presence of aspartame, even if they have as the main constituent of the lactose, wich is the most stable of natural sweeteners. According to the results we could also realize that all commercial sweeteners are in its composition by at least a natural sweeteners and are always found in large proportions, and lactose is the main constituent of 60% of the total recorded

Estudo termoanalítico da perlita hidrofobizada com óleo de linhaça

In this work, expanded perlite, a mineral clay, consisting of SiO2 and Al2O3 in the proportions of 72.1 and 18.5%, respectively, was used as an adsorbent for oil in its pure expanded form as well as hydrofobized with linseed oil. Thermogravimetry (TG), Derivative Thermogravimetry (DTG) and Differential Thermal Analysis (DTA) were used to study the thermal behavior and quantify the percent adsorption of perlite in differents processes comparing the results with the ones obtained using Gravimetric Analysis. In the process of hydrophobization with linseed oil granulometric fractions > 20, 20-32 and 32-60 mesh were used and adsorption tests with crude oil were performed in triplicate at room temperature. The results obtained by TG/DTG in dynamic atmosphere of air showed mass losses in a single step for the expanded perlite with pure adsorbed oil, indicating that the adsorption of oil was limited and that the particle size did not in this process. Linseed oil has performed well as an agent of hydrophobized perlite (32 to 60 mesh) indicating a maximum percentage of 59.9% and 68.6% the linseed with a fraction range from considering the data obtained by thermogravimetry and Gravimetry, respectively. The adsorption of oil in the expanded perlite and hydrofobized pure perlite with linseed oil did not produce good results, characterizing an increase of 0.5 to 4.6% in pure perlite and 3.3% in hydrofobized perlite with granulometric 32 to 60 mesh

Avaliação da estabilidade térmica e oxidativa do biodiesel de algodão e do efeito da adição de antioxidantes (α-tocoferol e BHT)

This work aims to study the effects of adding antioxidants, such as, α- tocopherol and BHT on the thermal and oxidative stability of biodiesel from cottonseed (B100). The Biodiesel was obtained through the methylical and ethylical routes. The main physical and chemical properties of cotton seed oil and the B100 were determined and characterized by FTIR and GC. The study of the efficiency of antioxidants, mentioned above, in concentrations of 200, 500, 1000, 1500, 2000ppm, to thermal and oxidative stability, was achieved by Thermogravimetry (TG), Differential Thermal Analysis (DTA), Differential Scanning Calorimetry (DSC), Differential Scanning Calorimetry - Hi-Pressure (P-DSC) and Rancimat. The Biodiesel obtained are within the specifications laid down by Resolution of ANP No7/2008. The results of TG curves show that the addition of both antioxidants, even in the lowest concentration, increases the thermal stability of Biodieseis. Through the DTA and DSC it was possible to study the physical and chemical transitions occurred in the process of volatilization and decomposition of the material under study. The initial time (OT) and temperature (Tp) of oxidation were determined through the P-DSC curve and they showed that the α-tocopherol has a pro-oxidant behavior for some high concentrations. The BHT showed better results than the α-tocopherol, with regard to the resistance to oxidation

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

Desenvolvimento de uma rota química alternativa de síntese de SrCo0,8Fe0,2O3- e LaNi0,3Co0,7O3- para aplicação na reação de oxidação do CO

This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d

Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

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 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

Caracterização de matérias-primas regionais e desenvolvimento de formulações de massas cerâmicas para porcelanato

Initially concentrated in some poles at the South and Southeast regions of Brazil, the ceramic tiles industry became wide during the 80 s decade, with a disconcentration industrial and regional pulverization. The competitiveness in the ceramic tiles internal and external consumers markets, it has debtor the industries to invest in sophisticated products each time more, either in design or the technology, but, mainly, in its final properties. Amongst the diverse types of ceramic coating, the porcelanato if has detached had to its process of technological production and excellent characteristics techniques. The Porcelanato is currently the material for coatings that presents the best technical and aesthetic features when compared with others ceramics found on the market. The chemical composition and the others raw materials characteristics have an importance that must to be ally to the inherent characteristics of fabrication process, essentially those related to the cycle of burning. This work had as purpose to develop formularizations of ceramic mass for production of porcelanato without glass coating, pertaining to the group BIa (text of absorption of water ≤ 0.5%) and with resistance superior mechanics 35MPa from raw materials characterized. The ceramic raw materials selected to the development of this study (A1 and A2 clays, feldspate, talc and quartz) were submitted to the following tests: X-ray fluorescence - chemical analysis determination; X-ray diffraction - Analysis of the stages mineralogics; Laser granulometry - size distribution of particles; and Differential thermal analysis - thermal behavior. Were performed tests of absorption of water, lineal retraction of it burns, apparent specific mass and rupture tension the flexing. The results had evidenced that the formularizations that had the A1 clay and talc on its composition were efficient for the porcelanato production remaining their technological characteristics inside of the intervals of variation desired by the Norms of the ABNT

Estudo das propriedades termofísicas com variação da expansibilidade de compósito desenvolvido com matriz PUR-NOP e carga funcional de argilomineral

In this study were conducted experimental procedures for determination of variation of the expandability of rigid polyurethane foam (PUR) from a natural oil polyol (NOP), specifically the Castor oil plant, Ricinus communis, pure and additions of the vermiculite in phase dispersed in different percentage within a range from 0% to 20%, mass replacement. From the information acquired, were defined the parameters for production of bodies of test, plates obtained through controlled expansion, with the final volume fixed. Initially, the plates were subjected to thermal performance tests and evaluated the temperature profiles, to later be extracted samples duly prepared in accordance with the conditions required for each test. Was proceeded then the measurement of the coefficient of thermal conductivity, volumetric capacity heat and thermal diffusivity. The findings values were compared with the results obtained in the tests of thermal performance, contributing to validation of the same. Ultimately, it was investigated the influence that changes in physical-chemical structure of the material had exerted on the variation of thermophysical quantities through gas pycnometry, scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectroscopy (EDXRF), infrared spectroscopy using Fourier transform (FTIR), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Based on the results obtained was possible to demonstrate that all load percentage analyzed promoted an increase in the potential expansion (PE) of the resin. In production of the plates, the composites with density near at the free expansion presented high contraction during the cure, being the of higher density adopted as definitive standard. In the thermal performance tests, the heating and cooling curves of the different composites had presented symmetry and values very close for lines of the temperature. The results obtained for the thermophysical properties of composites, showed little difference in respect of pure foam. The percentage of open pores and irregularities in the morphology of the composites were proportionate to the increment of vermiculite. In the interaction between the matrix and dispersed phase, there were no chemical transformations in the region of interface and new compounds were not generated. The composites of PUR-NOP and vermiculite presented thermal insulating properties near the foam pure and percentage significantly less plastic in its composition, to the formulation with 10% of load

Incorporação de cinzas da casca de café na produção de placas cerâmicas para revestimento

Brazil is the world s leading coffee producer. In 2008, 45.99 million of 60 kg bags of benefited coffee were produced. In the process of improvement 50% is grain and 50% is husk, thus, 1.38 million tons of coffee husk are produced annually. The husk is used as combustible in the drying and improvement ovens in the coffee farms, generating ash as residue. These ashes contain a high concentration of alkaline metals and earth metals, mainly K2O and CaO. This work studies the use of this residue in the ceramic tiles industry, as fluxing agents in substitution to the feldspar. Ten mixtures with equal ratios of clay and kaolin, proceeding from Bahia and the residue (varying from 30 to 5%) were defined and produced in uniaxial tool die of 60x20mm with approximately 5 mm of thickness and 45MPa compacting pressure. The samples were fired in four different temperatures: 1100 °C, 1150 °C, 1185 °C and 1200 °C during 60 minutes and characterized by means of X-ray fluorescence, X-ray diffraction, gravimetric thermal analysis and differential thermal analysis. The results of water absorption, apparent porosity, linear shrinkage, XRD, dilatometry, flexural strength and SEM were also analysed. The test specimen with addition of 10% of ash fired in 1200 °C resulted in 0.18% water absorption and 40.77 MPa flexural strength, being classified as porcelain stoneware tiles according to ABNT, UNI and ISO norms

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)

Desenvolvimento de catalisadores bifuncionais de óxido de zircônio modificado por óxidos de tungstênio e molibdênio contendo platina para a reação de isomerização de n-parafinas

Bifunctional catalysts based on zircon oxide modified by tungsten (W = 10, 15 and 20 %) and by molybdenum oxide (Mo= 10, 15 e 20 %) containg platinum (Pt = 1%) were prepared by the polymeric precursor method. For comparison, catalysts the tungsten base was also prepared by the impregnation method. After calcinations at 600, 700 and 800 ºC, the catalysts were characterized by X-ray diffraction, fourier-transform infrared spectroscopy, thermogravimetric and differential thermal analysis, nitrogen adsorption and scanning electron microscopy. The profile of metals reduction was determined by temperature programmed reduction. The synthesized catalysts were tested in n-heptane isomerization. X-ray diffractogram of the Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts revealed the presence of tetragonal ZrO2 and platinum metallic phases in all calcined samples. Diffraction peaks due WO3 and ZrO2 monoclinic also were observed in some samples of the Pt/WOx-ZrO2 catalysts. In the Pt/MoOx-ZrO2 catalysts also were observed diffraction peaks due ZrO2 monoclinic and Zr(MoO4)2 oxide. These phases contained on Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts varied in accordance with the W or Mo loading and in accordance with the calcination temperature. The infrared spectra showed absorption bands due O-W-O and W=O bonds in the Pt/WOx-ZrO2 catalysts and due O-Mo-O, Mo=O and Mo-O bonds in the Pt/MoOx-ZrO2 catalysts. Specific surface area for Pt/WOx-ZrO2 catalysts varied from 30-160 m2 g-1 and for the Pt/MoOx-ZrO2 catalysts varied from 10-120 m2 g-1. The metals loading (W or Mo) and the calcination temperature influence directly in the specific surface area of the samples. The reduction profile of Pt/WOx-ZrO2 catalysts showed two peaks at lower temperatures, which are attributed to platinum reduction. The reduction of WOx species was evidenced by two reduction peak at high temperatures. In the case of Pt/MoOx-ZrO2 catalysts, the reduction profile showed three reduction events, which are attributed to reduction of MoOx species deposited on the support and in some samples one of the peak is related to the reduction of Zr(MoO4)2 oxide. Pt/WOx-ZrO2 catalysts were active in the n-heptane isomerization with high selectivity to 3-methyl-hexane, 2,3- dimethyl-pentane, 2-methyl-hexane among other branched hydrocarbons. The Pt/MoOx-ZrO2 catalysts practically didn't present activity for the n-heptane isomerization, generating mainly products originating from the catalytic cracking

Síntese e caracterização de pós Ba(x)Sr(1-x)Co0,8Fe0,2O3- através do método de coprecipitação via oxalato

Ceramic powders based on oxides of perovskite-type structure is of fundamental interest nowadays, since they have important ionic-electronic conductivity in the use of materials with technological applications such as gas sensors, oxygen permeation membranes, catalysts and electrolytes for solid oxide fuel cells (SOFC). The main objective of the project is to develop nanostructured ceramic compounds quaternary-based oxide Barium (Br), Strontium (Sr), Cobalt (Co) and Iron (Fe). In this project were synthesized compounds BaxSr(1-x)Co0, 8Fe0,2O3- (x = 0.2, 0.5 and 0.8) through the oxalate co-precipitation method. The synthesized powders were characterized by thermogravimetric analysis and differential thermal analysis (TGADTA), X-ray diffraction (XRD) with the Rietveld refinement using the software MAUD and scanning electron microscopy (SEM). The results showed that the synthesis technique used was suitable for production of nanostructured ceramic solid solutions. The powders obtained had a crystalline phase with perovskite-type structure. The TGA-DTA results showed that the homogeneous phase of interest was obtained temperature above 1034°C. It was also observed that the heating rate of the calcination process did not affect the elimination of impurities present in the ceramic powder. The variation in the addition of barium dopant promoted changes in the average crystallite size in the nanometer range, the composition being BSCF(5582) obtained the lowest value (179.0nm). The results obtained by oxalate co-precipitation method were compared with those synthesis methods in solid state and EDTA-citrate method