993 resultados para difração de raios X
Resumo:
Pozzolanic materials such as rice husk ash are widely used to substitute part of cement, because they react with calcium hydroxide (CH) producing calcium silicate hydrate (C-S-H), which aggregate better physical, chemical and mechanical properties to the cement slurry. The usage of rice husk biomass ash from agribusiness in addition to or partially replacing cement is a noble purpose and a good way of sustainable development which currently is an obsession around the world. The ashes utilized in this study were characterized by: scanning electron microscopy technique (SEM), Fourier transform infrared spectroscopy (FTIR), Energy-dispersive X-ray spectroscopy (EDX) and BET method. The pozzolanic activity of RHA and WRHA in cement slurries was evaluated by: thermal-gravimetric technique and derivative thermogravimetry (TGA/DTG), X-ray diffraction (XRD) and Compressive Strength. The slurries formulated with additions of 10% and 20% of RHA and WRHA were cured for 28 days at 58 °C. The results of thermal analysis demonstrated that a 20% WRHA addition caused a reduction of approximately 73% of Portlandite (calcium hydroxide – CH) phase related to standard slurry (STD). The XRD scans also demonstrated the reduction of the Portlandite peaks’ intensity for each slurry compared with STD slurry. The RHA and WRHA react chemically with Portlandite producing calcium silicate hydrate (C-S-H), confirming their effect as a pozzolanic agent. The WRHA presented the best results as a pozzolanic material.
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Brazil is a country in development, rich in natural resources. In order to grow sustainably, it is necessary to Brazil to preserve its environment, which is an expressive challenge, especially to industries, such as those producing ceramic materials. This study was developed using Porcelain Tile Polishing Residue (RPP) in blends with soil to build compacted fills. This residue is a slurry generated during the polishing process of porcelain tiles and contains powdery material from the polished tile, the abrasives used during the process and cooling water. The RPP was collected from a private company located in Conde/PB and it was mixed with a sandy-clayey soil, to build the fills. Laboratorial tests were conducted with pure soil, pure RPP and blends in proportions of 5%, 10%, 15% and 20% of RPP in addition to the dry mass of pure soil. The Chemical and Physical Characterization tests performed were: specific solid weight, grain size distribution, laser analysis of grain size distribution, Atterberg limits, X ray fluorescence, X ray diffraction, scanning electron microscopy and soil compaction,. The materials and blends were also compacted and direct shear tests and plate load tests were performed. Plate load tests were conducted using a circular plate with 30 cm diameter, on specimens of pure soil and 5% blend, compacted in a metallic box inside the Soil Mechanics Laboratory of the Federal University of Rio Grande do Norte, Brazil. Both mechanical tests performed were conducted under inundated conditions, willing to reduce the influence of soil suction. An evaluation of the results of the tests performed shows that RPP is a fine material, with grain size distribution smaller than 0,015mm, composed mainly of silica and alumina, and particles in angular shape. The soil was characterized as a clayey sand, geologically known as a lateritic soil, with high percentages of alumina and iron oxide, and particles with rounded shape. Both the Soil and the blends presented low plasticity, while the residue showed a medium plasticity. Direct shear tests showed that the addition of RPP did not cause major changes into blends’ friction angle data, however, it was possible to note that, for the proportions studied, that is a tendency of obtain lower shear stresses for higher percentages of RPP in the blends. Both pure soil and 5% mixture showed a punching disruption for the Plate load test. For this same test, the allowable stress for 5% mixture was 44% higher than the pure soil, and smaller vertical settlement results for all stresses.
Resumo:
Brazil is a country in development, rich in natural resources. In order to grow sustainably, it is necessary to Brazil to preserve its environment, which is an expressive challenge, especially to industries, such as those producing ceramic materials. This study was developed using Porcelain Tile Polishing Residue (RPP) in blends with soil to build compacted fills. This residue is a slurry generated during the polishing process of porcelain tiles and contains powdery material from the polished tile, the abrasives used during the process and cooling water. The RPP was collected from a private company located in Conde/PB and it was mixed with a sandy-clayey soil, to build the fills. Laboratorial tests were conducted with pure soil, pure RPP and blends in proportions of 5%, 10%, 15% and 20% of RPP in addition to the dry mass of pure soil. The Chemical and Physical Characterization tests performed were: specific solid weight, grain size distribution, laser analysis of grain size distribution, Atterberg limits, X ray fluorescence, X ray diffraction, scanning electron microscopy and soil compaction,. The materials and blends were also compacted and direct shear tests and plate load tests were performed. Plate load tests were conducted using a circular plate with 30 cm diameter, on specimens of pure soil and 5% blend, compacted in a metallic box inside the Soil Mechanics Laboratory of the Federal University of Rio Grande do Norte, Brazil. Both mechanical tests performed were conducted under inundated conditions, willing to reduce the influence of soil suction. An evaluation of the results of the tests performed shows that RPP is a fine material, with grain size distribution smaller than 0,015mm, composed mainly of silica and alumina, and particles in angular shape. The soil was characterized as a clayey sand, geologically known as a lateritic soil, with high percentages of alumina and iron oxide, and particles with rounded shape. Both the Soil and the blends presented low plasticity, while the residue showed a medium plasticity. Direct shear tests showed that the addition of RPP did not cause major changes into blends’ friction angle data, however, it was possible to note that, for the proportions studied, that is a tendency of obtain lower shear stresses for higher percentages of RPP in the blends. Both pure soil and 5% mixture showed a punching disruption for the Plate load test. For this same test, the allowable stress for 5% mixture was 44% higher than the pure soil, and smaller vertical settlement results for all stresses.
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This study aimed to evaluate the potential of oxidative electrochemical treatment coupled with adsorption process using expanded perlite as adsorbent in the removal of textile dyes, Red Remazol and Novacron Blue on synthetic effluent. Dyes and perlite were characterized by thermogravimetry techniques (TG), Differential Scanning Calorimetry (DSC), Spectroscopy infrared (IR), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. Electrochemical treatments used as anodes, Ti/Pt and Pb/PbO2 under different conditions: 60 minutes, current density 20, 40 e 60 mAcm-2, pH 1, 4.5 e 8 and temperature variation 20, 40 e 60 ºC. In the case of adsorption tests, contact time of 30 minutes for the Remazol Red dye and 20 minutes for Novacron Blue were established, while pH 1, 4.5 e 8, 500 mg adsorbent and temperature variation 20, 40 e 60 ºC were used for both treatments. The results indicated that both treatments, electroxidation/adsorption and the adsorption/electroxidation, were effective for removing color from synthetic solutions. The consumption of electricity allowed to evaluate the applicability of the electrochemical process, providing very acceptable values, which allowed us to estimate the cost. Total organic carbon (TOC) and Gas Chromatography linked mass spectrometer (GC-MS) analyzes were performed, showing that the better combination for removing organic matter is by Pb/PbO2 and perlite. Meanwhile, GC-MS indicated that the by-products formed are benzoic acid, phthalic acid, thiocarbamic acid, benzene, chlorobenzene, phenol-2-ethyl and naphthalene when Remazol Red was degraded. Conversely, aniline, phthalic acid, 1, 6 - dimethylnaphthalene, naphthalene and ion hidroxobenzenosulfonat was detected when Novacron Blue was studied. Analyses obtained through atomic absorption spectrometry showed that there was release of lead in the electrochemical oxidation of analyzes that were performed with the anode Pb/PbO2, but these values are reduced by subjecting the effluent to adsorption analysis. According to these results, sequential techniques electroxidation/adsorption and adsorption/electroxidation are to treat solutions containing dyes.
Resumo:
This study aimed to evaluate the potential of oxidative electrochemical treatment coupled with adsorption process using expanded perlite as adsorbent in the removal of textile dyes, Red Remazol and Novacron Blue on synthetic effluent. Dyes and perlite were characterized by thermogravimetry techniques (TG), Differential Scanning Calorimetry (DSC), Spectroscopy infrared (IR), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. Electrochemical treatments used as anodes, Ti/Pt and Pb/PbO2 under different conditions: 60 minutes, current density 20, 40 e 60 mAcm-2, pH 1, 4.5 e 8 and temperature variation 20, 40 e 60 ºC. In the case of adsorption tests, contact time of 30 minutes for the Remazol Red dye and 20 minutes for Novacron Blue were established, while pH 1, 4.5 e 8, 500 mg adsorbent and temperature variation 20, 40 e 60 ºC were used for both treatments. The results indicated that both treatments, electroxidation/adsorption and the adsorption/electroxidation, were effective for removing color from synthetic solutions. The consumption of electricity allowed to evaluate the applicability of the electrochemical process, providing very acceptable values, which allowed us to estimate the cost. Total organic carbon (TOC) and Gas Chromatography linked mass spectrometer (GC-MS) analyzes were performed, showing that the better combination for removing organic matter is by Pb/PbO2 and perlite. Meanwhile, GC-MS indicated that the by-products formed are benzoic acid, phthalic acid, thiocarbamic acid, benzene, chlorobenzene, phenol-2-ethyl and naphthalene when Remazol Red was degraded. Conversely, aniline, phthalic acid, 1, 6 - dimethylnaphthalene, naphthalene and ion hidroxobenzenosulfonat was detected when Novacron Blue was studied. Analyses obtained through atomic absorption spectrometry showed that there was release of lead in the electrochemical oxidation of analyzes that were performed with the anode Pb/PbO2, but these values are reduced by subjecting the effluent to adsorption analysis. According to these results, sequential techniques electroxidation/adsorption and adsorption/electroxidation are to treat solutions containing dyes.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.
Resumo:
Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.
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Cement pastes used in cementing oil wells operations are prepared according to the specific characteristics of each well. The physical properties requested for each folder formulation depend on the temperature and pressure of the well to be cemented. The rheological properties of the pulp are important control parameter for efficiency in transportation and positioning the folder during the cementing operation. One of the main types of additive used for the adjustment of rheological properties of cement pastes is the dispersant additive. This work aims to study the influence of variation of the time of addition of the polycarboxylate (0, 5, 10 and 15 minutes) in cement pastes, considering the initial periods of hydration of cement particles as fundamental point for better performance dispersant additive. Pastes were prepared with a density set at 15.6 lb/gal (1.87 g/cm3) and polycarboxylate concentrations ranging from 0.01 gpc to 0.05 gpc circulation temperature (BHCT) of 51°C and static temperature (BHST) of 76 C. The pastes were characterized from a rheological measurements, volume filtered, thickening time and resistance to compression formulations. Also were carried out tests Diffraction X-ray (XRD) and Scanning Electron Microscopy (MEV). The results showed that the addition of policaboxilato after 15 minutes decreased by 70% the values of rheological parameters. According to results of DRX and MEV, the addition of dispersant after 15 minutes did not affect the chemical reactions and subsequent formation of cement hydration products. A study of the economic feasibility to realize the financial benefits of the technique, which can be seen only with the use of the technique in this work to reduce the cost of production of cement paste was carried out, can get up to $ 1015.00 for each folder 100 barrels produced with said formulations.
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Cement pastes used in cementing oil wells operations are prepared according to the specific characteristics of each well. The physical properties requested for each folder formulation depend on the temperature and pressure of the well to be cemented. The rheological properties of the pulp are important control parameter for efficiency in transportation and positioning the folder during the cementing operation. One of the main types of additive used for the adjustment of rheological properties of cement pastes is the dispersant additive. This work aims to study the influence of variation of the time of addition of the polycarboxylate (0, 5, 10 and 15 minutes) in cement pastes, considering the initial periods of hydration of cement particles as fundamental point for better performance dispersant additive. Pastes were prepared with a density set at 15.6 lb/gal (1.87 g/cm3) and polycarboxylate concentrations ranging from 0.01 gpc to 0.05 gpc circulation temperature (BHCT) of 51°C and static temperature (BHST) of 76 C. The pastes were characterized from a rheological measurements, volume filtered, thickening time and resistance to compression formulations. Also were carried out tests Diffraction X-ray (XRD) and Scanning Electron Microscopy (MEV). The results showed that the addition of policaboxilato after 15 minutes decreased by 70% the values of rheological parameters. According to results of DRX and MEV, the addition of dispersant after 15 minutes did not affect the chemical reactions and subsequent formation of cement hydration products. A study of the economic feasibility to realize the financial benefits of the technique, which can be seen only with the use of the technique in this work to reduce the cost of production of cement paste was carried out, can get up to $ 1015.00 for each folder 100 barrels produced with said formulations.
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The present study aims the characterization of thermally affected carbonate rocks from Jandaíra Formation in contact with Paleogene and Neogene basic intrusions in the region of the Pedro Avelino and Jandaíra municipalities (RN), northeastern Brazil. For this study, field, petrographic, x-ray diffraction, electron microprobe, and whole rock litogeochemistry data of carbonates were undertaken. The thermally unaffected limestones are classified like wackstones, grainstones and packstones. They may constitute carbonates grains of benthic foraminifera, echinoderm spines, ostracods, algae, corals, bivalves, gastropods, peloids and intraclasts. The porosities are classified like vug, intraparticle, interparticle, intercrystal and moldic types. The major minerals are calcite, ankerite and dolomite; the detrital are montmorillonite, pyrite, limonite, quartz and microcline. The thermally affected limestones are very coarse to very fine-grained and light to dark gray color. The fossiliferous components totally disappear, and the porosity tends to disappear. With the data obtained, it can be inferred that the carbonate protoliths would be calciferous to dolomitic limestones, both with small amount of clay minerals. Crystalline carbonates from dolomitic protolith have rhombohedral calcite and iron oxides / hydroxides, making the rocks much darker. The carbonates from calciferous protolith have a wide variation of grain size according to the recrystallization degree, increasing toward contact with the basic bodies. In this group, it was identified the minerals lizardite and spinel in weakly to moderately affected samples, and spinel and spurrite in strongly affected rocks, as well as calcite, that occur everywhere. The geological context (shallow level diabase intrusions), the crystallization of the pyrometamorphic minerals spurrite and olivine, and comparison with diagrams from the literature allow estimating temperatures and pressures around 1050-1200 °C and 0.5-1.0 kbar, respectively, for PTOTAL=PCO2. The post-intrusion cooling would have afforded the releasing of metasomatic / hydrothermal fluids, allowing the opening of the metamorphic system, with possible contribution of chemical elements from host units (sandstones, shales) and from basic intrusions. This would induce hydration of previous phases, allowing the formation of serpentine, chlorite and brucite. The results discussed here reveal the strong influence of the heat from basic intrusions within the sedimentary pile. Whereas in the offshore portion of the basin occur sills with up to 1000 m thickness, the understanding of pyrometamorphism might be useful for understanding and measuring the thermally affected rocks.
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The present study aims the characterization of thermally affected carbonate rocks from Jandaíra Formation in contact with Paleogene and Neogene basic intrusions in the region of the Pedro Avelino and Jandaíra municipalities (RN), northeastern Brazil. For this study, field, petrographic, x-ray diffraction, electron microprobe, and whole rock litogeochemistry data of carbonates were undertaken. The thermally unaffected limestones are classified like wackstones, grainstones and packstones. They may constitute carbonates grains of benthic foraminifera, echinoderm spines, ostracods, algae, corals, bivalves, gastropods, peloids and intraclasts. The porosities are classified like vug, intraparticle, interparticle, intercrystal and moldic types. The major minerals are calcite, ankerite and dolomite; the detrital are montmorillonite, pyrite, limonite, quartz and microcline. The thermally affected limestones are very coarse to very fine-grained and light to dark gray color. The fossiliferous components totally disappear, and the porosity tends to disappear. With the data obtained, it can be inferred that the carbonate protoliths would be calciferous to dolomitic limestones, both with small amount of clay minerals. Crystalline carbonates from dolomitic protolith have rhombohedral calcite and iron oxides / hydroxides, making the rocks much darker. The carbonates from calciferous protolith have a wide variation of grain size according to the recrystallization degree, increasing toward contact with the basic bodies. In this group, it was identified the minerals lizardite and spinel in weakly to moderately affected samples, and spinel and spurrite in strongly affected rocks, as well as calcite, that occur everywhere. The geological context (shallow level diabase intrusions), the crystallization of the pyrometamorphic minerals spurrite and olivine, and comparison with diagrams from the literature allow estimating temperatures and pressures around 1050-1200 °C and 0.5-1.0 kbar, respectively, for PTOTAL=PCO2. The post-intrusion cooling would have afforded the releasing of metasomatic / hydrothermal fluids, allowing the opening of the metamorphic system, with possible contribution of chemical elements from host units (sandstones, shales) and from basic intrusions. This would induce hydration of previous phases, allowing the formation of serpentine, chlorite and brucite. The results discussed here reveal the strong influence of the heat from basic intrusions within the sedimentary pile. Whereas in the offshore portion of the basin occur sills with up to 1000 m thickness, the understanding of pyrometamorphism might be useful for understanding and measuring the thermally affected rocks.
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Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.
Resumo:
Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.