Aditivação de pastas geopoliméricas com tetraborato de sódio e látex não iônico para cimentação de Poços de Petróleo

The development of activities in the oil and gas sector has been promoting the search for materials more adequate to oilwell cementing operation. In the state of Rio Grande do Norte, the cement sheath integrity tend to fail during steam injection operation which is necessary to increase oil recovery in reservoir with heavy oil. Geopolymer is a material that can be used as alternative cement. It has been used in manufacturing of fireproof compounds, construction of structures and for controlling of toxic or radioactive waste. Latex is widely used in Portland cement slurries and its characteristic is the increase of compressive strength of cement slurries. Sodium Tetraborate is used in dental cement as a retarder. The addition of this additive aim to improve the geopolymeric slurries properties for oilwell cementing operation. The slurries studied are constituted of metakaolinite, potassium silicate, potassium hydroxide, non-ionic latex and sodium tetraborate. The properties evaluated were: viscosity, compressive strength, thickening time, density, fluid loss control, at ambient temperature (27 ºC) and at cement specification temperature. The tests were carried out in accordance to the practical recommendations of the norm API RP 10B. The slurries with sodium tetraborate did not change either their rheological properties or their mechanical properties or their density in relation the slurry with no additive. The increase of the concentration of sodium tetraborate increased the water loss at both temperatures studied. The best result obtained with the addition of sodium tetraborate was thickening time, which was tripled. The addition of latex in the slurries studied diminished their rheological properties and their density, however, at ambient temperature, it increased their compressive strength and it functioned as an accelerator. The increase of latex concentration increased the presence of water and then diminished the density of the slurries and increased the water loss. From the results obtained, it was concluded that sodium tetraborate and non-ionic latex are promising additives for geopolymer slurries to be used in oilwell cementing operation

Novos monômeros obtidos a partir do metacrilato de glicidila, bisfenol A e 4, 4 isopropilidenodicicloexanol : síntese, caracterização estrutural e propriedades de compósitos para utilização em resinas de restauração dental

Nowadays, composite resins are the direct restorative materials more important in dental clinical performance, due to their versatility and aesthetic excellence. Bis-GMA (2,2-bis[4(2-hydroxy-3-metacryloxypropoxy)phenil]propane) is the base monomer more frequently used in restorative composite resins. However, this monomer presents some disadvantages, such as high viscosity and two aromatic rings in its structure that can promote allergic reactions to the humans. In this work, the main purpose was to synthesize new monomers from glycidyl methacrylate to use in dental restorative materials. Structural characterization of the monomers was carried out through FTIR and NMR 1H, and eight composites were produced from the new monomers, by addition of silane-treated alumino silicate particles (inorganic filler) and a photocuring system (camphorquinone and ethyl 4-dimethylaminebenzoate). The composites were analyzed by environmental scanning electronic microscopy and the water sorption and solubility, compressive strength and elastic modulus were determined. A commercial composite resin [Z100 (3M)] was used to comparison effect. The new composites presented general characteristics similar to the commercial ones; however, they didn t present the properties expected. This behavior was attributed to the lower degree of monomer reaction and to the granulometry and size distribution of the mineral filler in the polymeric matrix

Estudo termo-mecânico de interconector metálico recoberto com filme de La0,8Ca0,2CrO3 e de interconector cerâmico de La0,8Sr0,2Cr0,92Co0,08O3 para PaCOS

Doped lanthanum chromite ( LaCrO3 ) has been the most common material used as interconnect in solid oxide fuel cells for high temperature ( SOFC-HT ) that enabling the stack of SOFCs. The reduction of the operating temperature, to around 800 º C, of solid oxide fuel cells enabled the use of metallic interconnects as an alternative to ceramic LaCrO3, From the practical point of view, to be a strong candidate for interconnect the material must have good physical and mechanical properties such as resistance to oxidizing and reducing environments, easy manufacture and appropriate thermo-mechanical properties. Thus, a study on the physic-mechanical interconnects La0,8Sr0,2Cr0,92Co0,08O3 ceramics for SOFC -AT obtained by the method of combustion , as well as thermo-mechanical properties of metallic interconnects (AISI 444) covered with La0,8Ca0,2CrO3 by deposition technique by spray-pyrolysis fuel cells for intermediate temperature (IT-SOFCs). The La0,8Sr0,2Cr0,92Co0,08O3 was characterized by X -ray diffraction(XRD) , density and porosity , Vickers hardness (HV) , the flexural strength at room temperature and 900 °C and scanning electron microscopy (SEM). The X -ray diffraction confirmed the phase formation and LaCrO3 and CoCr2O4, in order 6 GPa hardness and mechanical strength at room temperature was 62 MPa ceramic Interconnector. The coated metal interconnects La0,8Ca0,2CrO3 passed the identification by XRD after deposition of the film after the oxidation test. The oxidative behavior showed increased resistance to oxidation of the metal substrate covered by La0,8Ca0,2CrO3 In flexural strength of the coated metal substrate, it was noticed only in the increased room temperature. The a SEM analysis proved the formation of Cr2O3 and (Cr,Mn)3O4 layers on metal substrate and confirmed the stability of the ceramic La0,8 Ca0,2CrO3 film after oxidative test

Estudo do resíduo fosfogesso na formulação de uma pasta para revestimento interno de edifícios

Universidade Federal do Rio Grande do Norte

Estudo da viabilidade do processo de reciclagem do material descartado do sistema Zirkonzanh® de produção de próteses dentárias

At present, the material of choice for performing aesthetic dental prosthetic work is in the ceramic. Among them, the ceramic base of stabilized zirconia with 3% yttria (3Y - TZP) stand out for having excellent physical and mechanical properties. During the machining of blocks of zirconia in the laboratory to prepare the various types of prostheses, much of the material is given off in the form of powder, which is subsequently discarded. The waste of this material results in financial loss, reflecting higher final cost treatment for patients, as well as damage to the environment, thanks to the processes involved in the manufacture and disposal of the ceramic. This research, pioneered the recycling of zirconium oxide powder obtained during milling of dental crowns and bridges, we highlight the social and environmental aspects and aims to establish a protocol for the reuse of waste (powder of zirconia Zirkonzahn® system) discarded to obtain a new block of compacted zirconia to maintain the same mechanical and microstructural properties of commercial high-cost imported material. To compare with the commercial material, samples were uniaxially (20 MPa) and isostatically (100 MPa), and its mechanical and microstructural characterization was performed through tests of density, porosity, dilatometry, X-ray diffraction (XRD), hardness, fracture toughness, resistance to fracture electron microscopy (SEM) and analysis of grain size. The results observed in the samples were isostatically pressed similiares those obtained with samples from the commercial material demonstrating the viability of the process

Avaliação do efeito da adição de resíduo de borracha de pneu e brita calcária na formulação de compósitos cimentíceos

Researches have shown that the introduction of rubber in concrete improves the features of its deformability, as well as contributes to environmental disposal of waste generated in the tire retreading process. Furthermore, there is a high availability of limestone within RN and CE country. Ignorance about this stone, does not allow its wide use as aggregate, leaving, this abundant supply idle. A composite of limestone gravel, with proportions of tire rubber waste which could be used as concrete would be an alternative to concrete for low applications. Therefore, this research aims to evaluate the characteristics of concrete containing limestone gravel and proportions of little aggregate replacement (sand) by tire rubber waste. To this goal, the material components of the concrete were characterized, concrete specimens with limestone gravel were made, from the dash 1.0: 2.5: 3.5, varying the water/cement ratio, and inserting a commercial plasticizer, without a proportion of residue, known as reference. From this, concrete with and without the presence of the additive in the same proportions were chosen, as well as these with the use of granite gravel, for being the most used. Selected the references, to these, replacements of little aggregate (sand) were added replaced by rubber waste from the tire retreading process, treated with 1M NaOH in proportions from 5.0 to 20.0 % by mass, cured and exposed to the semiarid environment. The results indicate the possibility of using limestone gravel in the concrete composition with workability correction using plasticizer. There was a decrease in the mechanical properties of the concrete with increments of waste rubber, but there is an improvement in toughness and deformability of the composite, which makes it interesting for the construction of non-structural concrete floors, as well as, the rubber waste delayed the hardening process, continuing to gain resistance after 28 days

Plásticos reforçados a base de tecidos híbridos: efeitos da anisotropia e geometria normativa na caracterização mecânica e da fratura

As most current studies, reinforced plastics have been, in recent years, a viable alternative in building structural elements of medium and large, since the lightness accompanied by high performance possible. The design of hybrid polymer composites (combination of different types of reinforcements) may enable structural applications thereof, facing the most severe service conditions. Within this class of composite materials, reinforced the underlying tissues hybrid high performance are taking space when your application requires high load bearing and high rigidity. The objective of this research work is to study the challenges in designing these fabrics bring these materials as to its mechanical characterization and fracture mechanisms involved. Some parameters associated with the process and / or form of hybridization stand out as influential factors in the final performance of the material such as the presence of anisotropy, so the fabric weave, the process of making the same, normative geometry of the specimens, among others. This sense, four laminates were developed based hybrid reinforcement fabrics involving AS4 carbon fiber, kevlar and glass 49-E as the matrix epoxy vinyl ester resin (DERAKANE 411-350). All laminates were formed each with four layers of reinforcements. Depending on the hybrid fabric, all the influencing factors mentioned above have been studied for laminates. All laminates were manufactured industrially used being the lamination process manual (hand-lay-up). All mechanical characterization and study of the mechanism of fracture (fracture mechanics) was developed for laminates subjected to uniaxial tensile test, bending in three and uniaxial compression. The analysis of fracture mechanisms were held involving the macroscopic, optical microscopy and scanning electron microscopy

Estudo de inibidores de corrosão em concreto armado, visando a melhoria na sua durabilidade

This thesis has as objective presents a methodology to evaluate the behavior of the corrosion inhibitors sodium nitrite, sodium dichromate and sodium molybdate, as well as your mixture, the corrosion process for the built-in steel in the reinforced concrete, through different techniques electrochemical, as well as the mechanical properties of that concrete non conventional. The addition of the inhibitors was studied in the concrete in the proportions from 0.5 to 3.5 % regarding the cement mass, isolated or in the mixture, with concrete mixture proportions of 1.0:1.5:2.5 (cement, fine aggregate and coarse aggregate), superplasticizers 2.0 % and 0.40 water/cement ratio. In the modified concrete resistance rehearsals they were accomplished to the compression, consistence and the absorption of water, while to analyze the built-in steel in the concrete the rehearsals of polarization curves they were made. They were also execute, rehearsals of corrosion potential and polarization resistance with intention of diagnose the beginning of the corrosion of the armors inserted in body-of-proof submitted to an accelerated exhibition in immersion cycle and drying to the air. It was concluded, that among the studied inhibitors sodium nitrite , in the proportion of 2.0 % in relation to the mass of the cement, presented the best capacity of protection of the steel through all the studied techniques and that the methodology and the monitoring techniques used in this work, they were shown appropriate to evaluate the behavior and the efficiency of the inhibitors

Efeito da velocidade de aquecimento nas propriedades de produtos da cerâmica estrutural

Heating rate is one of the main variables that determine a fire cycle. In industrial processes that use high temperatures, greater fire great can reduce the cost of production and increase productivity. The use of faster and more efficient fire cycles has been little investigated by the structural ceramic industry in Brazil. However, one of the possibilities that aims at modernizing the sector is the use of roller kilns and the inclusion of natural gas as fuel. Thus, the purpose of this study is to investigate the effect of heating rate on the technological properties of structural ceramic products. Clay raw materials from the main ceramic industries in the state of Rio Grande do Norte were characterized. Some of the raw materials characterized were formulated to obtain the best physical and mechanical properties. Next, raw materials and formulations were selected to study the influence of heating rate on the final properties of the ceramic materials. The samples were shaped by pressing and extrusion and submitted to rates of 1 °C/min, 10 °C/min and 20 °C/min, with final temperatures of 850 °C, 950 °C and 1050 °C. Discontinuous cycles with rates of 10 °C/min or 15 °C/min up to 600 °C and a rate of 20 °C/min up to final temperature were also investigated. Technological properties were determined for all the samples and microstructural analysis was carried out under a number of fire conditions. Results indicate that faster and more efficient fire cycles than those currently in practice could be used, limiting only some clay doughs to certain fire conditions. The best results were obtained for the samples submitted to slow cycles up to 600 °C and fast fire sinterization up to 950 °C. This paper presents for the first time the use of a fast fire rate for raw materials and clay formulations and seeks to determine ideal dough and processing conditions for using shorter fire times, thus enabling the use of roller kilns and natural gas in structural ceramic industries

Redução aluminotérmica do óxido de tântalo usando uma tocha de plasma como ignitor

In this work was used a plasma torch of non transferred arc with argon as work gas, using a power supply with maximum DC current of 250 A and voltage of 30 V to activate the plasma and keep it switched on. The flame temperature was characterized by optical emission spectroscopy, through Boltzmann-plot-method. The torch has been used like igniter in the aluminothermic reduction of the mixture tantalum oxide and aluminum, seeking to obtain metallic tantalum. In heating of the reagents only one particle will be considered to study interactions between plasma-particle, seeking to determinate its fusion and residence time. The early powders were characterized by laser granulometry, scanning electron microscopy (SEM) and X-ray diffraction analysis. The final product of this reaction was characterized by SEM and X-ray diffraction. Crystallite size was calculated by the Scherrer equation and microdeformation was determined using Willamsom-Hall graph. With Rietveld method was possible to quantify the percentile in weight of the products obtained in the aluminothermic reaction. Semi-quantitative chemical analysis (EDS) confirmed the presence of metallic tantalum and Al2O3 as products of the reduction. As was waited the particle size of the metallic tantalum produced, presents values in nanometric scale due the short cooling time of those particles during the process

Alternativas de ultimação de resíduo plástico termofixo

In the present work it was developed originals alternatives of enveronmentally safe and economically viable destination of thermoset plastic residue from a button factory, which at presnte stores such residue tempor and in a way that is inconvenient to the atmosphere, a waiting safe solutions. As the residue is not recycleab and its burning leberates strongly aggressive gases, safe alternatives were researched. Inicially, ghe residue in incineration was performed in cement ovens with precise control ofe emission of gases, but it was proved inviable due to its low calorific power, as well as the liberation of free lead in the ashes. An original and feasible option was the residue confinemente in soil-ciment blocks, lohich resulted in blocks highly resistant to simple compression with structural block, and also a significant increase in thermal resistence. Was got up other options of original and important composites as: making of blocks for pré-moulded flagstone, internal coating of walls with plaster being obtained good texture results, replenish of ceramic blocks and blocks with cement, also implying in increase of thermal resistance. Besides these original and scientific contributions, the it was technologically contribution of defreadation with suggestions of the material using torch of thermal plasm; for this was projected, built, characterized and tested a torch to it shapes it being obtained exciting results for the development of this technology come back for ending destruction from all the types of inconvenient garbage to the atmosphere

Aplicação da metodologia de planejamento de experimentos para formulação de massas cerâmicas para telhas

Rio Grande do Norte State stands out as one great producer of structural clay of the brazilian northeastern. The Valley Assu ceramic tiles production stands out obtained from ilitics ball clays that abound in the region under study. Ceramics formulation and the design of experiments with mixture approach, has been applied for researchers, come as an important aid to decrease the number of experiments necessary to the optimization. In this context, the objective of this work is to evaluate the effects of the formulation, temperature and heating rate in the physical-mechanical properties of the red ceramic body used for roofing tile fabrication of the Valley Assu, using design of mixture experiments. Four clays samples used in two ceramics industry of the region were use as raw material and characterized by X-ray diffraction, chemical composition, differential thermal analysis (DTA), thermogravimetric analysis (TGA), particle size distribution analysis and plasticity techniques. Afterwards, they were defined initial molded bodies and made specimens were then prepared by uniaxial pressing at 25 MPa before firing at 850, 950 and 1050 ºC in a laboratory furnace, with heating rate in the proportions of 5, 10 e 15 ºC/min. The following tecnologicals properties were evaluated: linear firing shrinkage, water absorption and flexural strength. Results show that the temperature 1050 ºC and heating rate of 5 ºC/min was the best condition, therefore presented significance in all physical-mechanical properties. The model was accepted as valid based of the production of three new formulations with fractions mass diferents of the initial molded bodies and heated with temperature at 1050 ºC and heating rate of 5 ºC/min. Considering the formulation, temperature and heating rate as variables of the equations, another model was suggested, where from the aplication of design of experiments with mixtures was possible to get a best formulation, whose experimental error is the minor in relation to the too much formulations

Síntese enzimática de ésteres de açúcar: surfactantes e polímeros como novos materiais ambientalmente seguros

Sugar esters are substances which possess surfactant, antifungical and bactericidal actions and can be obtained through two renewable sources of raw materials: sugars and vegetable oils. Their excellent biodegradability, allied to lhe fact that they are non toxic, insipid, inodorous, biocompatible, no-ionic, digestible and because they can resist to adverse conditions of temperature, pH and salinity, explain lhe crescent use of these substances in several sections of lhe industry. The objective of this thesis was to synthesize and characterize surfactants and polymers containing sugar branched in their structures, through enzymatic transesterification of vinyl esters and sugars, using alkaline protease from Bacillus subtilis as catalyst, in organic medium (DMF).Three types of sugars were used: L-arabinose, D-glucose and sucrose and two types of vinyl esters: vinyl laurate and vinyl adipate. Aiming to reach high conversions from substrates to products for a possible future large scale industrial production, a serie of variables was optimized, through Design of Experiments (DOE), using Response Surface Methodology (RSM).The investigated variables were: (1) enzyme concentration; (2) molar reason of substrates; (3) water/solvent rale; (4) temperature and (5) time. We obtained six distinct sugar esters: 5-0-lauroyl L-arabinose, 6-0-lauroyl D-glucose, 1'-O-lauroyl sucrose, 5-0-vinyladipoyl L-arabinose, 6-0-vinyladipoyl D-glucose and 1 '-O-vinyladipoyl sucrose, being lhe last three polymerizable. The progress of lhe reaction was monitored by HPLC analysis, through lhe decrease of sugar concentration in comparison to lhe blank. Qualitative analysis by TLC confirmed lhe formation of lhe products. In lhe purification step, two methodologies were adopted: (1) chromatographic column and (2) extraction with hot acetone. The acylation position and lhe chemical structure were determined by 13C-RMN. The polymerization of lhe three vinyl sugar esters was possible, through chemical catalysis, using H2O2 and K2S2O8 as initiators, at 60°C, for 24 hours. IR spectra of lhe monomers and respective polymers were compared revealing lhe disappearance of lhe vinyl group in lhe polymer spectra. The molar weights of lhe polymers were determined by GPC and presented lhe following results: poly (5-0-vinyladipoyl L-arabinose): Mw = 7.2 X 104; PD = 2.48; poly (6-0-vinyladipoyl D-glucose): Mw = 2.7 X 103; PD = 1.75 and poly (1'-O-vinyladipoyl sucrose): Mw = 4.2 X 104; PD = 6.57. The six sugar esters were submitted to superficial tension tests for determination of the critical micelle concentrations (CMC), which varied from 122 to 167 ppm. Finally, a study of applicability of these sugar esters, as lubricants for completion fluids of petroleum wells was' accomplished through comparative analysis of lhe efficiency of these sugar esters, in relation to three commercial lubricants. The products synthesized in this thesis presented equivalent or superior action to lhe tested commercial products

Estudo de Matérias-Primas do Rio Grande do Norte para Uso em Revestimento Poroso: Influência do teor de dolomita e temperatura de calcinação nas propriedades físico-mecânicas

The state of Rio Grande do Norte presents a great potentiality for the production of ceramic tiles because of having natural raw material in quantity and quality making its economical exploration possible, beyond the great energetic differential of the state, the natural gás. This works aims to study the influence of the dolomite and granulometry concentration and calcinations temperature in the obtaining of formulations for porous coverings which have to be coherent to the project,s specifications. The experiments have involved the physical-chemical and mineralogical characterizations of raw materials and mechanical tests in the dry and burnt proof bodies preceding a mixture experiment planning with the use of the response surface methodology, in order to get the best raw materials combinations to produce a ceramic mass with specific properties. The twelve ceramic masses studied in this work were prepared by the via dry process, characterized, shaped by uniaxial pressing and sinterized in the temperatures of 940ºC, 1000ºC, 1060ºC, 1120ºC and 1180ºC, using a fast burning cycle. The crystalline phases formed during the sintering in the temperatures in study have revealed the presence of anorthite and diopside beyond quartz with a remaining phase. These phases were the main responsible ones by the physical- mechanical properties of the sinterized proof bodies. The proof bodies after the sintering stage have presented water absorption higher than 10% and a good dimensional stability in all studied temperatures. However, the flexural breaking strength results in the temperatures of 940ºC, 1000ºC and 1060ºC, under the temperature zone of the vitrification of ceramic whiteware do not reach the flexural breaking strength specific for the porous wall tile (15 MPa), but in the temperature of 1120ºC next to the vitrification temperature zone, some whiteware ceramic (formulations) has reached the specified value for the porous wall tile. The results of this work have showed that the studied raw materials have great importance for used in the production of porous wall tiles (BIII)

Influência da substituição de areia natural por pó de pedra no comportamento mecânico, microestrutural e eletroquímico de concretos

The construction industry is one of the largest consumers of natural raw materials, and concrete is considered today the most used material wide. This accentuated consumption of natural resources has generated concern with the preservation of the environment, and has motivated various studies related to the use of resid ues, which can partially or entirely substitute, with satisfactory performance, some materials such as the aggregate, and in so doing, decrease the impact on the environment caused by the produced residues. Research has been done to better understand and improve the microstructure of concrete, as well as to understand the mechanism of corrosion in reinforced steel. In this context, this work was developed aiming at discovering the influence of the substitution of natural sand by artificial sand, with rega rd to mechanical resistance, microstructure, and durability. To obtain the electrochemical parameters, an adaptation was made to the galvanostatic electrochemical method to study the corrosion in reinforced steel. Concretes of categories 20 MPa and 40 MPa were produced, containing natural sand, and concretes of the same categories were produced with artificial sand substituting the natural sand, and with the addition of sodium nitrate and sodium chloride. Due to the use of rock dust reject (artificial sand), an evaluation was made of its environmental risk. The results indicate that the concretes of category 20 MPa present a better performance than the concrete made with natural sand, thus making it a viable substitute. For the category 40 MPa, the better performance is from the concrete containing natural sand. The adaptation of the galvanostatic electrochemical technique to the study of the corrosion of reinforced steel within concrete proved to be valid for obtaining electrochemical parameters with a high degree of reliability, considering the number of degrees of freedom