Validação de uma metodologia de ensaio de resistência ao cisalhamento para avaliação da aderência de interfaces revestimento metálico-bainha de cimento aplicada a poços de petróleo

Improving the adherence between oilwell metallic casing and cement sheath potentially decrease the number of corrective actions present/y necessary for Northeastern wells submitted to steam injection. In addition to the direct costs involved in the corrective operations, the economic impact of the failure of the primary cementing aIso includes the loss in the production of the well. The adherence between casing and cement is current/y evaluated by a simple shear tests non standardized by the American Petroleum Institute (API). Therefore, the objective of the present is to propose and evaluate a standardized method to assess the adherence of oilwell metallic casing to cement sheath. To that end, a section of a cemented oilwell was simulated and used to test the effect of different parameters on the shear stress of the system. Surface roughness and different cement compositions submitted or not to thermal cycling were evaluated. The results revealed that the test geometry and parameters proposed yielded different values for the shear stress of the system, corresponding to different adherent conditions between metallic casing and cement sheath

Superação da dormência de sementes de carrapicho-beiço-de-boi

Visando a obtenção de um tratamento para acelerar a germinação de sementes de Desmodium tortuosum (Sw.) DC., foram realizados dois experimentos, nos quais, segmentos unisseminados de lomentos (testemunha) foram submetidos a debulha manual; debulha manual seguida por escarificação manual empregando-se lixa n. 220; debulha mecânica (processador doméstico ); escarificação química com H2SO4 (95%) por 1,5 e 8 mim pré-aquecimento à 53°C por 4,10 e 16h em estufa com circulação forçada de ar; embebição, utilizando-se H,0 à 80°C por 1,3,5 e 10 min; H20 à 27°C por 2h e embebição com alternância térmica (H,0 à 80°C/ 5min e H20 à 13 °C / 1min) . Para a avaliação dos tratamentos foram empregados os testes de germinação, de emergência de plântulas em solo (E), de primeira contagem de germinação (PG) e de emergência (PE), índices de velocidade de germinação (I.V.G.) e de emergência (I.V.E.), e o comprimento de plântulas (CP). 0 delineamento estatístico adotado foi o inteiramente casualizado com 4 repetições de 100 (G, PG, I.V.G.) ou 20 sementes (C P) por tratamento no primeiro experimento e 4 repetições de 50 (G, PG, I.V.G.) ou 100 sementes (E, PE, I.V.E.) no segundo experimento. No primeiro experimento, os tratamentos que provocaram significativa redução da dormência (D) e, conseqüente elevação da germinação (G), em comparação à testemunha (D=82%; G=15%) foram, em ordem decrescente de eficácia: debulha e escarificação manuais (D=3%; G= 92%), debu lha mecânica (D=13%; G= 81%), embebição em H20 à 80°C por 1min (D=68%; G= 29%) e por 3 min (D=65%; G=32%). No segundo experimento, (testemunha com D=93% e G=3%) destacaram-se: debulha e escarificação manuais (D=2%; G= 93%), debulha mecânica (D = 2%; G = 87%), embebição em H20 à 80°C por 5min e alternância térmica (ambos com D=85% e G= 11%). 0s testes de vigor PC, I.V. G., I.V. E., CP, e E corroboraram esses resultados. 0s métodos de escarificação manual com lixa 220 e debulha mecânica, empregando-se processa dor, podem ser recomendados para a superação da dormência e promoção da germinação de sementes de D. tortuosum.

Extração e pirólise do óleo de girassol (Helianthus annus l.) visando a produção de biocombustíveis

Nowadays, the growing environmental worry leads research the focus the application of alternative materials from renewable resources on the industrial process. The most common vegetable oil extractant using around the world is the hexane, a petroleum derived, toxic and flammable. Based on this fact, the goal of this work was to test vegetable oil extractions from sunflower seeds cultivated on the Rio Grande do Norte State using two extraction process, the mechanical expelling and solvent extraction, this one using hexane and ethanol as a alternative solvent. The solvent extractions were carried out in the Soxhlet extractor in three different extraction times (4, 6, and 8 hours). The effect of solvent and extraction time was evaluated. The mechanical extraction was carried out in a expeller and the sunflower oil obtained was characterized by its physical-chemical properties and compared with sunflower refinery oil. Furthermore this work also explored the pyrolysis reaction carried out by thermogravimetry measurement as alternative route to obtain biofuel. For this purpose the oil samples were heated to ambient temperature until 900°C in heating rate of 5, 10, 20ºC min-1 with the objective evaluated the kinetics parameters such activation energy and isoconversion. The TG/DTG curves show the thermal profile decomposition of triglycerides. The curves also showed that antioxidant presents on the refinery oil not influence on the thermal stability of sunflower oil. The total yield of the extraction s process with hexane and ethanol solvent were compared, and the results indicated that the extraction with ethanol were more efficient. The pyrolysis reaction results indicated that the use of unpurified oil required less energy to obtain the bio-oil

Síntese e caracterização do carbeto de molibdênio nanoestruturado para fins catalíticos na reação de oxidação parcial do metano

The nanostructures materials are characterized to have particle size smaller than 100 nm and could reach 1 nm. Due to the extremely reduced dimensions of the grains, the properties of these materials are significantly modified relatively when compared with the conventional materials. In the present work was accomplished a study and characterization of the molybdenum carbide, seeking obtain it with particles size in the nanometers order and evaluate its potential as catalyst in the reaction of partial methane oxidation. The method used for obtaining the molybdenum carbide was starting from the precursor ammonium heptamolybdate of that was developed in split into two oven, in reactor of fixed bed, with at a heating rate of 5ºC/min, in a flow of methane and hydrogen whose flow was of 15L/h with 5% of methane for all of the samples. The studied temperatures were 350, 500, 600, 650, 660, 675 and 700ºC and were conducted for 0, 60, 120 and 180 minutes, and the percent amount and the crystallite size of the intermediate phases were determined by the Rietveld refinement method. The carbide obtained at 660ºC for 3 hours of reaction showed the best results, 24 nm. Certain the best synthesis condition, a passivating study was accomplished, in these conditions, to verify the stability of the carbide when exposed to the air. The molybdenum carbide was characterized by SEM, TEM, elemental analysis, ICP-AES, TG in atmosphere of hydrogen and TPR. Through the elemental analysis and ICP-AES the presence carbon load was verified. TG in atmosphere of hydrogen proved that is necessary the passivating of the molybdenum carbide, because occur oxidation in room temperature. The catalytic test was accomplished in the plant of Fischer-Tropsch of CTGAS, that is composed of a reactor of fixed bed. Already the catalytic test showed that the carbide presents activity for partial oxidation, but the operational conditions should be adjusted to improve the conversion

Influência do estresse nutricional programado na composição da microalga isochrysis galbana

Global warming due to Greenhouse Gases (GHG) emissions, especially CO2, has been identified as one of the major problems of the twenty-first century, considering the consequences that could represent to planet. Currently, biological processes have been mentioned as a possible solution, especially CO2 biofixation due to association microalgae growth. This strategy has been emphasized as in addition to CO2 mitigation, occurs the production of biomass rich in compounds of high added value. The Microalgae show high photosynthetic capacity and growth rate higher than the superior plants, doubling its biomass in one day. Its culture does not show seasons, they grow in salt water and do not require irrigation, herbicides or pesticides. The lipid content of these microorganisms, depending on the species, may range from 10 to 70% of its dry weight, reaching 90% under certain culture conditions. Studies indicate that the most effective method to promote increased production of lipids in microalgae is to induce stress by limiting nitrogen content in the culture medium. These evidences justify research continuing the production of biofuels from microalgae. In this paper, it was studied the strategy of increasing the production of lipids in microalgae I. galbana with programmed nutritional stress, due to nitrogen limitation. The physiological responses of microalgae, grown in f / 2 with different concentrations of nitrogen (N: P 15,0-control, N: 5,0 P and N: P 2,5) were monitored. During exponential phase, results showed invariability in the studied conditions. However the cultures subjected to stress in stationary phase, showed lower biomass yields. There was an increase of 32,5% in carbohydrate content and 87.68% in lipids content at N: P ratio of 5,0 and an average decrease of 65% in protein content at N: P ratios of 5, 0 and 2.5. There were no significant variations in ash content, independently of cultivation and growth phase. Despite the limitation of biomass production in cultures with N: P smaller ratios, the increase of lipid accumulation highest lipids yields were observed as compared to the control culture. Given the increased concentration of lipids associated to stress, this study suggests the use of microalgae Isochrysis galbana as an alternative raw material for biofuel production

Aplicação de ultrassons no deslocamento de petróleo em meio poroso

The objective of this study was to evaluate the displacement of petroleum/diesel solutions, at different concentrations, observing the effect of ultrasonic vibrations in fluids present in porous media to obtain an increase in oil production. The bubbles produced by ultrasound implode asymmetrically in the rock, generating liquid jets with high speed, displacing the oil present in porous media. The oil/diesel solutions were prepared with concentrations ranging from 20 g/L to 720 g/L in oil in relation to diesel and its viscosities were obtained in a Brookfield Rheometer RS2000, with temperature ranging from 25 to 55 °C. After, calculations were performed to obtain the activation energy data for oil/diesel solutions. For oil recovery experiments, cylindrical samples of porous rock (core samples), with resin around the perimeter and its two circular bases free to allow the passage of fluids, were first saturated with 2% KCl solution and after with oil solutions. The results of oil extraction were satisfactory for all studied solutions, being obtained up to 68% partial displacement with saline solution injection. The ultrasound system was used after saline injection, increasing oil displacement, with oil extractions ranging from 63% to 79%. During the experiments, it was observed the warming of core samples, helping to reduce the viscosity of more concentrated systems, and consequently enhancing the percentage of advanced recovery for all studied solutions

Estudo de um sistema híbrido de destilação solar para polimento de águas produzidas

The oil industry, experiencing a great economic and environmental impact, has increasingly invested in researches aiming a more satisfactory treatment of its largest effluent, i.e., produced water. These are mostly discarded at sea, without reuse and after a basic treatment. Such effluent contains a range of organic compounds with high toxicity and are difficult to remove, such as polycyclic aromatic hydrocarbons, salts, heavy metals, etc.. The main objective of this work was to study the solar distillation of produced water pre-treated to remove salts and other contaminants trough of a hybrid system with a pre-heater. This developed apparatus was called solar system, which consists of a solar heater and a conventional distillation solar still. The first device consisted of a water tank, a solar flat plate collector and a thermal reservoir. The solar distillator is of simple effect, with 1m2 of flat area and 20° of inclination. This dissertation was divided in five steps: measurements in the solar system, i.e. temperatures and distillate flow rate and weather data; modeling and simulation of the system; study of vapor-liquid equilibrium of the synthetic wastewater by the aqueous solution of p-xylene; physical and chemical analyses of samples of the feed, distillate and residue, as well as climatology pertinent variables of Natal-RN. The solar system was tested separately, with the supply water, aqueous NaCl and synthetic oil produced water. Temperature measurements were taken every minute of the thermal reservoir, water tank and distillator (liquid and vapor phases). Data of solar radiation and rainfall were obtained from INPE (National Institute for Space Research). The solar pre-heater demonstrated to be effective for the liquid systems tested. The reservoir fluid had an average temperature of 58°C, which enabled the feed to be pre-heated in the distillator. The temperature profile in the solar distillator showed a similar behavior to daily solar radiation, with temperatures near 70°C. The distillation had an average yield of 2.4 L /day, i.e., an efficiency of 27.2%. Mathematical modeling aided the identification of the most important variables and parameters in the solar system. The study of the vapor-liquid equilibrium from Total Organic Carbon (TOC) analysis indicated heteroazeotropia and the vapor phase resulted more concentrated in p-xylene. The physical-chemical analysis of pH, conductivity, Total Dissolved Solids (TDS), chlorides, cations (including heavy metals) and anions, the effluent distillate showed satisfactory results, which presents a potential for reuse. The climatological study indicates the region of Natal-RN as favorable to the operation of solar systems, but the use of auxiliary heating during periods of higher rainfall and cloud cover is also recommended

Estudo da influência da temperatura na degradação termoquímica da biomassa de avelós

The bio-oil obtained from the pyrolysis of biomass has appeared as inter-esting alternative to replace fossil fuels. The aim of this work is to evaluate the influence of temperature on the yield of products originating from the pyrolysis process of the powder obtained from the dried twigs of avelós (Euphorbia tirucalli), using a rotating cylinder reactor in laboratory scale. The biomass was treated and characterized by: CHNS, moisture, volatiles, fixed carbon and ashes, as well as evaluation of lignin, cellulose and hemicellulose, besides other instrumental techniques such as: FTIR, TG/DTG, DRX, FRX and MEV. The activation energy was evaluated in non-isothemichal mode with heating rates of 5 and 10 oC/min. The obtained results showed biomass as feedstock with potential for biofuel production, because presents a high organic matter content (78,3%) and fixed-carbon (7,11%). The activation energy required for the degradation of biomass ranged between 232,92 392,84 kJ/mol, in the temperature range studied and heating rate of 5 and 10°C/min. In the pyrolysis process, the influence of the reaction temperature was studied (350-520 ° C), keeping constant the other variables, such as, the flow rate of carrier gas, the centrifugal speed for the bio-oil condensationa, the biomass flow and the rotation of the reactor. The maximum yield of bio-oil was obtained in the temperature of 450°C. In this temperature, the results achieved where: content of bio-oil 8,12%; char 32,7%; non-condensed gas 35,4%; losts 23,8%; gross calorific value 3,43MJ/kg; pH 4,93 and viscosity 1,5cP. The chromatographic analysis of the bio-oil produced under these conditions shows mainly the presence of phenol (17,71%), methylciclopentenone (10,56%) and dimethylciclopentenone (7,76%)

Estudo da influência da temperatura na degradação termoquímica da biomassa de avelós (euphorbia tirucalli Linn)

The bio-oil obtained from the pyrolysis of biomass has appeared as inter-esting alternative to replace fossil fuels. The aim of this work is to evaluate the influence of temperature on the yield of products originating from the pyrolysis process of the powder obtained from the dried twigs of avelós (Euphorbia tirucalli), using a rotating cylinder reactor in laboratory scale. The biomass was treated and characterized by: CHNS, moisture, volatiles, fixed carbon and ashes, as well as evaluation of lignin, cellulose and hemicellulose, besides other instrumental techniques such as: FTIR, TG/DTG, DRX, FRX and MEV. The activation energy was evaluated in non-isothemichal mode with heating rates of 5 and 10 oC/min. The obtained results showed biomass as feedstock with potential for biofuel production, because presents a high organic matter content (78,3%) and fixed-carbon (7,11%). The activation energy required for the degradation of biomass ranged between 232,92 392,84 kJ/mol, in the temperature range studied and heating rate of 5 and 10°C/min. In the pyrolysis process, the influence of the reaction temperature was studied (350-520 ° C), keeping constant the other variables, such as, the flow rate of carrier gas, the centrifugal speed for the bio-oil condensationa, the biomass flow and the rotation of the reactor. The maximum yield of bio-oil was obtained in the temperature of 450°C. In this temperature, the results achieved where: content of bio-oil 8,12%; char 32,7%; non-condensed gas 35,4%; losts 23,8%; gross calorific value 3,43MJ/kg; pH 4,93 and viscosity 1,5cP. The chromatographic analysis of the bio-oil produced under these conditions shows mainly the presence of phenol (17,71%), methylciclopentenone (10,56%) and dimethylciclopentenone (7,76%)

Preparação de poliuretana à base de óleo de mamona

Polyurethanes are very versatile macromolecular materials that can be used in the form of powders, adhesives and elastomers. As a consequence, they constitute important subject for research as well as outstanding materials used in several manufacturing processes. In addition to the search for new polyurethanes, the kinetics control during its preparation is a very important topic, mainly if the polyurethane is obtained via bulk polymerization. The work in thesis was directed towards this subject, particularly the synthesis of polyurethanes based castor oil and isophorone diisocianate. As a first step castor oil characterized using the following analytical methods: iodine index, saponification index, refraction index, humidity content and infrared absorption spectroscopy (FTIR). As a second step, test specimens of these polyurethanes were obtained via bulk polymerization and were submitted to swelling experiments with different solvents. From these experiments, the Hildebrand parameter was determined for this material. Finally, bulk polymerization was carried out in a differential scanning calorimetry (DSC) equipment, using different heating rates, at two conditions: without catalyst and with dibutyltin dilaurate (DBTDL) as catalyst. The DSC curves were adjusted to a kinetic model, using the isoconversional method, indicating the autocatalytic effect characteristic of this class of polymerization reaction

Estudo da reidratação do feijão verde (Vigna unguiculata L. Walp) desidratado por micro-ondas com e sem pré-tratamento osmótico

The green bean has organoleptic and nutritional characteristics that make it an important food source in tropical regions such as the Northeast of Brazil. It is a cheap source of protein and important for nutrition of rural population contributing significantly in subsistence farming of the families from Brazil s northeast. It is consumed in entire region and together with the dry meat and other products composes the menu of typical restaurants, being characterized as an important product for economy of Northeast. The green bean is consumed freshly harvested and has short cycle, being characterized as a very perishable food, which hampers your market. The drying method is an alternative to increase the lifetime and provide a reduction volume of this product making easier your transportation and storage. However is necessary to search ways of drying which keep the product quality not only from the nutritional standpoint but also organoleptic. Some characteristics may change with the drying process such as the coloring, the rehydration capacity and the grains cooking time. The decrease of drying time or of exposure of the grains to high temperature minimizes the effects related with the product quality loss. Among the techniques used to reduce the drying time and improve some characteristics of the product, stands out the osmotic dehydration, widely used in combined processes such as the pretreatment in drying food. Currently the use of the microwaves has been considered an alternative for drying food. The microwave energy generates heat inside of materials processed and the heating is practically instantaneous, resulting in shorter processing times and product quality higher to that obtained by conventional methods. Considering the importance of the green beans for the Northeast region, the wastefulness of production due to seasonality of the crop and your high perishability, the proposal of this thesis is the study of drying grain by microwaves with and without osmotic pretreatment, focusing on the search of conditions of processes which favor the rehydration of the product preserving your organoleptic characteristics. Based on the analysis of the results of osmotic dehydration and dielectric properties was defined the operating condition to be used in pretreatment of the green bean, with osmotic concentration in saline solution containing 12,5% of sodium chloride, at 40°C for 20 minutes. The drying of green bean by microwave was performed with and without osmotic pretreatment on the optimized condition. The osmotic predehydration favored the additional drying, reducing the process time. The rehydration of dehydrated green bean with and without osmotic pretreatment was accomplished in different temperature conditions and immersion time according to a factorial design 22, with 3 repetitions at the central point. According to results the better condition was obtained with the osmotically pretreated bean and rehydrated at a temperature of 60°C for 90 minutes. Sensory analysis was performed comparing the sample of the green bean in natura and rehydrated in optimized conditions, with and without osmotic pretreatment. All samples showed a good acceptance rate regarding the analyzed attributes (appearance, texture, color, odor and taste), with all values above 70%. Is possible conclude that the drying of green bean by microwave with osmotic pretreatment is feasible both in respect to technical aspects and rehydration rates and sensory quality of the product

Obtenção de emulsões asfálticas modificadas utilizando resíduos industriais

The main objective of this research was the development and characterization of conventional and modified cationic asphalt emulsions. The asphalt emulsions were developed by using the Petroleum Asphalt Cement (CAP 50-70) from Fazenda Belém (Petrobras -Aracati-Ce). The first step in this research was the development of the oil phase (asphalt + solvent) and the aqueous phase (water + emulsifying agent + acid + additives), separately. During the experiments for the obtaining of the conventional asphalt emulsion, the concentration of each constituent was evaluated. For the obtaining of the oil phase, kerosene was used as solvent at 15 and 20 wt.%. For the development of the aqueous phase, the emulsifying agent was used at 0.3 and 3.0 wt.%, whereas the acid and the additive were set at 0.3 wt.%. The percentage of asphalt in the asphalt emulsion was varied in 50, 55, and 60 wt.% and the heating temperature was set at 120 °C. The aqueous phase in the asphalt emulsion was varied from 16.4 to 34.1 wt.% and the heating temperature was set at 60 °C. After the obtaining of the oil and the aqueous phases, they were added at a colloidal mill, remaining under constant stirring and heating during 15 minutes. Each asphalt emulsion was evaluated considering: sieve analysis, Saybolt Furol viscosity, pH determination, settlement and storage stability, residue by evaporation, and penetration of residue. After the characterization of conventional emulsions, it was chosen the one that presented all properties in accordance with Brazilian specifications (DNER-EM 369/97). This emulsion was used for the development of all modified asphalt emulsions. Three polymeric industrial residues were used as modifier agents: one from a clothing button industry (cutouts of clothing buttons) and two from a footwear industry (cutouts of sandals and tennis shoes soles), all industries located at Rio Grande do Norte State (Brazil).The polymeric residues were added into the asphalt emulsion (1 to 6 wt.%) and the same characterization rehearsals were accomplished. After characterization, it were developed the cold-mix asphalts. It was used the Marshall mix design. For cold-mix asphalt using the conventional emulsion, it was used 5, 6 and 7 wt.% asphalt emulsion. The conventional mixtures presented stability values according Brazilian specification (DNER-369/97). For mixtures containing asphalt modified emulsions, it was observed that the best results were obtained with emulsions modified by button residue

Evolução microestrutural da cerâmica KSr2Nb5O15 dopada com CuO:B2O3

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of lentil tannins on albumin hydrolysis by trypsin

Os taninos da casca da semente de lentilha foram extraídos e purificados, levados à interação com albumina isolada de lentilha e com caseína; e estudados por turbidimetria. As interações da albumina e caseína com taninos purificados, a várias relações tanino-proteína, mostraram ser independente e dependente do pH, respectivamente. Hidrólise in vitro com tripsina das proteínas sem taninos indicou que o aquecimento a 99°C/15 min reduzia a susceptibilidade da albumina e aumentava a da caseína à tripsina. A influência de diferentes relações tanino:proteína (1:40; 1:20; 1:5; 1:2,5) na hidrólise mostrou maior inibição para caseína que para albumina de lentilha, independente de aquecimento. Após aquecimento ambas proteínas foram mais hidrolizadas para qualquer das relações tanino proteínas estudadas. A eletroforese em gel de poliacrilamida-dodecilsulfato de sódio do transcurso da hidrólise da interação tanino-albumina nativa mostra a dependência da relação tanino:proteína.

Caracterização e hidrólise in vitro da globulina principal de grão-de-bico (Cicer arietinum L.), var. IAC-Marrocos

No presente estudo procedeu-se ao isolamento e caracterização da fração globulina majoritária (11 S) de grão-de-bico, var. IAC-Marrocos. A globulina majoritária extraída foi isolada por cromatografia de filtração em gel e de troca-iônica mostrando apenas uma banda de proteína na eletroforese em gel de poliacrilamida. A globulina majoritária, após passagem em coluna de Sephadex, revelou duas bandas protéicas de 55 e 52,5kDa e três bandas menores em gel de poliacrilamida dodecilsulfato de sódio. Na presença de 2-mercaptoetanol 6 polipeptídios na faixa de 18 a 42kDa foram revelados na eletroforese. A globulina isolada foi submetida à ação da tripsina e quimotripsina onde a forma nativa mostrou-se resistente à ação enzimática enquanto o aquecimento (96 e 121°C/15min) não foi suficiente para aumentar a susceptibilidade à hidrólise, significativamente. Adição de NaCl 0,3M levou a um aumento da estabilidade estrutural com menor susceptibilidade à digestão proteolítica, fato em parte perdido com o aquecimento. As hidrólises foram acompanhadas por eletroforese em gel de poliacrilamida dodecilsulfato de sódio.