Síntese, caracterização e avaliação catalítica do silicoaluminofosfato SAPO-11 sulfatado

Due to environmental restrictions around the world, clean catalytic technology are of fundamental importance in the petrochemical industry and refineries. Creating the face of this a great interest in replacing the liquid acids for solid acids, so as molecular sieves have been extensively studied in reactions involving the acid catalysis to produce chemical substances with a high potential of quality. Being the activity of the catalysts involved in the reaction attributed to the acid character of them involved for the Lewis and Brönsted acid sites. Based on this context, this study aimed to prepare catalysts acids using a molecular sieve silicoalumino-phosphate (SAPO-11) synthesized in hidrotermical conditions and sulphated with sulphuric acid at different concentrations, using to it the method of controlled impregnating. The samples resulting from this process were characterized by x-ray difratometry (DRX), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), thermal analysis (TG-DTG) and determination of total acidity (by n-butilamin adsorption). The results show that the synthesis method used was efficient in the formation of AEL structure of SAPO-11 and when being incorporated the sulfate groups in this structure the acidity of the material was increased, pointing out that to very high concentrations of acid there is a trend of decrease the main peaks that form the structure. Finally they were tested catalytictly by the reaction model of conversion of m-xylene which showed favorable results of conversion for this catalyst, showing to be more selective of cracking products than isomerization, as expected, in order that for the o-xylene selectivity there was no positive change when to sulfate a sample of SAPO-11, while for light gases of C1-C4 this selectivity was remarkably observed

Estudo da regeneração de aditivos para catalisadores de craqueamento aluminofosfatos (ALPO s)e silicoaluminofosfatos (SAPO s)

Heterogeneous catalysts such as aluminophosphate and silicoaluminophosphate, molecular sieves with AEL of ALPO-11 and SAPO-11, were synthesized by the hydrothermal method with the following molar composition: 2.9 Al +3.2 P + 3.5 DIPA +32.5 H20 (ALPO-11); 2.9 Al +3.2 P + 0.5 Si + 3.5 DIPA +32.5 H20 (SAPO-11) starting from silica (only in the SAPO-11), pseudoboehmite, orthophosphoric acid (85%) and water, in the presence of a di-isopropylamine organic template. The crystallization process occurred when the reactive hydrogel was charged into a vessel and autoclaved at 170ºC for a period of 48 hours under autogeneous pressure. The obtained materials were washed, dried and calcined to remove the molecular sieves of DIPA. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), thermo gravimetric differential thermal analysis (TG/DTA) and nitrogen adsorption (BET). The acidic properties were determined using adsorption of n-butylamine followed by programmed thermodessorption. This method revealed that ALPO-11 has weaker acid sites due to structural defects, while SAPO-11 shows an acidity that ranges from weak to moderate. However, a small quantity of strong acid sites could be detected there. The deactivation of the catalysts was conducted by the cracking of the n-hexane in a fixed bed continuous flow microrreator coupled on line to a gas chromatograph. The main products obtained were: ethane, propane, isobutene, n-butane, n-pentane and isopentane. The Vyazovkin (model-free) kinetics method was used to determine the regeneration and removal of the organic template

Estudo do comportamento térmico e da luminescência de filmes de quitosana com os íons Eu3+ e Tb3+

Films of chitosan with trivalent lanthanides ions Eu3+ and Tb3+ were respectively prepared in the ratio of 3:1 m/m (chitosan: lanthanide) and 6:1 m/m (chitosan: lanthanide). There were no formations of films in a ratio of 1:1 m/m (chitosan: lanthanides). The films of chitosan with the Tb3+ ion have the same transparent appearance than the pure chitosan films. The film of chitosan with Eu3+ ion has a muddy appearance. These films present good resistance to tear. The appearance of the compounds prepared in ratio 1:1m/m is a white powder. The films and compounds of chitosan were characterized by Elementary Analysis (CHN), Thermal Analysis (TG/DTG) and Spectroscopy of Luminescence. The CHN analysis was made only for compounds prepared in ratio 1:1m/m, suggesting that these compounds possess the formula QUILn.6H2O, where QUI = Chitosan and Ln = Lanthanide. The results of the curves TG/DTG indicated that there are strong interactions between Eu3+ or Tb3+ and chitosan, causing a lesser lost of mass in the films. The luminescence analysis showed that the films of chitosan with the ions Eu3+ and Tb3+ present emissions in the region of the visible one, with bands of the chitosan and of the Eu3+ ion. The luminescence analysis of the compounds of chitosan with the Eu3+ and Tb3+ ions suggest that the chitosan does not transfer into energy to the ions lanthanides, however the chemical neighborhood around of the ion lanthanides breaks the selection rules and, conseqüently the 4f-4f transitions of the lanthanide ions are observed

Caracterização de látices acrílicos em função da neutralização de seus grupos carboxilas

Latexes based on acrylic acid, acrylamide, ethyl methacrylate, and ethyl acrylate were synthesized via emulsion polymerization with different monomer compositions. The resultant latices were thickened with different molar ratios of NaOH to acrylic acid and were analyzed in terms of acid‐basis titrimetry, turbidimetry, rheology, and tensiometry. Titrimetry, turbidimetry, and rheometry were used to analyze factors such as carboxyl group availability and particle solubilization, tensiometry monitoring the influence of carboxyl neutralization on polymer‐surfactant interactions. For the acrylic acid content used in this work (20 wt%), the results indicated that as carboxyl groups distribution became more homogeneous, the process of latex thickening became more effective

Reavaliação da eficiência de óleo de coco saponificado e de sua microemulsão como inibidores de corrosão em uma célula eletroquímica

An interesting development in surfactants science and technology is their application as corrosion inhibitors, since they act as protective films over anodic and cathodic surfaces. This work aims to investigate the efficiency of saponified coconut oil (SCO) as corrosion inhibitor and of microemulsified system (SCO + butanol + kerosene oil + distilled water), in saline medium, using an adapted instrumented cell, via techniques involving linear polarization resistance (LPR) and mass loss coupons (MLC). For this, curves of efficiency versus SCO concentration (ranging between 0 and 75 ppm) have been constructed. According to the obtained results, the following efficiency levels were reached with OCS: 98% at a 75 ppm concentration via the LPR method and 95% at 75 ppm via the MLC method. The microemulsified system, for a concentration of 15 ppm of SCO, obtained maximum inhibition of 97% (LPR) and 93% (MLC). These data indicate that it is possible to optimize the use of SCO in similar applications. Previous works have demonstrated that maximal efficiencies below 90% are attained, typically 65% as free molecules and 77% in microemulsified medium, via the LPR method in a different type of cell. Therefore, it can be concluded that the adapted instrumented cell (in those used methods) showed to be an important tool in this kind of study and the SCO was shown effective in the inhibition of the metal

Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)

Síntese análise das propriedades magnéticas da ferrita de NiMg e características de absorção de radiação

It was synthesized different Ni1-xMgxFe2O4 (0,2 ≤ x ≤ 0,7) compositions by use of citrate precursor method. Initially, the precursory citrates of iron, nickel and magnesium were mixed and homogenized. The stoichiometric compositions were calcined from 350°C to 1200°C at ambient atmosphere or in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, magnetic measures and reflectivity using the wave guide method. I was observed pure magnetic phase formation between 350°C and 500°C, with formation of ferrite and hematite after 600°C at ambient atmosphere. The calcined powder at argon atmosphere formed pure ferromagnetic phase at 1100°C and 1200°C. The Rietveld analyses calculated the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (11-66 nm), that at 900°C/3h presents micrometric sizes (0,45 - 0,70 Om). The better magnetization results were 54 Am2/Kg for x= 0,2 composition, calcined at 350°C/3h and 30 min, and 55,6 Am2/Kg for x= 0,2 1200°C, calcined in argon. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The materials presented absorption less or equal the 50 % in ranges specific frequency. As for the 2,0 and 3,0 thickness (in 11,0 - 11,8 GHz), the reflectivity of the x= 0,3, 0,5 and 0,4 compositions, all calcined at 900°C/3h showed agreement with MS and O. Various factors contribute for the final radiation absortion effect, such as, the particle size, the magnetization and the polymer characteristics in the MARE composition. The samples that presented better magnetization does not obtaining high radiation absorption. It is not clear the interrelaction between the magnetization and the radiation absorption in the strip of frequencies studied (8,2 - 12,4 GHz)

Avaliação termoanalítica da eficiência de antioxidantes na estabilidade oxidativa do biodiesel de mamona

The biodiesel is defined as the mono-alkyl ester derived from long-chain fatty acids, from renewable sources such as vegetable oils or animal fat, whose use is associated with the replacement of fossil fuels in diesel engine cycle. The biodiesel is susceptible to oxidation when exposed to air and this process of oxidation affects the quality of fuel, mainly due to long periods of storage. Because of this, the oxidation stability has been the focus of numerous researches since it directly affects the producers, distributors and users of fuel. One of the possibilities to increase the resistance of biodiesel is the autoxidation treatment with inhibitors of oxidation. The antioxidants can be used as potential inhibitors of the effects of oxidation on the kinematic viscosity and the index of acidity of biodiesel, thereby increasing oxidative stability. This work aims to examine the efficiency of antioxidants, α-tocopherol and butylated hydroxy-toluene (BHT), added the biodiesel content of remembrance through Pressurized-Differential Scanning Calorimetry (P-DSC), Thermogravimetry (TG) and Petrology. The results showed that the use of antioxidant BHT, at the concentration of 2000ppm, increased resistance to oxidation of the biodiesel and oxidative induction time (OIT), which is a better result as antioxidant than the α-tocopherol. With the thermogravimetric analysis, it was observed that the biodiesel presented an initial decomposition temperature of lower tendency than that of oil, demonstrating to be more volatile, bearing great similarity to the diesel and being characterized as an alternative fuel. The rheological analysis indicated that each sample of biodiesel behaved as a Newtonian fluid

Obtenção e aplicação de sistemas microemulsionados na recuperação avançada de petróleo

Due to the need of increasing production in reservoirs that are going through production decline, methods of advanced recovery have frequently been used in the last years, as the use of conventional methods has not been successful in solving the problem of oil drifting. In this work, the efficiency of different microemulsionated systems in the flow of oil from cores from Assu and Botucatu formations. Regarding drifting tests, cores were calcinated at a temperature of 1000°C, for 18 hours, with the aim of eliminating any organic compound present in it, increasing the resultant permeability. Following, the cores were isolated with resin, resulting in test specimens with the following dimensions: 3.8 cm of diameter and 8.7 cm of length. Cores were saturated with brine, composed of aqueous 2 wt % KCl, and oil from Guamaré treatment station (Petrobras/RN). A pressure of 20 psi was used in all tests. After core saturation, brine was injected again, followed by oil at constant flow rate. The system S3 - surfactant (anionic surfactant of short chain), isoamillic alcohol, pine oil, and water - presented the best drift efficiency, 81.18%, while the system S1E commercial surfactant, ethyl alcohol, pine oil, and distilled water presented low drift efficiency, 44,68%

Avaliação do comportamento de argila ativada na presença de água destilada, soluções salinas e inibidores de hidratação catiônicos

The clay swelling is today one of the major problems during the well drilling. Nearly 50% of clays that constitute shale expand easily in the presence of water molecules. During the drilling of a geological formation containing swelling clays, when is feasible the use of water base fluids, it is necessary to apply clay inhibitors. This avoids the incorporation of the cutting to the drilling fluid which is responsible for the wall swelling and crumbling. The aim of this work was to evaluate the synergistic behavior that occurs when swelling clay inhibitors are associated to NaCl and KCl salts. Three swelling clay inhibitors samples, INIB A, INIB B and INIB C, were analyzed. Each inhibitor was characterized by the amount of chlorides and active matter content. For the water-clay interaction evaluation in the presence of various fluids, it was used the Capillary Suction Timer (CST, Fann) and Linear Swell Meter (LSM 2000, Fann). For better interpretation of results, a Design of Experiments (DOE, Umetrics MODDE 7.0 TM) through Result Surface Methodology (RSM) was employed, taking into account the type, the swelling inhibitors concentration and the contact time with the clay. The results showed different efficiencies among the inhibitors employed, and the salt-inhibitors mixtures were more efficient than those products alone. However, for field operation, other parameters should be taking into account, as operational cost, environmental requests and time of application for each product

Avaliação do potencial anticorrosivo de tiossemicarbazonas solubilizadas em sistemas microemulsionados

In this work thiosemicarbazones [4-N-cinnamoyl-thiosemicarbazone (CTSC), 4-N-(2'-methoxycinnamoyl)-thiosemicarbazone (MCTSC), and 4-N-(4'-hydroxy-3'-methoxybenzoyl)-thiosemicarbazone (HMBTSC)] were solubilized in an microemulsion system (ME_OCS) which is rich in aqueous phase (O/W system). The system ME_OCS was obtained with saponified coconut oil (OCS) as (surfactant), butanol (cosurfactant), and kerosene as oil phase (Fo), using 40% of C/T (cosurfactant/surfactant), 5% of Fo and 55% of aqueous phase. The microemulsions systems CTSC_ME_OCS, MCTSC_ME_OCS and HMBTSC_ME_OCS effectiveness on a AISI 1020 carbon steel corrosion inhibition process were evaluated in a saline solution (NaCl 0.5%), using a galavostatic method. The tested thiosemicarbazones (TSC) showed highest inhibitors effects (85.7% for CTSC_ME_OCS, 84.0% for MCTSC_ME_OCS, and 83.3% HMBTSC_ME_OCS) at lower concentrations [0.19% of CTSC, 0.07% (MCTSC), and 0.26% (HMBTSC)]. Comparatively, the surfactant OCS (solubilized in H2O) as well as the system ME_OCS showed lower efficacy [71% for OCS (at 0.20 - 0.25% of concentration) and 74% for ME_OCS (at 0.5% of concentration)]. Since the microemulsion systems ME_OCS showed satisfactory interfacial adsorption, the greatest inhibitory effect of those TSC_ME_OCS systems could be correlated to both chemical composition of each tested TSC (which is rich in heteroatoms and aromatic ring) and also the presence of the surfactant OCS

Desenvolvimento de uma metodologia para caracterização de amostras de sedimento: Rio Jundiaí RN

The study of sediment in water bodies presents great environmental importance, because of its ability to adsorb the pollutants, they may facilitate the understanding of the history of the current quality of the water system. Depending on how it is done the collection, analysis can show both a recent contamination as old. The detailed characterization of the sediment may reveal details that can understand how each type of pollutant interacts with the material given its composition. In this work it has developed a systematic methodology to characterize samples of sediment, with the aim to understand how a series of metal is distributed in different size fractions of the sediment. This study was conducted in five samples of sediment (P1, P2, P3a, P3B and P3c) collected in Jundiaí river, one of the most important tributaries of the river Potengi in the region of Macaíba, RN. The characterization was made with the samples previously sieved into meshes with different granulometries (+8#, -8+16#, -16+65# - 65+100#,-100+200#,-200+250# and -250#), using the following techniques: Analysis of specific surface area by BET method, determining the levels of organic matter (OM%) and humidity through the gravimetry and Analysis Thermogravimetric (TG), Infrared Spectroscopy in a Fourier transform (FTIR ), Analysis of X ray diffraction (XRD), analysis of heavy metals by optical emission spectrometry with the Argon Plasma (ICP-OES). The analyzed elements were Al, Cd, Cr, Cu, Fe, Mn, Ni, Zn and P. In addition to the techniques of characterization above, was also made the rebuilding of the samples P1, P2 and P3B in relation to the levels of organic matter and concentration of heavy metals. Then, the results of the recomposed samples were compared with those obtained in crude samples, showing great consistency. The gravimetry, used in determining the levels of organic matter, was not considered an appropriate method because the clay minerals present in the sediment samples analyzed fall apart in the same range of temperature (550-600 0C) used in roasting (600 0C). The results also showed the trend of organic matter and heavy metals to focus on the thin fractions, although the largest concentrations of metals are in intermediate fractions

Hidróxidos duplos lamelares aplicados à obtenção de biodiesel

In this paper, the Layered Double Hydroxides (LDH s) type hydrotalcite were synthesized, characterized and tested as basic heterogeneous catalysts for the production of biodiesel by transesterification of sunflower oil with methanol. The synthesis of materials Layered Double Hydroxides (LDH s) by co-precipitation method from nitrates of magnesium and aluminum, and sodium carbonate. The materials were submitted to the variation in chemical composition, which is the amount of Mg2+ ions replaced by Al3+. This variation affects the characteristic physico-chemical and reaction the solid. The molar ratio varied in the range of 1:1 and 3:1 magnesium / aluminum, and their values between 0.2 and 0.33. This study aims to evaluate the influence of variation of molar ratio of mixed oxides derived from LDH s and the influence of impregnation of a material with catalytic activity, the KI, the rate of conversion of sunflower oil into methyl esters (biodiesel) through transesterification by heterogeneous catalysis. .The catalysts were calcined at 550 ° C and characterized by X-ray diffraction (XRD), scanning electron microscopy and energy dispersive spectroscopy of X-ray (SEM / EDS), thermogravimetric analysis (TG) and test basicity. The transesterification reaction was performed for reflux is a mixture of sunflower oil and methanol with a molar ratio of 15:1, a reaction time of 4h and a catalyst concentration of 2% by weight. The physical-chemical characterization of sunflower oil and biodiesel obtained by the route methyl submitted according NBR, EN, ASTM. Subsequently, it was with the chromatographic and thermogravimetric characterizations of oils. The results of chromatographic analysis showed that the catalysts were effective in converting vegetable oil into biodiesel, in particular the type hydrotalcite KI-HDL-R1, with a conversion of 99.2%, indicating the strong influence of the chemical composition of the material, in special due to presence of potassium in the structure of the catalyst

Diagnóstico ambiental das águas do estuário Jundiaí-Potengi pela determinação dos índices de qualidade da água e toxidez

This study is an environmental diagnosis of the Jundiaí-Potengi/RN estuarine system waters, using calculations of pollution indicator indices such as the Water Quality Index (WQI) and the Toxicity Index (TI). The samples were collected at twelve points on the estuary, at high and low tide, between August and November 2007, over four campaigns. The study area, located in a high impact region, has various activities on its banks such as: discharge of untreated or undertreated domestic and industrial sewage, shrimp farming, immunizer stabilization lakes, riverside communities, etc. All the parameters analyzed were compared to the limits of CONAMA Resolution No. 357 of 2005 for healthy and saline Class 1 waters. The results found prove the impact caused by various activities, mainly the parameters related to the presence of organic material, such as DQO, DBO, COT and thermotolerant colliforms. The IQA for most of the collection points was of medium quality. For the metals, although values above the Resolution limits were found, most of them were lower than the detection limits of ICP-OES used, indicating that they tend to be transported by the dynamic of the tides or rainfall and are deposited in bottom sediments, resulting in a TI of 1.0 in this water, when they are absent, which occurs in most cases, or 0.0, when heavy metals are found in these waters

Síntese, caracterização e aplicação de MCM-41 funcionalizado com diisopropilamina no processo de adsorção do dióxido de carbono

Emissions of CO2 in the atmosphere have increased successively by various mechanisms caused by human action, especially as fossil fuel combustion and industrial chemical processes. This leads to the increase in average temperature in the atmosphere, which we call global warming. The search for new technologies to minimize environmental impacts arising from this phenomenon has been investigated. The capture of CO2 is one of the alternatives that can help reduce emis ions of greenhouse gases. The CO2 can be captured through the process of selective adsorption using adsorbents for this purpose. Were synthesized by hydrothermal method, materials of the type MCM-41 and Al-MCM-41 in the molar ratio Si / Al equal to 50. The synthesis of gels were prepared from a source of silicon, sodium, water and aluminum in the case of Al-MCM-41. The period of synthesis of the materials was 5 days in autoclave at 100°C. After that time materials were filtered, washed and dried in greenhouse at 100 º C for 4 hours and then calcined at 450 º C. Then the calcined material was functionalized with the Di-isopropylamine (DIPA) by the method of wet impregnation. We used 0.5 g of material mesopores to 3.5 mL of DIPA. The materials were functionalized in a closed container for 24 hours, and after this period were dried at brackground temperature for 2 hours. Were subsequently subjected to heat treatment at 250°C for 1 hour. These materials were used for the adsorption of CO2 and were characterized by XRD, FT-IR, BET / BJH, SEM, EDX and TG / DTG. Tests of adsorption of CO2 was carried out under the following conditions: 100 mg of adsorbent, temperature of 75°C under flow of 100 mL/min of CO2 for 2 hours. The desorption of CO2 was carried out by thermogravimetry from ambient temperature to 900ºC under flow of 25 mL min of He and a ratio of 10ºC/min. The difratogramas X-ray for the synthesized samples showed the characteristic peaks of MCM-41, showing that the structure of it was obtained. For samples functionalized there was a decrease of the intensities of these peaks, with a consequent reduction in the structural ordering of the material. However, the structure was preserved mesopores. The adsorption tests showed that the functionalized MCM-41 is presented as a material promising adsorbent, for CO2 capture, with a loss of mass on the desorption CO2 of 7,52%, while that in Al-MCM- 41 functionalized showed no such loss