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

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

Síntese e caracterização de compostos de coordenação do Ácido 4-cloro-2-(2- furilmetilamino)-5- sulfamoil-benzóico com os íons níquel, cobalto e zinco

This work aimed to promote the synthesis, characterization and propose a plausible molecular structure for coordination compounds involving furosemide (4-Chloro-2-(2- furylmethylamino)-5-sulfamoyl-benzoic acid) with the metal ions Ni+2, Zn+2 and Co+2. The compounds were obtained in methanoic medium by evaporation of the solvent after the synthesis procedure. For characterization of coordination compounds determining the levels of metals by EDTA complexometry, infrared spectroscopy (FTIR), solubility of compounds in various solvents, thermogravimetry (TG), differential scanning calorimetry (DSC), differential thermal analysis were made (DTA), determination of the carbon , hydrogen and nitrogen (CHN). The results of infrared spectroscopy in the region suggest that the organic ligand is coordinated in a bidentate fashion to the metal ions, the metal center interactions to occur by the coordination of the nitrogen atom of the amino group and the oxygen atom of the carboxylic acid of the structure of furosemide. With the results of the levels of metal, elemental analysis (CHN) and thermal analysis has been possible to propose the structure of the ligand. The values of the molar conductivity of the complex in acetonitrile behavior suggest the non acetonitrile electrolyte solution. With the solubility tests it was found that the compounds have high solubility in methanol and acetonitrile, as are partially insoluble in water. From the results of thermal analysis (TG, DSC, DTA), it was possible to obtain the thermal behavior of the compounds as stages of dehydration, thermal stability, decomposition and the energies involved.

Aplicação da perlita expandida modificada com ortofenantrolina na remoção do negro de eriocromo T em águas residuais geradas em laboratórios de ensino de química

In this study, we carried out the study of Eriochrome black T removal using expanded perlite modified orthophenanthroline by adsorption technique. The study of the adsorption process was performed by investigating the effect of the initial dye concentration, contact time and pH range of the solution (acidic and alkaline) in the adsorption process, for a so-called synthetic effluent (aqueous solution of black eriochrome T) and a real effluent (generated from the test for determining the water hardness, by complexation titration). The materials were characterized by Thermogravimetry / Differential Thermal Analysis (TG / DTA), absorption spectroscopy in the infrared (IR), X-ray Diffraction (XRD) and scanning electron microscopy (SEM). By analysis of XRD observed thinking on orthophenanthroline the modified expanded perlite. And by IR analysis showed an increase in intensity and a detailed enlargement of the absorption band related to the axial deformation of the OH bond of silanol groups of perlite (Si-OH). In the equilibration time of the study, in the evaluated time range (5-230 min) was not possible to observe the existence of a balance of time, probably attributed to the type of interaction between the Eriochrome black-T and the expanded perlite modified orthophenanthroline, being an interaction of surface origin. In the study effect of the initial concentration of the adsorbate in the case 2,0x10-4 mol / L natural pH (pH 5) gave the highest removal percentage value of eriochrome T black color with 63.74 % removal in 20 minutes of contact. In evaluating the effect of varying the pH of Eriochrome black T solution in the adsorption process, it was found that the more acidic the environment, the greater the percentage stain removal, being a result of acid-base interaction between the adsorbate and the adsorbent. In T Eriochrome black removal study in real effluent we used the optimized conditions by studying with synthetic sewage. The dye removal at pH 10, natural pH of the effluent was no significant reaching the maximum amount of color removal percentage of 8.12%, obtained already at pH 3 with maximum color removal 100.00% of color, once more proving that eriochrome black T and effectively interact better with the adsorbent at acid pH values (pH 5 or 3), and most efficiently at pH 3. thus one can mention that the perlite expanded (an amorphous aluminosilicate naturally acid) modified with orthophenanthroline (one Bronsted base) consists of a master and effective removal of coloring material in the acid-type aqueous solution, the conditions expressed in this study, can be applied as an adsorbent of this dye also mums real effluent.

Elucidação molecular e micelar dos superagregados de anfotericina B

A Anfotericina B (AmB) é amplamente utilizada no tratamento de infecções fúngicas sistêmicas. No entanto, a sua utilização é limitada devido a sua elevada toxicidade aguda e crônica. Os superagregados de AmB (H-AmB) obtido pelo processo de aquecimento controlado apresentam um potencial reduzido de toxicidade quando comparados à Anfotericina B micelar não aquecida (M-AmB). Diante do exposto, o objetivo deste estudo foi avaliar as características físico-químicas do processo de formação dos superagregados após a liofilização do H-AmB, por meio de técnicas tais como a calorimetria de exploratória diferencial (DSC), termogravimetria (TG) e análise térmica diferencial (DTG), ressonância magnética nuclear (RMN), espalhamento dinâmico de luz (DLS) e difração de raios X (DRX). Os dados de DLS indicaram um tamanho de aproximadamente 260 nm deste novo sistema, sendo este tamanho compatível e viável para administração intravenosa. A análise de DRX demonstrou a formação de um novo estado cristalino do sistema micelar, podendo este estar relacionado a presença de grande proporção de desoxicolato de sódio (NaDC) na formulação. O aquecimento do NaDC resulta na formação de uma estrutura helicoidal intermolecular, promovendo desta forma o aumento da agregação micelar e consequentemente aumento de seu tamanho. Os estudos das análises térmicas demonstraram que o processo de aquecimento não influência no comportamento das amostras. Os dados de RMN da H-AmB demonstraram a presença de ácido desoxicólico além do NaDC. O ácido desoxicólico é formado após o processo de aquecimento e sugere-se que o equilíbrio entre ambas as moléculas seja responsável pela redução da toxicidade da AmB. Os resultados aqui apresentados sugerem que o processo de aquecimento controlado altera a organização estrutural das micelas, resultando na diminuição da toxicidade, na melhoria da estabilidade térmica e na manutenção da atividade.

Elucidação molecular e micelar dos superagregados de anfotericina B

A Anfotericina B (AmB) é amplamente utilizada no tratamento de infecções fúngicas sistêmicas. No entanto, a sua utilização é limitada devido a sua elevada toxicidade aguda e crônica. Os superagregados de AmB (H-AmB) obtido pelo processo de aquecimento controlado apresentam um potencial reduzido de toxicidade quando comparados à Anfotericina B micelar não aquecida (M-AmB). Diante do exposto, o objetivo deste estudo foi avaliar as características físico-químicas do processo de formação dos superagregados após a liofilização do H-AmB, por meio de técnicas tais como a calorimetria de exploratória diferencial (DSC), termogravimetria (TG) e análise térmica diferencial (DTG), ressonância magnética nuclear (RMN), espalhamento dinâmico de luz (DLS) e difração de raios X (DRX). Os dados de DLS indicaram um tamanho de aproximadamente 260 nm deste novo sistema, sendo este tamanho compatível e viável para administração intravenosa. A análise de DRX demonstrou a formação de um novo estado cristalino do sistema micelar, podendo este estar relacionado a presença de grande proporção de desoxicolato de sódio (NaDC) na formulação. O aquecimento do NaDC resulta na formação de uma estrutura helicoidal intermolecular, promovendo desta forma o aumento da agregação micelar e consequentemente aumento de seu tamanho. Os estudos das análises térmicas demonstraram que o processo de aquecimento não influência no comportamento das amostras. Os dados de RMN da H-AmB demonstraram a presença de ácido desoxicólico além do NaDC. O ácido desoxicólico é formado após o processo de aquecimento e sugere-se que o equilíbrio entre ambas as moléculas seja responsável pela redução da toxicidade da AmB. Os resultados aqui apresentados sugerem que o processo de aquecimento controlado altera a organização estrutural das micelas, resultando na diminuição da toxicidade, na melhoria da estabilidade térmica e na manutenção da atividade.

Avaliação da potencialidade de argilas do Rio Grande do Norte – Brasil

DUTRA, Ricardo Peixoto Suassuna ; SILVA, Jaquelígia Brito da ; MORAES, Márcio Luiz Varela Nogueira de ; NASCIMENTO, R. M. ; GOMES, Uilame Umbelino ; PASKOCIMAS, Carlos Alberto . Avaliação da potencialidade de argilas do Rio Grande do Norte. Cerâmica Industrial, v. 13, p. 47-50, 2008.

Avaliação da dolomita funcionalizada para remoção de H2S em gás natural

The natural gas is an alternative source of energy which is found underground in porous and permeable rocks and being associated or not to the oil. Its basic composition includes methane, other hydrocarbon and compounds such as carbon dioxide, nitrogen, sulphidric gas, mercaptans, water and solid particles. In this work, the dolomite mineral, a double carbonate of calcium and magnesium whose the chemical formula is CaMg(CO3)2, was evaluated as adsorbent material. The material was characterized by granulometric analysis, X-ray fluorescence, X-ray diffraction, thermogravimetric analysis, differential thermal analysis, specific surface area, porosity, scanning electronic microscopy and infrared spectroscopy. Then the material was functionalized with diethanolamine (dolomite+diethanolamine) and diisopropylamine (dolomite+diisopropylamine). The results indicated that the adsorbents presented appropriate physiochemical characteristics for H2S adsorption. The adsorption tests were accomplished in a system coupled to a gas chromatograph and the H2S monitoring in the output of the system was accomplished by a pulsed flame photometric detector (PFPD). The adsorbents presented a significant adsorption capacity. Among the analyzed adsorbents, the dolomite+diethanolamine presented the best capacity of adsorption. The breakthrough curves obtained proved the efficiency of this process

Desenvolvimento de formulações para produção de grés porcelanato a partir de matérias-primas da região da bacia do Parnaíba

Brazil is a great ceramic raw materials productor because of the its big number of clay deposits, in various areas of the ceramic industry. Although, the majority of the natural reservations are unknown or not studied yet, so there is no scientific technical dates that can guide their usage and industrial application, as well as the racional and optimazed way of usage by the industrial sector. The state of Maranhão has a gigant mineral wealth as esmectite, bentonite, kaolin, clays, feldspates, marine salt, iron and others, but produce only products with small agregated value compared to the porcelanato, one of the most expensives ceramic cover tiles, the reason for that is the low water absorption (lower than 0,5%), beside present amazing tecnicals features, like mechanical resistence. The main objective of the work is to do the characterization of four clays, with the finallity of find an application by the results and develop formulations to produce porcelanato using these raw materials from Timon-MA. For this were made the raw materials characterization using X ray fluorecence; X ray diffraction; Differencial thermal analysis; Dilatometric analysis and Tecnological properties, planing three formulations that were sinterized at six different temperatures: 1150, 1170, 1190, 1210, 1230 and 1250ºC for 7 minutes. After the sinteratization, the samples were submitted to tension resistance analysis. Were attained two formulations with the requested properties to produce porcelanato

Formulação e caracterização de matérias-primas para revestimento cerâmico Semi-Poroso com adição de chamote de telhas

The ceramics industry in Piauí is nowadays with 55 industries where 11 are in Teresina which is the mainstream of the state, producing 55 million shingles; in which 10 % is of this production is wasted being sometimes thrown on the margins of rivers, roads and highways provoking an environmental degradation. The main goal of this work is to verify the potential of producing semi porous ceramic using grog of shingles, on the first part of this work bodies-of-proof were produced from a basic formula of an industry, doping it with 5 %, 10 %, 15 % and 20 % in mass and in the second part of this work some bodies-of-proof were produced from a formula where one raw material was substituted by 50 % of grog and another substituting it all by grog, bodies-of-proof made of a basic formula previously announced was used for experiment control.The grog and the raw materials were characterized by: particle size analysis , thermal differential analysis, X ray diffraction , X ray fluorescence, an thermal gravimetric analysis and rational analyses. The bodies-of-proof were sintetisized in an industrial oven obeying the normal cycle adopted by an industry, with peak temperatures of 1135 oC and a fast burning cycle of 25 minutes having as energetic fuel liquefied petroleum gas . The pieces that were obtained by this were submersed in rehearsed physics of: water absorption of, apparent specific mass, apparent porosity, lineal retraction, rupture tension to the flexural and dilatometry; mineralogical analysis for X ray diffraction; and microstructural for electronic microscope of sweeping. For all the formulas with addition of grog, superior priorities to the requested by the requirements for semi porous and for the formula to F2-2,5 superior priorities to standard formulas which justifies the incorporation of the shingles in mass for the semi porous ceramic

Caracterização de atapulgita visando aplicação para reforço de materiais poloméricos

The clay mineral attapulgite is a group of hormitas, which has its structures formed by microchannels, which give superior technological properties classified the industrial clays, clays of this group has a very versatile range of applications, ranging from the drilling fluid for wells oil has applications in the pharmaceutical industry. Such properties can be improved by activating acid and / or thermal activation. The attapulgite when activated can improve by up to 5-8 times some of its properties. The clay was characterized by X-ray diffraction, fluorescence, thermogravimetric analysis, differential thermal analysis, scanning electron microscopy and transmission electron microscopy before and after chemical activation. It can be seen through the results the efficiency of chemical treatment, which modified the clay without damaging its structure, as well as production of polymer matrix composites with particles dispersed atapugita

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

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

Estudo da adição do resíduo proveniente da extração de minério de ferro em argilas do Rio Grande do Norte

The mining industry is responsible for the generation of waste from their natural process of extraction. The mining impacts in urban areas are of special importance due to the high urban occupation, which are exacerbated due to the proximity of the mined areas and populated areas. Some solutions to wastedisposal have the potential to significantly reduce the environmental risks and liabilities, but represent higher costs in the stages of deployment and operation. The addition of mining waste as raw material in the development of commercial products reduces the environmental impacts, transforming the waste into a positive element in the generation of employment and income. This thesis studies the incorporation of waste iron ore in two clays, one from the ceramic industry of the City of Natal and the other from the ceramic industry of the Seridó Region, both in the State of Rio Grande do Norte, Brazil. Percentages of iron ore waste of 5%, 10% , 15%, 20%, 25% and 30% were used in the tested ceramic matrix. The two clays and the iron ore waste used as part of this investigation were characterized by X-ray diffraction tests, X-ray fluorescence tests, differential thermal analysis, thermogravimetric analysis and dilatometric analysis. The samples were sintered under temperatures of 850 °C, 950 °C and 1050°C at a heating rate of 5 °C/min with isotherms of two hours. The following tests were performed with the samples: linear shrinkage, water absorption, apparent porosity, apparent density, mass loss in fire and bending resistance in order to obtain their physical and mechanical properties. An amount of 5% of waste iron ore in the matrix clay at a temperature of 850 0C resulted in na increase of about 65% in the tensile strength of the clay samples from the Natal ceramic industry. A linear shrinkage of only 0.12% was observed for the samples, which indicates that the physical properties of the final product were not influenced by the addition of the waste

Obtenção de uma porcelana dielétrica a partir de matérias-primas do Rio Grande do Norte

The dielectric porcelain is usually obtained by mixing various raw materials proportions and is used in the production of electronic equipment for various applications, from capacitors of high and low Power to insulators for low, medium, high and extra high voltage, which are used in distribution lines and transmission of electricity.This work was directed to the s tudy of technological properties of technic porcelain, made from raw materials extracted from pegmatites found in the regions of Seridó and the Alto Oeste of Rio Grande do Norte, which are made of kaolin, quartz and feldspar, abundant and high quality in these regions. The technic ceramics were obtained by mixing in appropriate levels, kaolin, feldspar, quartz and clay, the last item from a pottery in the city of Sao Gonçalo do Amarante, Rio Grande do Norte. During the development the following characterizations correlated to raw materials were made: laser particle sizing, x-ray diffraction, DTA and TG. The compositions studied were formed by uniaxial pressing at a pressure of 50 MPa and sintered at temperatures ranging from 1150 to 1350ºC and levels (times) of sintering between 30, 60, 90 and 120 minutes. The characterization of the samples were taken from the analysis of weight loss, linear shrinkage, porosity, stoneware curve, bulk density, flexural strength of three points, SEM and X-ray diffraction, TMA, Dielectric and cross Resistivity. The studied materials can be employed in producing the objects used in electrical engineering such as: insulators for low, medium and high-voltage electrical systems, command devices, bushing insulation for transformers, power capacitors, spark plugs, receptacles for fluorescent and incandescent light bulbs and others

Estudo de massa cerâmica triaxial visando à otimização do ciclo de queima da indústria de cerâmica estrutural

Over recent years the structural ceramics industry in Brazil has found a very favorable market for growth. However, difficulties related to productivity and product quality are partially inhibiting this possible growth. An alternative for trying to solve these problems and, thus, provide the pottery industry the feasibility of full development, is the substitution of firewood used in the burning process by natural gas. In order to contribute to this process of technological innovation, this paper studies the effect of co-use of ceramic phyllite and kaolin waste on the properties of a clay matrix, verifying the possible benefits that these raw materials can give to the final product, as well as the possibility of such materials to reduce the heat load necessary to obtain products with equal or superior quality. The study was divided into two steps: characterization of materials and study of formulations. Two clays, a phyllite and a residue of kaolin were characterized by the following techniques: laser granulometry, plasticity index by Atterberg limits, X-ray fluorescence, X-ray diffraction, mineralogical composition by Rietveld, thermogravimetric and differential thermal analysis. To study the formulations, specifically for evaluation of technological properties of the parts, was performed an experimental model that combined planning involving a mixture of three components (standard mass x phyllite x kaolin waste) and a 23 factorial design with central point associated with thermal processing parameters. The experiment was performed with restricted strip-plot randomization. In total, 13 compositional points were investigated within the following constraints: phyllite ≤ 20% by weight, kaolin waste ≤ 40% by weight, and standard mass ≥ 60% by weight. The thermal parameters were used at the following levels: 750 and 950 °C to the firing temperature, 5 and 15 °C/min at the heating rate, 15 and 45min to the baseline. The results showed that the introduction of phyllite and/or kaolin waste in ceramic body produced a number of benefits in properties of the final product, such as: decreased absorption of water, apparent porosity and linear retraction at burn; besides the increase in apparent specific mass and mechanical properties of parts. The best results were obtained in the compositional points where the sum of the levels of kaolin waste and phyllite was maximal (40% by weight), as well as conditions which were used in firing temperatures of 950 °C. Regarding the prospect of savings in heat energy required to form the desired microstructure, the phyllite and the residue of kaolin, for having small particle sizes and constitutions mineralogical phases with the presence of fluxes, contributed to the optimization of the firing cycle.

Efeito da tecnologia de microondas nas propriedades tecnológicas dos componentes de cerâmica estrutural

O processamento térmico de materiais cerâmicos via energia de microondas, no estágio atual, vem ganhando cada dia mais importância, tendo em vista suas inúmeras aplicações, como por exemplo: aplicação de microondas na área de processamento mineral (aquecimento de minérios antes da moagem, secagem, redução carbotérmica de óxidos minerais, lixiviação, fusão, pré-tratamento de minérios e concentrados de ouro refratário, regeneração de carvão, etc. de acordo com Kigman & Rowson, 1998). Em virtude de uma série de vantagens em potencial, frente aos métodos convencionais de aquecimento, como redução no tempo de processamento; economia de energia; diminuição do diâmetro médio das partículas e melhoramento nas propriedades tecnológicas em geral, esta tecnologia vem se destacando. Neste contexto, o objetivo geral deste trabalho, é desenvolver uma pesquisa visando identificar e caracterizar novas opções de matérias-primas cerâmicas como argilas, feldspatos e caulins que sejam eficazes para definir a formulação de uma ou mais massas para produção de componentes de cerâmica estrutural com propriedades físicas, mecânicas e estéticas adequadas após passarem por sinterização convencional e por energia de microondas destacando as vantagens desta última. Além dos requisitos técnicos e de processo, as formulações apresentadas deverão atender às expectativas de preço e de logística de fornecimento. No estudo foram conformados corpos-de-prova por extrusão e prensagem, sinterizados em fornos microondas e convencional, sob ciclos de queima mais rápidos que os atualmente praticados. As matérias-primas foram caracterizadas e analisadas, utilizando as técnicas de fluorescência por raios X (FRX), difração por raios X (DRX), análise térmica diferencial (DTA), análise térmica gravimétrica (DTG), análise granulométrica (AG), microscopia eletrônica de varredura (MEV), absorção d agua (AA), massa especifica aparente (MEA), porosidade aparente (PA), retração linear (RL) e tensão de ruptura e flexão (TRF). Os resultados obtidos indicaram que as propriedades tecnológicas de Absorção de água (AA) e Tensão de Ruptura e flexão (TRF), proposto no trabalho foram adquiridos com sucesso e estão bem além do limite exigido pelas especificações das normas da ABNT NBR 15.270/05 e 15.310/09