Investigação da reatividade e da cinética de dissolução do metacaulim em ácido sulfúrico

Um estudo da reatividade e da cinética de dissolução do metacaulim foi desenvolvido para o caulim de cobertura de papel oriundo da região do Rio Capim, Pará. O caulim foi calcinado a 600, 700, 800, 900 e 1000 ºC por 2 h para obtenção do metacaulim e posteriormente lixiviado com ácido sulfúrico em temperaturas constantes dentro do intervalo 50-95 °C ± 3 °C. Nas lixiviações foram usadas quantidades de ácido sulfúrico correspondentes a 10% acima do valor estequiométrico em relação ao alumínio presente no material. Foram coletadas amostras, com intervalos pré-determinados a cada 15 min até tempo total de 3 h, as quais foram submetidas à análise de teor de alumínio pelo método titrimétrico com EDTA. Os resultados mostraram que a reatividade do caulim calcinado diminuiu com o aumento da temperatura de calcinação e que a cinética de dissolução do alumínio do metacaulim obtido por calcinação a 700 °C seguiu os métodos de reação homogênea utilizados: método integral, método das meia-vidas e método das velocidades iniciais. Uma energia de ativação de 96,25 kJ/mol foi encontrada bem como reação de lixiviação de primeira ordem em relação ao alumínio do metacaulim e de primeira ordem em relação à concentração ácida. Pesquisas realizadas anteriormente, utilizando excesso de um dos reagentes acima de 90% e modelos de reação heterogênea, estão em consonância com os dados encontrados neste trabalho desenvolvido com excesso de apenas 10%.

Desenvolvimento de processos de síntese de sodalita a partir de rejeitos de caulins da região Amazônica

No estudo da síntese de Sodalita foram utilizados dois rejeitos de caulins provenientes de duas empresas de beneficiamento de caulim para cobertura de papel, localizadas na região Amazônica, que operam na região do Rio Capim (CRC) e do Rio Jari (CRJ). Além desses rejeitos, também foi utilizado como fonte de alumina e sílica o metacaulim, obtida através da calcinação dos caulins (MRC e MRJ, respectivamente). Dessa forma, para obter informações das suas características foram realizadas análises químicas e mineralógicas destes caulins. A síntese da Sodalita foi realizada variando alguns parâmetros, como material de partida: partindo-se diretamente de caulim nas temperaturas de 80, 100, 120 e 150 °C; e, partindo-se de metacaulim na temperatura de 95 °C. Posteriormente, as sínteses foram realizadas variando-se as soluções básicas a fim de verificar a influencia da presença dos íons OH^-, Cl^- e CO₃^2-, bem como a influencia da relação Na₂O/Al₂O₃ na síntese, com a temperatura fixa em 95 ºC para o material de partida MRC. Verificou-se ainda, a influência da temperatura de síntese variando as em 85, 90 e 95 °C, fixando-se a relação Na₂O/Al₂O₃ na mistura reacional para determinar as condições ótimas de síntese de Sodalita. Os materiais de partida e os produtos de síntese foram identificados e caracterizados através de DRX, FRX, MEV, ATD/TG e EIV. O método de síntese que apresentou melhor resultado foi utilizou o metacaulim como material de partida, com solução NaOH + Na₂CO₃ apresentando relação Na₂O/Al₂O₃de 3,89 conduzida sob agitação, a 95°C, pressão atmosférica e tempo de 4 horas, para os dois tipos de caulins (CRC e CRJ). A utilização do metacaulim MRC, a partir do caulim do Rio Capim, nas condições mencionadas acima obteve-se a conversão de 86,5% em massa de Sodalita, e o metacaulim MRJ, caulim do Rio Jari, a conversão foi de 73,6% em sodalita. No que se refere ao tamanho de poros, os produtos partindo de metacaulim tanto do Rio Capim quanto do Rio Jari foram caracterizados como materiais mesoporosos, porém o produto partindo de metacaulim do Rio Jari apresentou maior área especifica.

Sedimentação coluvial pleistocênica na região de Presidente Figueiredo, nordeste do estado do Amazonas

Depósitos coluviais pleistocênicos são descritos e datados na região de Presidente Figueiredo, Estado do Amazonas. O estudo sedimentológico-estratigráfico de afloramentos, integrado com análise geomorfológica e datação por luminescência opticamente estimulada, permitiu caracterizar a arquitetura e litofácies destas sucessões sedimentares e fornecer informações sobre a história da denudação e modificações da paisagem da Amazônia Central durante o Pleistoceno. Os depósitos coluviais consistem em areias e, principalmente, cascalhos com arcabouço aberto, matriz arenosa, acamamento maciço e, localmente, gradação inversa, sugestivos de deposição por fluxos gravitacionais e torrenciais, em condições de alta energia. Dois tipos de depósitos coluviais foram identificados: Depósito coluvial tipo 1, datado em 57.000±5.000 anos AP, que é composto por cascalhos e areias com fragmentos de pelito, crosta laterítica e arenito ferruginizado, recobrindo rochas do Eopaleozóico; e Depósito coluvial tipo 2, datado em 22.100±2.600 anos AP, que consiste em cascalhos com fragmentos de caulim semi-flint e crosta laterítica, encontrado principalmente sobre os depósitos siliciclásticos caulínicos da Formação Alter do Chão, do Cretáceo-Terciário (?). A composição dos fragmentos indica como fontes as rochas fanerozóicas intemperizadas e os paleossolos lateríticos bauxítico-ferruginosos que foram removidos durante a denudação dos platôs. Os dois eventos de coluviação descritos aqui parecem confirmar que as fases principais de geomorfogênese seriam correlatas às duas fases climáticas secas e de recuo da floresta registradas para o final do Pleistoceno na Amazônia.

Síntese, caracterização e avaliação biológica de quelatos metálicos contendo ligantes de origem natural

O trabalho que será aqui apresentado teve como finalidade reunir os resultados obtidos dentro do Laboratório de Organometálicos II em relação aos estudos realizados acerca da interação de íons metálicos com ligantes orgânicos naturais. Os dados apresentados foram obtidos pela autora deste trabalho, e também pelos professores Francisco Otávio Cintra Ferrarini, José Roberto Stefanelli Junior e pela aluna de Iniciação Científica Angélica Romão Carvalho. Hidrolisado proteico de soro de leite bovino e torta de linhaça foram os materiais obtidos, após uma série de operações que envolveram filtração com caulim, diálise, hidrólise enzimática, liofilização, etc., após as quais foram utilizados neste trabalho como ligantes de origem natural. Os metais de transição cobre, ferro, cobalto, zinco, paládio, platina e prata foram utilizados nas reações de complexação com os hidrolisados para obtenção de complexos metálicos, através do uso de diferentes rotas sintéticas (convencional, micro-ondas, hidrotérmica, difusão) e parâmetros experimentais (pH, solvente, natureza do precursor, etc.). A escolha dos íons metálicos baseou-se no interesse em preparar compostos que apresentassem ao mesmo tempo alta biodisponibilidade, baixa citotoxicidade e diversas aplicações biológicas. O uso do cobalto deveu-se à reconhecida propriedade que os micro-organismos do sistema digestório dos ruminantes apresenta de sintetizar a vitamina B12 e, portanto, os compostos desse metal podem ser usados em rações visando um melhor desenvolvimento do animal. O ferro, conhecidamente, é um importante metal para os seres humanos, estando presente na hemoglobina, sendo assim, também consiste em uma substância nutracêutica de relevado interesse. À propósito, cabe salientar que os compostos de ferro (III) obtidos nesse trabalho serão objeto de avaliação do uso como suplemento alimentar, em colaboração com o Departamento de...

Síntese, caracterização e avaliação biológica de quelatos metálicos contendo ligantes de origem natural

O trabalho que será aqui apresentado teve como finalidade reunir os resultados obtidos dentro do Laboratório de Organometálicos II em relação aos estudos realizados acerca da interação de íons metálicos com ligantes orgânicos naturais. Os dados apresentados foram obtidos pela autora deste trabalho, e também pelos professores Francisco Otávio Cintra Ferrarini, José Roberto Stefanelli Junior e pela aluna de Iniciação Científica Angélica Romão Carvalho. Hidrolisado proteico de soro de leite bovino e torta de linhaça foram os materiais obtidos, após uma série de operações que envolveram filtração com caulim, diálise, hidrólise enzimática, liofilização, etc., após as quais foram utilizados neste trabalho como ligantes de origem natural. Os metais de transição cobre, ferro, cobalto, zinco, paládio, platina e prata foram utilizados nas reações de complexação com os hidrolisados para obtenção de complexos metálicos, através do uso de diferentes rotas sintéticas (convencional, micro-ondas, hidrotérmica, difusão) e parâmetros experimentais (pH, solvente, natureza do precursor, etc.). A escolha dos íons metálicos baseou-se no interesse em preparar compostos que apresentassem ao mesmo tempo alta biodisponibilidade, baixa citotoxicidade e diversas aplicações biológicas. O uso do cobalto deveu-se à reconhecida propriedade que os micro-organismos do sistema digestório dos ruminantes apresenta de sintetizar a vitamina B12 e, portanto, os compostos desse metal podem ser usados em rações visando um melhor desenvolvimento do animal. O ferro, conhecidamente, é um importante metal para os seres humanos, estando presente na hemoglobina, sendo assim, também consiste em uma substância nutracêutica de relevado interesse. À propósito, cabe salientar que os compostos de ferro (III) obtidos nesse trabalho serão objeto de avaliação do uso como suplemento alimentar, em colaboração com o Departamento de...

0.1T magnetic resonance image in the study of experimental hydrocephalus in rats. Accuracy of the method in the measurements of the ventricular size

PURPOSE: To investigate the accuracy of 1.0T Magnetic Resonance Imaging (MRI) to measure the ventricular size in experimental hydrocephalus in pup rats. METHODS: Wistar rats were subjected to hydrocephalus by intracisternal injection of 20% kaolin (n=13). Ten rats remained uninjected to be used as controls. At the endpoint of experiment animals were submitted to MRI of brain and killed. The ventricular size was assessed using three measures: ventricular ratio (VR), the cortical thickness (Cx) and the ventricles area (VA), performed on photographs of anatomical sections and MRI. RESULTS: The images obtained through MR present enough quality to show the lateral ventricular cavities but not to demonstrate the difference between the cortex and the white matter, as well as the details of the deep structures of the brain. There were no statistically differences between the measures on anatomical sections and MRI of VR and Cx (p=0.9946 and p=0.5992, respectively). There was difference between VA measured on anatomical sections and MRI (p<0.0001). CONCLUSION: The parameters obtained through 1.0T MRI were sufficient in quality to individualize the ventricular cavities and the cerebral cortex, and to calculate the ventricular ratio in hydrocephalus rats when compared to their respective anatomic slice.

Uso da cinza do bagaço da cana-de-açúcar como matéria-prima na substituição dos fundentes para aplicações em porcelanato

The present study aims to evaluate the potential use of bagasse ash from sugar cane (CBC) as a flux, replacing phyllite and/or feldspar in standard industrial mass production of enameled porcelain, verifying the possibility of the CBC contribute to the overall reduction of the coefficient of thermal expansion of the ceramic mass. To this end, as a result of the research, we characterized the raw material components of the standard mass (clay, phyllite, kaolin, feldspar, quartz and talc) and the residue of BCC, by testing by XRF, XRD, AG, DTA and ATG. Specimens (CDP) were manufactured in the dimensions of 100 mm x 50 mm x 8 mm in uniaxial matrix under compaction pressure of 33 MPa, assembled in batches of 3 units subsequently sintered at temperatures of 1150°C to 1210°C by varying the Rating Scale at 10°C, heating and cooling ramp of 50°C/min and 25°C/min, with levels of 1 min, 3 min, 5 min, 8 min, 10 min, 15 min, 30 min and 60 min. analyzing the results of the physical properties of water absorption (WA), linear firing shrinkage (LFS), dilatometric analysis (DTA), flexural strain (SFT) and SEM of the sintered bodies in order to verify the adequacy of CDP to ISO 13006, ISO 10545, NBR 13816 standards; NBR 13817 and NBR 13818. The study showed that the formulations that best suit the requirements of the standards are:. G4 - which was applied in 10% of replacing the CBC phyllite, sintering temperature 1210 ° C for 10 min and porch, and F3 - with application of 7.5% of CBC to replace the feldspar in the sintering temperatures of 1190°C, 1200°C and 1210°C for 10 min and porch. These formulations showed better performance regarding the formation of primary and secondary mullite, with considerable reduction of cracks and pores, meeting the prerequisites of standards for glazed porcelain. The results shows that the use of the CBC as a flux in the preparation of porcelain mass meets standard parameters for the manufacture of the product, and thereby can reduce environmental impact and the cost of production. Therefore, it is recommended to use this residue in the ceramics industry, due to its industrial, commercial and collaborative viability for sustainability.

Uso de resíduos de queima de casca de café e argila da região sul da Bahia na obtenção de isolador elétrico cerâmico

The electrical ceramic insulators industry, uses noble raw materials such as siliceous and aluminous clays of white burning, in order to provide plasticity of the mass and contribute to electrical and mechanical properties required of the product, and feldspar with the flux function In literature references the composition of the masses indicates that the clay participates in percentage between 20 and 32, and feldspar 8 to 35, these materials have significant cost. In this research was performed the total replacement of commercial clay, for white burning clay from Santa Luzia region in southern Bahia and partial replacement of feldspar by ash residue of husk conilon coffee burning, from extreme south of Bahia. The objective of replacement these raw materials is to aver its technical feasibility and call attention for the embryo pole of ceramic industry for the existing in the south and extreme south of Bahia, which has significant reserves of noble raw materials such as clay white burning, kaolin, quartz and feldspar, and generates significant volume of gray husk conilon coffee as alternate flux. Clay Santa Luzia is prima noble material whose current commercial application is the production of white roofing. The residue of coffee husk ash is discarded near of production sites and is harmful to the environment. Phase diagrams and statistic design of experiments, were used for optimization and cost savings in research. The results confirmed the expectations of obtaining electrical ceramic insulators, with white burning clay of Santa Luzia and partial replacement up to 35.4% of feldspar, by treaty residue of conilon ash coffee husk burning. The statistic design that showed best results was for formulation with percentages of: clay 26.4 to 30.4%; kaolin 14.85 to 17.1%; feldspar 12.92 to 16.96%; R2 residue 7.08 to 9.2% and Quartz 32.5 to 38.75%, relative to the total mass of the mixture. The best results indicated; 0.2 to 1.4% apparent porosity , water absorption 0.1 to 0.7%, flexural strength 35 to 45MPa , dielectric strength 35-41 kV/cm , the transverse resistivity 8x109 2.5x1010 Ω.cm and for the dielectric constant ε/ε0 7 to 10.4, specification parameters for manufacturing ceramic electrical insulators of low and medium voltage.

Estudo do aproveitamento de resíduos PAE no desenvolvimento de materiais cerâmicos

This work presents a new ceramic material obtained through the incorporation of solid waste from the steel industry and known as dedusting powder PAE - in ceramic formulations based on clay, potassium and sodium feldspars, kaolin and talc. Formulations were prepared with ceramic residue levels of 0% (basic mass - MB), 2%, 4% and 8%, subjected to firing at temperatures of 1000 ° C, 1050ºC, 1100ºC and 1150ºC for periods of 15 min. and 120 min. The physicchemical and mechanical properties of these ceramic formulations were determined based on the firing temperature, residence time in the oven and the percentage of waste. Since the physicochemical and mechanical properties of the sintered materials were evaluated by chemical analysis techniques (fluorescence X-rays - FRX), particle size distribution, specific surface area, apparent density, structural analysis by diffraction of X-rays (DRX) and characterization of surface by scanning electron microscopy (SEM). The magnetic response characteristics and the pattern of magnetic ferrites of the samples were analyzed in the assay conditions, having noticed that the saturation magnetic susceptibility depend on the sintering temperature of the material and it is associated with its crystal structure. From the analysis results, it was concluded that the ceramic material with better physical and mechanical properties is obtained when the 8% from PAE residue is added to standard formulation under the burn time of 15 minutes and temperature of 1150ºC.

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

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

Efeito da adição de feldspato e/ou resíduo de caulin em formulações à base de argila ilítica

The red pottery industry in Piauí state is well developed and stands out at the national context for the technical quality of its products. The floor and wall tile industry, however, is little developed since the state has only one company that produces red clay-based ceramic tiles. This thesis aims at using the predominantly illitic basic mass of the above mentioned industry, with the addition of feldspar and/or kaolin residue in order to obtain products of higher technical quality. Kaolin residue consists basically of kaolinite, muscovite mica and quartz; the feldspar used was potassic. In this experiment, basic mass (MB) was used for experimental control and fifteen formulations codified as follows: F2, F4, F8, F16, F32, FR2, FR4, FR8, FR16, FR32, R2, R4, R8, R16 and R32. All raw materials were dry-milled, classified, formulated and then humidified to 10% water. Thereafter, test samples were produced by unixial pressing process in a rectangular steel matrix (60.0 x 20.0 x 5.0) mm3 at (25 MPa). They were fired at four temperatures: 1080°C, 1120°C, 1160°C, with a heating rate of 10°C/min during up to 10 min in an electric oven, and the last one in an industrial oven with a peak of 1140°C, aim ing to confirm the results found in laboratory and, finally, technological tests were performed: MEA, RL, AA, PA, TRF and PF. The results revealed that the residue under study can be considered a raw material with large potential in the industry of red clay-based ceramic tiles, since the results found both in laboratory and in the industry have shown that the test samples produced from the formulations with up to 4% feldspar and those produced with up to 8% feldspar and residue permitted a reduction in the water absorption rate and an increase in the mechanical resistance while those samples produced with up to 4% residue had an increase in the mechanical resistance when compared to those produced from the basic mass and that the formulation with 2% feldspar and residue presented the best technological properties, lowering the sintering temperature down to 1120°C

Uso de resíduo e de minerais de pegmatito da região do seridó RN e de argilas portuguesas em formulações de grês porcelanato

In the State Rio Grande do Norte, Brazil, the most significant deposits of minerals in the production of granite and pegmatite are Seridó region. Municipalities of Parelhas and Equador are the main responsible for the production of feldspar, quartz, kaolin and granite. The ceramic industries are always in search of competitiveness by investing in new products or improving existing techniques. The stoneware is a type of pottery that stands in the market because it presents technical and aesthetic characteristics superior to other existing products. Characteristics of the raw materials initially obtained with chemical analysis and mineralogical analysis are crucial in getting a product that satisfies the conditions in a manufacturing process and is, in principle, directly related to the firing cycle. This research aimed at developing new formulations for the mass production of ceramic stoneware. The raw materials initially characterized were feldspar, quartz, kaolin and granite. As part of the research was developed at the University of Aveiro, in Portugal, we used two clays used in the production of Portuguese ceramics. The raw material Brazilian and Portuguese and the final product, both in Portugal and Brazil, were analyzed for X-ray fluorescence, X-ray diffraction, granulometric analysis, dilatometric analysis, thermal analysis and analysis of scanning electron microscopy (MEV). The specimens prepared at the University of Aveiro (DECV) were sintered at 10000C and 12000C and the specimens prepared in UFRN were sintered at 10000C, 10500C, 11000C, 11500C, 12000C, 12500C and 13000C, but the best results and demonstrating the presence of the mineral mullite were at temperatures of 12000C, 12500C and 13000C. The results showed that the granite waste used may be considered raw material of excellent quality for use in the ceramic industry and coating floors and more accurately by the industry of stoneware. Physical and mechanical tests conducted on samples of the formulations F01 and F02 developed in UFRN showed a water absorption and mechanical strength suitable for the stoneware

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.