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Otimiza??o do processo de s?ntese do aluminato de cobalto via m?todo de polimeriza??o de complexos (MPC) atrav?s do planejamento fatorial fracionado / Optimization of process of synthesis of cobalt aluminate via complex polymerization method (CPM) through fractional factorial planning.Gomes, Yara Feliciano 20 December 2012 (has links)
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Previous issue date: 2012-12-20 / In the ceramics industry are becoming more predominantly inorganic nature pigments. Studies in this area allow you to develop pigments with more advanced properties and qualities to be used in the industrial context. Studies on synthesis and characterization of cobalt aluminate has been widely researched, cobalt aluminate behavior at different temperatures of calcinations, highlighting especially the temperatures of 700, 800 and 900? C that served as a basis in the development of this study, using the method of polymerization of complex (CPM), economic, and this method applied in ceramic pigment synthesis. The procedure was developed from a fractional factorial design 2 (5-2) in order to optimize the process of realization of the cobalt aluminate (CoAl2O4), having as response surfaces the batch analysis data of Uv-vis spectroscopy conducted from the statistic software 7.0, for this were chosen five factors as input variables: citric acid (stoichiometric manner), puff or pyrolysis time (h), temperature (? C), and calcinations (? C/min), at levels determined for this study. By applying statistics in the process of obtaining the CoAl2O4 is possible the study of these factors and which may have greater influence in getting the synthesis. The pigments characterized TG/DSC analyses, and x-ray diffraction (XRD) and scanning electron microscope (SEM/EDS) in order to establish the structural and morphological aspects of pigment CoAl2O4, among the factors studied it were found to statically with increasing calcinations temperature 700?< 800 <900 ?C, the bands of Uv-vis decrease with increasing intensity of absorbance and that with increasing time of puff or pyrolysis (h) there is an increase in bands of Uv-vis proportionally, the generated model set for the conditions proposed in this study because the coefficient of determination can explain about 99.9% of the variance (R?), response surfaces generated were satisfactory, so it s possible applicability in the ceramics industry of pigments / Na ind?stria cer?mica utilizam-se cada vez mais pigmentos de natureza predominantemente inorg?nica. Os estudos nessa ?rea permitem desenvolver pigmentos com qualidades e propriedades mais avan?adas para serem empregados em ?mbito industrial. Estudos de s?ntese e caracteriza??o do aluminato de cobalto t?m sido amplamente pesquisados, o comportamento do aluminato de cobalto em diferentes temperaturas de calcina??es, destacando principalmente as temperaturas de 700, 800 e 900?C utilizando o m?todo de polimeriza??o de complexos (MPC), m?todo este, econ?mico e aplicado em s?ntese de pigmentos cer?micos. O procedimento foi desenvolvido a partir de um planejamento fatorial fracionado 2(5-2) com o objetivo de otimizar o processo de realiza??o do aluminato de cobalto (CoAl2O4), tendo como superf?cies de respostas os dados da an?lise de espectroscopia do Uv-vis realizados a partir do software statistic 7.0, para isso, foram escolhidos cinco fatores como vari?veis de entrada: concentra??es de ?cido c?trico (de maneira estequiom?trica), tempo de puff ou pir?lise (h), temperatura (?C), tempo e taxas de calcina??es(?C/min), em patamares determinados para este estudo. Atrav?s da aplica??o estat?stica no processo de obten??o do CoAl2O4 foi poss?vel estudar entre estes fatores quais possam ter maior influ?ncia na obten??o da s?ntese. Os p?s-precursores foram caracterizados pelas an?lises termogravim?tricas TG/DSC, e os p?s-calcinados (pigmentantes) foram analisados pela difra??o de raios- x (DRX) e microscopia eletr?nica de varredura com energia dispersiva (MEV/EDS) a fim de comprovar os aspectos estruturais e morfol?gicos do CoAl2O4, entre os fatores estudados estaticamente verificou-se que com o aumento da temperatura de calcina??o 700<800<900?C, as bandas do Uv-vis diminuem com o aumento da intensidade da absorb?ncia e que com o aumento do tempo de puff ou pir?lise (h) h? um aumento das bandas do Uv-vis proporcionalmente, o modelo gerado ajustou-se para as condi??es propostas neste estudo, pois o coeficiente de determina??o consegue explicar cerca de 99,9%, da vari?ncia (R?), as superf?cies de respostas geradas foram satisfat?rias, sendo assim sua poss?vel aplicabilidade na ind?stria cer?mica de pigmentos
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Avalia??o da incorpora??o combinada dos res?duos de cascalho de perfura??o de po?o de petr?leo e de polimento do porcelanato em cer?mica vermelhaSilva, Moacir Guilhermino da 10 February 2012 (has links)
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Previous issue date: 2012-02-10 / Among the industries, those that produce ceramic porcelain for use in construction industry and oil, during the exploration and production period, play an important role in the production of waste. Much research has been carried out both by academia and the productive sector, sometimes reintroducing them in the same production line that generated them, sometimes in areas unrelated to their generation, as in the production of concrete and mortar for the construction, for example, but each one in an isolated way. In this research, the aim is to study the combined incorporation of the waste drill cuttings of oil well and the residue of the polishing of porcelain, generated in the final stage of finishing of this product in a clay matrix, for the production of red pottery, specifically bricks, ceramic blocks and tiles. The clay comes from the municipality of S?o Gon?alo, RN, the drilling waste is from the Natal basin, in Rio Grande do Norte, and the residue of the polishing proceeds from a ceramic porcelain of the State of Para?ba. For this purpose, we used a mixture of a plastic clay with a non-plastic, in a ratio of 50% each, settling formulations with the addition of these two residues in this clay matrix. In the formulations, both residues were incorporated with a minimum percentage of 2.5% and maximum of 12.5%, varying from 2.5% each, in each formulation, which the sum of the waste be no more than 15%. It should be noted that the residue of the polishing of ceramic porcelain is a IIa class (not inert). The materials were characterized by XRF, XRD, TG, DTA, laser granulometry and the plasticity index. The technological properties of water absorption, apparent porosity, linear shrinkage of burning, flexural tensile strength and bulk density were evaluated after the sintering of the pieces to 850 ?C, 950 ?C and 1050 ?C, with a burning time of 3 hr, 3 hr and 30 minutes, and 3 hr and 50 minutes, respectively, with a heating rate of 10 ?C/minute, for all formulations and landing of 30 minutes. To better understand the influence of each residue and temperature on the evaluated properties, we used the factorial planning and its surfaces of response for the interpretation of the results. It was found that the temperature has no statistical significance at a 95% of reliability level in flexural tensile strength and that it decreases the water absorption and the porosity, but increases the shrinkage and the bulk density. The results showed the feasibility of the desired incorporation, but adjusting the temperature to each product and formulation, and that the temperatures of 850 ?C and 950 ?C were the one that responded to the largest number of formulations / A ind?stria de produ??o de porcelanatos para uso na constru??o civil e a do petr?leo, na fase de explora??o e produ??o, exercem um papel importante na produ??o de res?duos. Muitas pesquisas t?m sido realizadas tanto pela academia quanto pelo setor produtivo, ora reintroduzindo esses res?duos na mesma linha de produ??o que os gerou, ora em setores alheios ao de sua gera??o, como na produ??o de concretos e argamassas para a constru??o civil, por exemplo, mas cada um de forma isolada. O objetivo desta pesquisa ? estudar a incorpora??o combinada do res?duo de cascalho de perfura??o de po?o petrol?fero e do res?duo do polimento do porcelanato, gerado na fase de acabamento final do produto, numa matriz argilosa, para a produ??o de cer?mica vermelha - especificamente tijolos, blocos cer?micos e telhas. A argila utilizada ? oriunda do munic?pio de S?o Gon?alo do Amarante, RN; o res?duo de perfura??o, da bacia potiguar, no Rio Grande do Norte; e o do polimento ? de uma cer?mica de porcelanato do Estado da Para?ba. Utilizou-se a mistura de uma argila pl?stica com uma n?o pl?stica, numa propor??o de 50 % de cada uma (que ? o percentual de mistura adotado na cer?mica fornecedora dessa argila), estabelecendo-se formula??es com a incorpora??o dos dois res?duos nessa matriz argilosa. Nas formula??es, os dois res?duos foram incorporados com um percentual m?nimo de 2,5 % e m?ximo de 12,5 %, variando-se em 2,5 % cada um, em cada formula??o, de modo que a soma dos res?duos fosse no m?ximo 15 %. ? oportuno registrar que o res?duo do polimento do porcelanato ? de classe IIa (n?o inerte). Os materiais foram caracterizados por FRX, DRX, TG, DTA, granulometria a laser e pelo ?ndice de plasticidade. As propriedades tecnol?gicas de absor??o de ?gua, porosidade aparente, retra??o linear de queima, tens?o de ruptura ? flex?o e massa espec?fica aparente, foram avaliadas ap?s a sinteriza??o das pe?as a 850 ?C, 950 ?C e 1050 ?C, com ciclo de queima de 3 h , 3 h e 30 min e 3 h e 50 min, respectivamente, com taxa de aquecimento de 10 ?C/min. e patamar de 30 min., para todas as formula??es. Para melhor compreender-se a influ?ncia de cada res?duo e de cada temperatura nas propriedades avaliadas, utilizou-se o planejamento fatorial e suas superf?cies de resposta para interpreta??o dos resultados. Verificou-se que a temperatura n?o tem signific?ncia estat?stica no n?vel de 95 % de confiabilidade na tens?o de ruptura ? flex?o e que ela diminui a absor??o de ?gua e a porosidade, mas aumenta a retra??o e a massa espec?fica aparente. Os resultados mostraram a viabilidade da incorpora??o pretendida, adequando-se a temperatura a cada produto e cada formula??o, e as temperaturas de 850 ?C e 950 ?C foram as que atenderam ao maior n?mero de formula??es
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