Made available in DSpace on 2014-12-17T14:07:24Z (GMT). No. of bitstreams: 1 MarcioLVNM.pdf: 5750272 bytes, checksum: b9659e465f3e2145cd82ea67e7bd6083 (MD5) Previous issue date: 2007-07-02 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Nowadays, industries from all sectors have great concerns over the disposition of the residues generated along the productive process. This is not different in the mineral sector, as this generates great volumes of residues. It was verified that the kaolin improvement industry generates great volumes of residue basically constituted of kaolinite, muscovite mica and quartz, which are basic constitution elements to formularisations of ceramics masses to the production of covering of stoneware tiles type. This happens because the methodology applied to the improvement process is still very rudimentary, what causes a very low yield, only ? from all the material volume that enters the improvement process, in the end, is marketable. The disposal of this residue, in a general way, causes a very big negative environmental impact, what has justified the researches efforts aiming to find a rational solution to this problem. In this way, the intention of this present work is the utilization of this residue in the manufacture of products to high quality ceramics covering, stoneware tiles in an industrial scale. For this purpose, the influence of the addition of the residue to a standard ceramics mass used by a ceramics sector company, already established in the market, with the intention of verifying the possibility of use of this residue as the mass complementary raw material and even the possible partial or total substitution of one of the components of the mass for the raw material in evidence will be studied. To the accomplishment of this work, the kaolin improvement residue generated by an industry of exploitation and improvement of kaolin, located in the region of Equador-RN, in the levels 1,2,4,8, 16 and 32% will be added to the standard mass already used for the production of stoneware tiles. The raw materials used, kaolin residue and the standard mass, were characterized through DRX, FRX, DTA, TGA and dilatometry. After the sintering of the bodies of test, tests of water absorption, apparent porosity, post burning linear retraction, apparent specific mass and flexural strength (3 point bending) were realized to determinate the technological properties of these materials. The results show the studied residue can be considered raw material of great potential to the industry of floor and ceramics covering of the stoneware tiles type / Atualmente, h? uma grande preocupa??o por parte das ind?strias, de todos os setores, com a disposi??o dos res?duos gerados ao longo do processo produtivo. No setor mineral n?o ? diferente, pois este gera grandes volumes de res?duos. Verificou-se que a ind?stria de beneficiamento do caulim gera grandes volumes de res?duo constitu?do basicamente de caulinita, mica muscovita e quartzo, que s?o constituintes b?sicos para formula??es das massas cer?micas para produ??o de revestimento tipo porcelanato, isso se d? porque a metodologia aplicada no processo de beneficiamento ainda ? muito rudimentar o que ocasiona um rendimento muito baixo, apenas 1/4 de todo o volume de material que entra do processo de beneficiamento, ao final, ? produto comercializ?vel. O descarte desse res?duo, de um modo geral, ocasiona um impacto ambiental negativo muito grande, o que tem justificado os esfor?os de pesquisas visando encontrar uma solu??o racional para este problema. Deste modo, o presente trabalho tem como objetivo a utiliza??o desse res?duo na fabrica??o de produtos para revestimento cer?mico de alta qualidade, gr?s e/ou porcelanato, em escala industrial. Para isso ser? estudada a influ?ncia do acr?scimo do mesmo a uma massa cer?mica padr?o utilizada por uma empresa do setor cer?mico, j? consolidada no mercado, com a inten??o de verificar a possibilidade de uso desse res?duo como mat?ria-prima completar desta massa em quest?o. Para a realiza??o deste trabalho ser? adicionado o res?duo do beneficiamento do caulim gerado por uma ind?stria de explora??o e beneficiamento de caulim, localizada na regi?o de Equador-RN, nos teores de 1, 2, 4, 8, 16 e 32% na massa padr?o j? utilizada para produ??o de porcelanato. As mat?rias-primas utilizadas, res?duo de caulim e a massa padr?o, foram caracterizadas atrav?s de DRX, FRX, DTA, ATG e dilatometria. Ap?s sinteriza??o dos corpos-de-prova foram realizados ensaios de absor??o de ?gua, porosidade aparente, retra??o linear ap?s queima, massa espec?fica aparente e tens?o de ruptura ? flex?o tr?s pontos para determina??o das propriedades tecnol?gicas destes materiais. Os resultados mostram que o res?duo estudado pode ser considerado como mat?ria-prima de grande potencial para a ind?stria de pisos e revestimentos cer?micos do tipo porcelanato. De acordo com os resultados obtidos verificou-se a possibilidade de utiliza??o do res?duo de caulim em um percentual de at? 16% de adi??o a massa padr?o, MP16. Essa formula??o apresentou resultados compat?veis com os exigidos pela norma em vigor, NBR 13818/1997 Placas cer?micas para revestimento especifica??o e m?todos de ensaios, al?m de diminuir o custo da massa e o custo com energia durante o ciclo de queima. Observou-se que o valor do m?dulo de ruptura a flex?o em tr?s pontos encontrado na temperatura 1210 ?C (55,4 MPa) ? inferior ao obtido quando se sinteriza a mesma formula??o MP16 a 1230 ?C (61,3 MPa). Por?m, o exigido pela norma em vigor s?o 35 MPa, que est? muito abaixo do menor valor. Para os outros ensaios, os valores obtidos para esta formula??o sinterizada a 1210 ?C s?o sempre melhores que os resultados a 1230 ?C

Cette étude a eu pour objectif de contribuer à une meilleure compréhension du comportement photochimique de certains micropolluants de type antibiotiques vétérinaires (sulfaquinoxaline, pyriméthamine) ou antibactérien (triclosan) en solution aqueuse et à la surface de la kaolinite, utilisée comme un modèle de sol.L’étude du comportement photochimique de la sulfaquinoxaline a été réalisée sous excitation à 254 nm et 365 nm. Dans tous les cas, une dégradation efficace est observée avec un rendement quantique qui dépend de la longueur d’onde d’excitation, du pH et la concentration d’oxygène dissous. De plus, la présence de l’oxygène moléculaire dans le milieu conduit à une inhibition partielle la photodégradation mettant en évidence l’implication partielle de l’état excité triplet. Ce dernier a pu être mis en évidence par photolyse laser nanoseconde à travers un transfert Triplet-Triplet (T-T) en employant le β-carotène comme accepteur. Sur le plan analytique, la phototransformation de la sulfaquinoxaline conduit à la formation d’un grand nombre de produits qui ont été identifiés par HPLC/ESI/MS/MS en identifiant les processus de fragmentation intervenant pour chaque molécule étudiée. L’étude a permis de montrer que les états excités singulet et triplet sont tout les deux impliqués dans la photodegradation et que les processus principaux intervenant sont la photohydrolyse, la désulfonation avec un réarrangement intramoléculaire, l'hydroxylation des motifs aromatiques et l'isomérisation selon un processus de type photo Fries.L’étude de la photoréactivité de la pyriméthamine a montré que la dégradation est plus efficace avec la forme neutre. Le rendement quantique a été évalué à environ 4,0x10-2 en milieu aéré et sous excitation à 254 nm. L’étude par photolyse laser a montré la formation intermédiaire de l’état excité triplet mais également de l’électron solvaté (absorption à 700 nm). Les processus de formation des photoproduits primaires sont la substitution de l’atome de chlore par un groupement hydroxyle ou par un atome d’hydrogène et l’hydroxylation du noyau aromatique.La dégradation des micropolluants à la surface du sol a pu être abordée en utilisant l’argile kaolinite comme support modèle. Ce système simplifié nous a permis d’étudier la photodégradation sous excitation en Suntest sur le plan cinétique et analytique. L’étude cinétique a été entreprise en fonction de différents paramètres tels que l’épaisseur de la kaolinite et la concentration initiale du substrat. Le premier effet nous a permis de montrer que pour des épaisseurs inférieures à 70 µm, la vitesse de diffusion du composé des zones sombres vers les zones irradiées est très rapide devant la photolyse et de ce fait, elle peut être négligée. Cet aspect a conduit à la détermination du rendement quantique de disparition à la surface de la kaolinite. Sur le plan analytique, les réactions observées sur l’argile sont différentes de celles observées en solution aqueuse. En effet, dans le cas de la sulfaquinoxaline, seul le produit de désulfonation est observé. Au contraire de la sulfaquinoxaline, l’étude complète de la molécule de triclosan a montré la formation de plusieurs produits et notamment des dimères ou des oligomères ce qui suggère la présence du substrat sous forme d’agrégats à la surface de l’argile. Afin de confirmer cette observation expérimentale, nous avons abordé une étude de modélisation par dynamique moléculaire. Celle-ci a donnée des informations très importantes sur l’organisation des molécules à la surface de la kaolinite. Ainsi, l’adsorption du triclosan fait intervenir d'importantes liaisons hydrogène avec la surface de la kaolinite. En présence de plusieurs molécules, la formation d’agrégats est gouvernée par une importante interaction entre les noyaux aromatiques de type π-stacking. / The study undertaken within this thesis concerns the photochemical behavior of the veterinary antibiotics sulfaquinoxaline and pyrimethamine, as well as the antimicrobial triclosan in aqueous solutions and at the surface of kaolin, used as a soil model.The photochemical study on sulfaquinoxaline was performed at 254 and 365 nm. In all cases, an efficient degradation was observed with a quantum yield that depends on the excitation wavelength, pH and the dissolved molecular oxygen concentration. Molecular oxygen acts as an inhibitor which reflects the involvement of the triplet excited state. Sulfaquinoxaline was clearly shown to be a photosensitizer of β-carotene via a triplet-triplet transfer process. From the analytical point of view, several photoproducts were generated and identified by using HPLC/ESI/MS/MS technique through a close analysis of the fragmentation processes. The byproducts that were formed via the singlet as well as the triplet excited states were mainly generated by photohydrolysis, desulfonation, hydroxylation and isomerisation reactions.The photochemical study of pyrimethamine indicates an efficient photoreactivity with the molecular form. The laser flash photolysis study reveals the implication of singlet and triplet excited states. The byproducts were mainly formed through the substitution of the chlorine atom by an hydroxyl group and the hydroxylation of the aromatic moiety.The photochemical study at the surface of soil was undertaken by using kaolin as a model support. Such simple system appears to be a guideline for precise kinetic and analytical studies. The former was performed as a function of several important parameters such as the layer thickness and the initial concentration of the substrate. The first parameter clearly indicates that for a thickness lower than 70 µm, the rate of diffusion is so fast that this process can be neglected when compared to the photochemical process. Thus, the first rate constant at the surface of kaolin was determined. Only the product of desulfonation was observed with sulfaquinoxaline while with triclosan, several byproducts were obtained such as dimers and oligomers suggesting the formation of aggregates at the surface of the solid support. In order to confirm this aspect, molecular dynamics studies were undertaken and indicate that the adsorption of triclosan mainly occurs at the surface of kaolin via hydrogen molecular bonds. The arrangement of the molecules in a cluster is governed by π-stacking type interactions between the aromatic moieties.

Thesis (DTech (Electrical Engineering))--Cape Peninsula University of Technology, 2011 / Ultrasonic Velocity Profiling (UVP) is both a method and a device to measure an instantaneous one-dimensional velocity profile along a measurement axis by using Doppler echography. UVP is an ideal technique since it is non-invasive, works with opaque systems, inexpensive, portable and easy to implement relative to other velocity profile measurement methods. Studies have suggested that the accuracy of the measured velocity gradient close to wall interfaces need to be improved. The reason for this is due to, depending on the installation method, distortion caused by cavities situated in front of ultrasonic transducers, measurement volumes overlapping wall interfaces, refraction of the ultrasonic wave as well as sound velocity variations. A new ultrasonic transducer, which incorporates a delay line material optimised for beam forming could reduce these problems (Wiklund, 2007). If these could be addressed, UVP could be used for the measurement of velocity profiles in complex geometries (e.g. contractions, valves, bends and other pipe fittings) where the shape of the velocity profile is critical to derive models for estimating fluid momentum and kinetic energy for energy efficient designs. The objective of this research work was to optimise the UVP system for accurate complex flow measurements by evaluating a specially designed delay line transducer and implementing advanced signal processing techniques. The experimental work was conducted at the Material Science and Technology (MST) group at the Cape Peninsula University of Technology (CPUT). This work also formed part of a collaborative project with SIK - The Swedish Institute for Food and Biotechnology. Acoustic characterisation of the ultrasonic transducers using an advanced robotic setup was done at SI K. Different concentrations of the following non-Newtonian fluids exhibiting different rheological characteristics were used for testing: carboxymethyl cellulose (CMC) solutions, kaolin and bentonite suspensions. Water was used for calibration purposes.

Made available in DSpace on 2014-12-17T14:57:47Z (GMT). No. of bitstreams: 1 JoaoDPV.pdf: 1303151 bytes, checksum: 407305d41d4b24852e57967eeba5cfd5 (MD5) Previous issue date: 2007-08-17 / Companies involved in kaolin mining and treatment represent an important area of industrial development in Brazil, significantly contribution to the worldwide production of such mineral. As a result, large volumes of kaolin residue are constantly generated and abandoned in the environment, negatively contributing to its preservation. In this scenario, the objective of the present study was to characterize the residue generated from kaolin mining as well as to assess its potential use as raw material for the production of ceramic tiles. Ceramic mixtures were prepared from raw materials characterized by X-ray fluorescence, X-ray diffraction, particle size analysis and thermal analysis. Three compositions were prepared using kaolin residue contents of 10%, 20% and 30%. Samples were uniaxially pressed, fired at 1200?C and characterized aiming at establishing their mineralogical composition, water absorption, apparent porosity, specific mass, linear retraction and modulus of rupture. The results showed that the residue basically consisted of kaolinite and successfully replaced raw kaolin in the preparation of ceramic title formulations without significantly affecting the properties of the fired material / As ind?strias de minera??o e beneficiamento de caulim s?o um importante segmento econ?mico do pa?s, com uma produ??o bastante significativa no cen?rio internacional. Em fun??o disso, a produ??o de res?duos ? muito grande, poluindo e agredindo o meio ambiente. Assim, esse trabalho tem por objetivo a caracteriza??o do res?duo do beneficiamento do caulim e a avalia??o de sua aplicabilidade como mat?riaprima alternativa na produ??o de cer?mica de revestimento. As mat?rias-primas utilizadas neste trabalho foram caracterizadas por t?cnicas de: fluoresc?ncia de raios X; difra??o de raios X; analise granulom?trica; an?lise termogravim?trica e an?lise termodiferencial. Foram formuladas tr? s composi??es contendo o res?duo de caulim, em propor??es de 10%, 20%, e 30%. Foram confeccionados corpos-de-prova por prensagem e suas massas foram queimadas a 1200?C e caracterizadas qu?mica e mineralogicamente com o objetivo de identificar suas composi??es, seus elementos e suas fases. Estes corpos-de-prova foram avaliados quanto ? absor??o de ?gua, porosidade aparente, massa espec?fica aparente, retra??o linear, difra??o de raios X e o m?dulo de ruptura ? flex?o. Pode-se concluir que o res?duo de caulim ? constitu?do basicamente por caulinita, e que a incorpora??o nas propor??es estudadas teve resultados altamente satisfat?rios nas formula??es, para a produ??o de cer?micas de revestimento

Made available in DSpace on 2014-12-17T14:57:49Z (GMT). No. of bitstreams: 1 JoseEVC_capa_ate_resumo.pdf: 114113 bytes, checksum: 65c5a81ce8eceb533010608034415ec0 (MD5) Previous issue date: 2009-08-10 / The production of red ceramic is an industrial activity that causes an intense impact. The manufacture of its products considerably increases the demand for natural resources, mainly with the extraction of raw material. The ceramic material produced generates waste, such as ash firewood and chamote. The residue from the beneficiation of kaolin is deposited in a poor, degrades the environment and contaminate water sources and soil, constituting in this manner, ecological disasters. The main objective of this work is to develop the formulation of a ceramic product consisting solely of industrial solid wastes, from ceramic tiles, (chamote) residue of kaolin and ash firewood. It is assumed that this product made in the laboratory can be used in coatings, wall and floor. The aim is to facilitate the replacement of the raw material of original composition of a ceramic body, for waste, while the process of production equal to the conventionally used, so that the properties of the product are reproduced. This work is characterized waste as its chemical composition, analysis of particle size, X-ray diffraction and thermal behavior. Several formulations were studied. The mass of waste was prepared by dry process, pressed to 25 MPa, and then burned in muffle type oven to 850, 950, 1050 and 1150 ?C. The results showed that it is technically possible to produce porous tiles only with waste. It was found that the formulations of bodies play a key role in the properties of the final product, as well as the sintering temperature and heating rates. RN in the waste of kaolin is estimated at 15,000 t/month, about 3,000 gray t/month and chamote with 10 million pieces/month damaged. The presence of carbonates of calcium and magnesium at 1050 ? C results in an appropriate porosity and mechanical strength. The formulation M3JE, composed of 69% waste of kaolin, 7.7% and 23.3% of chamote of gray, became suitable for porous materials with the strength and absorption within the level of national and international standards / A produ??o de cer?mica vermelha ? uma atividade industrial que provoca um intenso impacto ambiental. A confec??o de seus produtos aumenta sobremaneira a demanda por recursos naturais, principalmente com a extra??o da mat?ria prima, argila. O material cer?mico produzido gera res?duo, como o chamote e a cinza vegetal. O res?duo proveniente do beneficiamento do caulim que ? depositado de forma inadequada degrada o meio ambiente e contamina os mananciais da ?gua e do solo, constituindo dessa maneira, desastres ecol?gicos. O principal objetivo deste trabalho ? desenvolver formula??o de um produto cer?mico constitu?do exclusivamente de res?duos s?lidos industriais, oriundos de telhas cer?micas, (chamote), res?duo de caulim e cinza vegetal. Presume-se que este produto confeccionado em laborat?rio possa ser aproveitado em revestimentos de parede e piso. Pretende-se assim viabilizar a substitui??o das mat?rias-primas da composi??o original de uma massa cer?mica, por res?duos, mantendo-se o processo de produ??o igual ao convencionalmente utilizado, a fim de que as propriedades do produto sejam reproduzidas. No presente trabalho caracteriza-se os res?duos quanto a sua composi??o qu?mica, an?lise de tamanho de part?cula, difra??o de raios X e comportamento t?rmico. Diversas formula??es foram estudadas. A massa de res?duos foi preparada pelo processo via seca com corpos de provas prensados a 25 MPa, posteriormente queimados em forno mufla a 850, 950, 1050 e 1150 ?C. Os resultados obtidos evidenciaram tecnicamente que ? poss?vel se produzir placas cer?micas porosos exclusivamente com res?duos. Verificou-se que as formula??es das massas desempenham um papel fundamental nas propriedades do produto final, assim como as temperaturas de sinteriza??o e taxas de aquecimento. No RN os res?duos de caulim s?o estimados em 15000 t/m?s, a cinza com aproximadamente 3000 t/m?s e o chamote com 10 milh?es pe?as/m?s danificadas. A presen?a de carbonatos de c?lcio e magn?sio em 1050 ?C resulta em uma adequada porosidade e resist?ncia mec?nica. A formula??o M3JE, composta de 69% de res?duo de caulim, 7,7% de chamote e 23,3 % de cinza, se tornou adequado aos materiais porosos, com a resist?ncia mec?nica e absor??o dentro do patamar das normas nacionais e internacionais

Made available in DSpace on 2014-12-17T14:57:49Z (GMT). No. of bitstreams: 1 JaniaraFA.pdf: 946913 bytes, checksum: 7a2683c43f2b9a59eaca617cf3e52563 (MD5) Previous issue date: 2008-11-13 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The production of roof tiles in the state of Rio Grande do Norte accounts for around 60% of the total of ceramic pieces produced. There is a need for investment to improve quality and productivity, thereby promoting technological innovations. Accordingly, the aim of this study is to determine the effect of kaolin, potassium feldspar and quartz in two standard formulations, as well as the effect of sintering temperature on the technological properties of linear firing shrinkage, water absorption and bending rupture stress, by fitting the statistical model and using multiple linear regression to assess the relationship between technological properties and independent variables. The raw materials were characterized using the following techniques: X-ray fluorescence (XRF), X-ray diffraction (XRF), rational analysis (RA), differential thermal analysis (DTA) and granulometric analysis (GA). The test specimens were compacted by uniaxial pressure (25 MPa), dried in a stove at 110 ?C for 24 hours and sinterized at 850 ?C, 950 ?C and 1050 ?C and held isothermal for 30 minutes. The results obtained indicate that the addition of kaolin to two standard formulations (M and R) promoted a reduction in water absorption values and an increase in bending rupture stress values. The sintering temperatures for group M that resulted in the lowest linear firing shrinkage and water absorption values were 850 ?C and 950 ?C, respectively, and the highest bending rupture stress values were reached at a temperature of 950 ?C. In the case of group R, the sintering temperature that obtained the lowest water absorption and linear firing shrinkage values was 850 ?C, and the highest bending rupture stress values were attained at a temperature of 1050 ?C. This work explains the statistical approach used to fit the model that describes the relationship between the technological properties and percentage of kaolin, quartz and feldspar, as well as the models that enable predictions, provided that the lower and upper limits of the percentage of clay minerals, flux and quartz used in this study are respected. Statistica 6 software was used and results were obtained by stepwise forward regression / A produ??o de telha no Estado do Rio Grande do Norte representa cerca de 60 % do total de pe?as cer?micas produzidas. Percebe-se a necessidade de investimento na melhoria da qualidade e da produtividade, promovendo assim inova??es tecnol?gicas. Neste contexto, o objetivo geral deste trabalho ? verificar o efeito da adi??o de caulim, feldspato pot?ssico e quartzo em duas formula??es padr?o, assim como o efeito da temperatura de sinteriza??o nas propriedades tecnol?gicas de retra??o linear de queima, absor??o de ?gua e tens?o de ruptura ? flex?o, atrav?s do ajuste do modelo estat?stico, sendo utilizada a regress?o linear m?ltipla para avaliar a rela??o entre as propriedades tecnol?gicas e as vari?veis independentes. As mat?rias-primas foram caracterizadas atrav?s das seguintes t?cnicas: fluoresc?ncia de raios X (FRX), difra??o de raios X (DRX), an?lise racional (AR), an?lise t?rmica diferencial (DTA) e an?lise granulom?trica (AG). Os corpos-de-prova foram compactados por prensagem uniaxial (25 MPa), e na sequ?ncia secos em estufa a 110 ?C por 24 horas, em seguida sinterizados a 850 ?C, 950 ?C e 1050 ?C, com isoterma de 30 minutos. Os resultadosobtidos indicaram que a adi??o de caulim, em duas formula??es padr?o (M e R) promoveu redu??o nos valores de absor??o de ?gua e aumento nos valores de tens?o de ruptura ? flex?o. As temperaturas de sinteriza??o para o grupo M que proporcionaram os menores valores para a retra??o linear de queima e absor??o de ?gua foram 850 ?C e 950 ?C, respectivamente, e os maiores valores para a tens?o de ruptura ? flex?o foram alcan?ados na temperatura de 950 ?C. No caso do grupo R a temperatura de sinteriza??o que proporcionou os menores valores para absor??o de ?gua e retra??o linear de queima, foi a de 850 ?C, e os maiores valores para a tens?o de ruptura ? flex?o foram atingidosna temperatura de 1050 ?C. Este trabalho descreve a abordagem estat?stica para ajustar o modelo de regress?o linear m?ltipla e apresenta o ajuste do modelo que descreve a rela??o entre as propriedades tecnol?gicas e a porcentagem de caulim, quartzo e feldspato, assim como os modelos que possibilitam a realiza??o de predi??es, desde que n?o sejam ultrapassados os limites inferiores e superiores da porcentagem de argilominerais, fundente e quartzo utilizados neste trabalho. Para isto utilizou-se o software Statistica vers?o 6, obtendo resultados atrav?s da regress?o stepwise forward

Made available in DSpace on 2014-12-17T14:57:53Z (GMT). No. of bitstreams: 1 JorgeFB.pdf: 2466045 bytes, checksum: 390a8dfd299d465779890586b1bd5be1 (MD5) Previous issue date: 2009-10-19 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The State Bahia, Brazil, presents different geological sites it with a very expressive variety minerals. It is situated among the very important States which produces minerals for industries, such as pointed aggregate, ornamentals stones and ceramics raw materials. Nowadays only four companies producting ceramics tiles. Porcelainized stoneware tiles is one of the noblest ceramics, depicting low water absorption (typically below of 0,5%), in addition to excellent staining resistance and mechanical strength. The present work aims at investigating the potential of local raw materials for the production of porcelainized stoneware tiles. For this purpose, these materials were characterized by X-ray fluorescence, X-ray diffraction, particle size analysis, thermal gravimetric analysis, thermal differential analysis and dilatometric analysis. Admixtures containing different compositions were prepared and fired at four temperatures, 1100 ?C, 1150 ?C, 1200 ?C and 1250 ?C with isotherm for 60 minute and heathing rate of 5 oC/min. After firing the samples, they were characterized by water absorption tests, linear retraction, analysis, apparent porosity, apparent specific mass, flexural strength, and microstructural analysis by X-ray diffraction and scanning electron microscopy . The results revealed three ceramics with porcelainized stoneware tiles characteristics and porcelain tile will be produce from raw materials originated in the State of Bahia / O Estado da Bahia apresenta uma diversidade de terrenos geol?gicos que encerra uma expressiva dota??o mineral e est? situado entre os mais importantes Estados produtores de minerais industriais, ressaltando-se agregados, rochas ornamentais e mat?rias-primas cer?micas. Atualmente somente quatro empresas produzem placas cer?micas. O gr?s porcelanato ? uma das mais nobres cer?micas de revestimento devido a sua baixa absor??o d ?gua (tipicamente abaixo de 0,5%), al?m de apresentar excelentes caracter?sticas t?cnicas, destacando-se pelas elevadas resist?ncias mec?nica, ao risco e ao manchamento. O presente trabalho tem a finalidade de avaliar o potencial das mat?rias-primas, feldspato, argila e caulim, utilizado na produ??o de gr?s porcelanato no estado da Bahia. Para isso, foi feita a caracteriza??o das mat?rias-primas por fluoresc?ncia de raios X (FRX), difra??o de raios X (DRX), an?lise granulom?trica (AG), an?lise t?rmica gravim?trica (TG), an?lise t?rmica diferencial (DTA) e an?lise dilatom?trica, elaborando-se sete formula??es que foram queimadas nas temperaturas: 1100 ?C, 1150 ?C, 1200 ?C e 1250 ?C, com isoterma de 60 minutos e taxa de aquecimento de 5 oC/ min. Ap?s a queima, os corpos-de-prova foram submetidos a ensaios de absor??o de ?gua, retra??o linear, an?lise dilatom?trica, porosidade aparente, massa espec?fica aparente, resist?ncia ? flex?o, difra??o de raios X e microscopia eletr?nica de varredura. Em tr?s formula??es foram obtidas, propriedades compat?veis com as exigidas para a produ??o do gr?s porcelanato com mat?rias-primas oriundas do Estado da Bahia

The mesoporous materials Al-MCM-41 produced from kaolin, low cost raw material, by means of hydrothermal acid treatment route, has shown potential for being used as adsorbent in removal process of methylene blue. The process of synthesis of Al-MCM-41 is based on calcination of kaolin, dealumination by acid treatment, hydrothermal synthesis and extraction of the surfactant. The characterization of de obtained mesoporous material was carried out by techniques such as: X-ray diffraction, vibrational spectroscopy in the infrared, 29Si and 27Al nuclear magnetic resonance in the solid state, scanning electron microscopy, transmission electron microscopy and N2 adsorption/desorption. The X-ray diffraction at low angles allowed the determination of the cell parameter, which was 4.02 nm. The analyses of scanning and transmission electron microscopy revealed important morphological properties of the synthesized material. N2 adsorption/desorption showed a BET specific surface area of 1,303 m2 g-1, pore volume of 1.23 cm3 g-1 and average diameter of 2.45 nm. PZC measurements showed a pHPZC of 2.69. The adsorption of methylene blue by Al-MCM-41 adsorbent showed high kinetic and high adsorption capacity, with values around 316 mg g-1. / O material mesoporoso Al-MCM-41 produzido a partir de caulim, matÃria-prima de baixo custo, por meio de rota hidrotÃrmica com tratamento Ãcido, mostrou-se promissor para ser usado como adsorvente do corante azul de metileno. O processo de sÃntese da Al-MCM-41 Ã baseado na calcinaÃÃo do caulim, desaluminizaÃÃo por tratamento Ãcido, sÃntese hidrotÃrmica e eliminaÃÃo do surfactante. A caracterizaÃÃo do material mesoporoso foi realizada por meio de tÃcnicas como: difraÃÃo de raios-X, espectroscopia vibracional na regiÃo do infravermelho, ressonÃncia magnÃtica nuclear no estado sÃlido de 29Si e 27Al, microscopia eletrÃnica de varredura, microscopia eletrÃnica de transmissÃo e adsorÃÃo de N2. A anÃlise de difraÃÃo de raios-X em baixo Ãngulo da Al-MCM-41 permitiu a determinaÃÃo do parÃmetro de cÃlula que apresentou valor de 4,02 nm. As anÃlises de microscopia eletrÃnica de varredura e de transmissÃo revelaram importantes propriedades morfolÃgicas do material sintetizado. Utilizando as medidas de adsorÃÃo e desorÃÃo de gÃs N2 a Ãrea superficial especÃfica BET da Al-MCM-41 apresentou valor 1.303 m2 g-1, com um volume de poros de 1,23 cm3 g-1 e diÃmetro mÃdio de 2,45 nm. O teste do PZC determinou um pHPZC de 2,69. Os testes de adsorÃÃo do azul de metileno pelo adsorvente Al-MCM-41 mostraram que o mesmo apresenta alta capacidade de adsorÃÃo com valores em torno de 316 mg g-1.

Cette étude a fait l'objet de deux parties. L'une porte sur l'effet de différents types d'activation (chimique, thermique, mécanique) de kaolins (géo-matériaux riches en kaolinite) sur leurs propriétés de décoloration vis-à-vis de l'huile de riz. L'autre traite de l'effet de la taille et de la morphologie de kaolinites de synthèse sur leurs propriétés d'adsorption.Cette étude a montré que lorsque le kaolin était chauffé à plus de 100°C avant de subir une activation acide en milieu sulfurique, citrique ou oxalique, la capacité de décoloration vis-à-vis de l'huile de riz était fortement réduite. Cet effet a été directement mis en relation avec la destruction partielle ou totale de la structure de la kaolinite, associée à une forte lixiviation de l'aluminium de l'échantillon et à la précipitation de silice amorphe. Il s'est donc avéré que la préservation des sites aluminols présents sur les surfaces externes des particules de kaolinites semblait être un critère primordial à conserver en vue d'obtenir de bonne capacité de décoloration. Dans ce contexte, les meilleures capacités de décoloration (82% environ) ont été obtenues en utilisant conjointement un traitement thermique modéré (<100°C), un broyage mécanique de l'échantillon avant l'étape d'activation acide, une concentration en acide de l'ordre de 0.3 à 0.5 mol/L et un rapport (argile)/(solution acide) de l'ordre de 1/50. Notons que les plus fortes valeurs de surfaces spécifiques n'ont pas forcément été associées aux échantillons présentant les meilleures capacités de décoloration en raison de la présence de silice amorphe et de la non-préservation des sites aluminols de la kaolinite ; sites responsables de l'adsorption des pigments de molécules de chlorophylle-a.Par ailleurs, aucune étude à notre connaissance ne reliait directement les morphologies de particules de phyllosilicates à leurs propriétés d'adsorption vis-à-vis de deux cations inorganiques. Dans le cas des kaolinites naturelles, une charge permanente souvent significative et attribuable à des impuretés minéralogiques empêche toute tentative de relier directement la forme des particules à un coefficient de sélectivité entre deux cations pour des sites latéraux donnés. Des kaolinites ont donc été synthétisées par voie hydrothermale en considérant différentes conditions physico-chimiques, afin d'obtenir des morphologies variées (hexagones plus ou moins anisotropes). Pour ces échantillons synthétiques pour lesquels aucune impureté minéralogique et charge permanente n'a été détectée, des isothermes expérimentales d'adsorption entre Na+ et H+ ont été mesurées. Ces cations ont été choisis étant donné leur présence ubiquiste dans les eaux naturelles et leur fort pouvoir compétiteur par rapport aux cations traces métalliques. Grâce aux surfaces spécifiques des sites latéraux et des densités de site issues de la cristallographie des différentes faces présentes dans nos échantillons ((010), (110), (1-10)), un coefficient de sélectivité entre Na+ et H+ sur l'ensemble des sites latéraux d'une morphologie donnée a pu être estimé à l'aide d'un modèle de complexation de surface. Les résultats ont montré que le coefficient de sélectivité Na+/H+ dépendait très fortement de la morphologie de la particule, et que par conséquent les propriétés d'adsorption des kaolinites ne pouvaient pas être obtenues avec précision sans une connaissance fine de la morphologie des particules. / The dissertation consists of two main parts; the first part is devoted to the effect of physical/thermal and chemical activation of kaolin on bleaching of rice bran oil. In this study, samples were prepared from natural Ranong kaolin. This study focused on the effects of both thermal treatment (from 100 to 900°C) and chemical activation (sulfuric acid, hydrochloric acid, citric acid and oxalic acid using different acid concentrations or different clay/acid ratio) on the capacity of kaolins to bleach rice bran oil. When kaolin was treated with high temperature (>100°C) prior to reflux and with a high acid concentration during reflux, the kaolinite structure was partially or completely destroyed associated to a dramatic leaching of alumina, and amorphous silica dominated the samples. The measured maximum bleaching capacity obtained was not consistent with the highest specific surface area and pore volume; rather, it depended on the alumina contents in the samples. Thus, the partial preservation of the kaolinite structure is crucial to obtain an appropriate bleaching capacity of kaolin. This is directly related to the preservation of the aluminol sites present at the kaolinite surface. XRF analysis showed that the alumina contents of 28-34% were values to reach in order to obtain optimum bleaching capacities of kaolin, independently of the different acid used. Finally, optimum bleaching of ~83%, ~82% and ~81% were achieved by grinding the kaolin prior to reflux with low acid concentration of hydrochloric acid (0.5 M), sulfuric acid (0.3 M) and citric acid (0.5 M), respectively with clay/acid ratio of 1:50.The second part of the thesis aims to elucidate the influence of morphology of kaolinites on their sorption properties. For that, Na+/H+ sorption isotherms in water saturated conditions of synthetic kaolinites and natural well crystallized kaolinite, called KGa--1b commercialized by the Clay Mineral Society, were performed and interpreted. Kaolinites used in this study were hydrothermally synthesized from partially crystallized kaolinite as a function of different final pH (pHF) ranging from 0.8 to 8.3. Results obtained for KGa--1b were compared with data obtained in literature for this mineral, in order to fully validate this approach. This study found that cation exchange capacity, due to both isomorphic substitutions in the crystals (permanent charge), and silanol and aluminol edge sites were highly variable. Typically, CEC at pH=9 varied from ~0.8 cmolc/kg for well crystallized kaolinite (pHF 0.8) to ~33 cmolc/kg for disordered lath-shaped kaolinite (pHF 8.3). Na+/H+ sorption isotherms were obtained for all synthetic kaolinites as a function of pH ranging from pH 3 to 11. Results showed that sorption of Na+ increases dramatically with pH. Typically for all kaolinite samples except for the one synthesized at pHF=8.3, Na+ sorption is rigorously equal to zero when pH<7, indicating no permanent charge in the samples (in contrast to natural KGa--1b kaolinite), and increases when pH>7 due to sorption on edge sites. The amount of dissolved silica measured during Na+/H+ isotherm is higher for experiments performed with kaolinites synthesized in basic conditions (for pHF 7.4 and pHF 8.3) than for kaolinites synthesized in acid conditions (for pHF 0.8 and pHF 3.3). These latter results lead to conclude that sorption site density can be considered constant when pH is between 4 and 10, independently of the morphologies of particles. In this context, a thermodynamic modeling procedure using a complexation model was applied to interpret the data obtained with hexagonal- and lath-shaped particles. During this procedure, selectivity coefficient between Na+ and H+ cations were obtained considering the total edge site densities calculated from lateral specific surfaces estimated for synthetic kaolinites and crystallography data.

The first part of the thesis discuss general characterization of heterogeneous processes in silicates. This part is focused on kinetics of heterogeneous processes and mathematical description of reactions time behavior. The other part describes important technologies in silicate industry such as sintering, solid matter decomposition, transition modification, etc. Another chapter deals mineralogy, structure and properties of eminent silicate raw materials. Emphases is given to characterization of clay minerals and their utilising. The experimental part handle the analytic techniques used for investigation of thermal decompostion, dehydroxylation, crystalization of Al-Si spinel phase and sintering process of washed kaolin Sedlec Ia from the region Carlsbad (Czech Republic). Concluding chapter reports on results of experimental work.