The aim of this dissertation is to appraise and critically reflect on the physical pertinence of governing equations and closure relations often used for the modeling of gas-phase transport phenomena in high-temperature solid-oxide fuel cells (SOFCs). More precisely, this work conducts a critical literature review on the concentration-induced voltage losses (i.e., concentration polarization) resulting from mass transfer limitations. Thus, the overall object of this work was to stress awareness of the limits of mathematical models studied and developed in the SOFC literature to date, and which are specifically related to concentration polarization processes. To a great extent, the design of SOFC porous layers is likened to that of optimizing the transport of multicomponent gas mixtures in structured porous catalysts, for which diffusional and flow limitations are of cardinal importance. In both cases, severe inconsistencies in mass transport models cannot be simply ignored and the main uncertainties in utilizing such models should be clarified. It is hoped that the information herein will serve usefully to support future developments of more consistent theoretical frameworks, thereby improving the confidence on the results of numerical simulations. The critical literature review has been carried out so to identify a number of physical inconsistences, ill-defined approximations, and misleading mathematical derivations. Along the review, it is argued that the choice (or, more properly, the lack of conceptual refinement) of a particular mathematical model can significantly impair the \"prediction\" of transport processes relevant to concentration-induced power losses in SOFCs. One of the keystones of this work was therefore to re-interpret and thus to reassess the frequently contradictory literature related to certain classes of gas-phase transport models pertinent to the evaluation of concentration polarization. With this revisionary approach, it is expected that one could reduce confusion, clear up apparent contradictions, and improve the possibility of gaining new insights. / Esta dissertação tem o objetivo de avaliar e refletir criticamente sobre a pertinência física de equações de conservação e de relações de fechamento, frequentemente utilizadas na modelagem multiescala de fenômenos de transporte em células a combustível de óxido-sólido (SOFC). Dêu-se atenção especial ao escoamento em \"microescala\" de misturas gasosas multicomponentes, dentro de meios porosos quimicamente reativos. Em outras palavras, esta monografia busca ressaltar quais os limites para aplicação de certas classes de modelos matemáticos, os quais têm sido desenvolvidos e utilizados na literatura de SOFCs até o presente momento. O projeto de camadas porosas de SOFCs assemelha-se à tarefa de otimizar processos de transporte em catalisadores estruturados, para os quais a existência de limitações de transporte por difusão e por escoamento tem importância primordial. Por esta razão, inconsistências originadas em modelos de fenômenos de transporte não podem ser, simplesmente, negligenciadas e, portanto, as principais incertezas ao se utilizar tais modelos devem ser devidamente esclarecidas. Espera-se, com efeito, que as informações contidas neste trabalho sejam úteis para futuros desenvolvimentos teóricos mais consistentes, de forma a aumentar a confiabilidade no uso de resultados obtidos por simulações numéricas.

Orientador: Renato Sprung / Tese doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica / Made available in DSpace on 2018-08-06T18:06:45Z (GMT). No. of bitstreams: 1 Villanueva_SandraBizarriaLopes_D.pdf: 2768871 bytes, checksum: ec40bbcbf8152a8c34f6d7fdd395af83 (MD5) Previous issue date: 2005 / Resumo: Materiais do tipo hidrotalcita foram sintetizados, calcinados e caracterizados, assim como utilizados na conversão catalítica de etanol. As sínteses foram realizadas com razões molares AI/(AI + Mg) iguais a 0,20; 0,25 e 0,33; em todos os casos os difratogramas de raios-X demonstraram que, efetivamente, fases de hidrotalcitas tinham sido obtidas. Esses materiais apresentaram áreas superficiais BET de cerca de 50 a 70 m2.g-l, à exceção da hidrotalcita sintetizada com agentes precipitantes contendo amônio, em que a área superficial foi de cerca de 7 m2g -I. A quimissorção de CO2 desses materiais revelou que hidrota1citas calcinadas são sólidos básicos e tal basicidade relaciona-se com o teor de magnésio substituído e também com a temperatura de ca1cinação. Os testes catalíticos foram realizados a temperaturas de 3000 C a 4000 C e verificou-se o aumento da taxa de reação com o incremento da temperatura. Os produtos de condensação éter etílico e nbutanol foram obtidos em maior proporção. Hidrotalcitas da série sódio apresentaram maior rendimento de n-butanol independentemente do teor de alumínio presente na amostra. Todas as amostras utilizadas apresentaram, a baixas conversões, quantidades significativas de n-butanol, o que pode indicar que, além da via de condensação aldólica, a formação desse produto também ocorre via condensação direta do etanol, ou seja, sem a dessorção para a fase gasosa da molécula de acetaldeído. Testes catalíticos comparativos realizados com óxido de magnésio e alumínio resultaram principalmente em acetaldeído e etileno, respectivamente. Traços de n-butanol foram identificados no óxido de magnésio quando testado a 4000 C, e éter etílico foi observado em maior quantidade no óxido de alumínio quando testado a 3000 C / Abstract: Hydrotalcites-like materiaIs were prepared, calcined and characterized as well as used in the catalytic reaction of ethanol. The synthesis were perfonned with AI/(AI + Mg) ratios of 0.20; 0.25 and 0.33; in all cases the x-ray showed hydrotalcites phases. These materiaIs resulted in BET areas of 50 at 70 m2.g-1, except for the hydrotalcite synthesized with NH3, that resulted in a BET area 00 m2g-1. The CO2 chemisorption on these materiaIs revealed that calcined hydrotalcites are basic catalysts and their basicity was related to the quantity of substituted magnesium and to the calcination temperature. The catalytic reactions were performed at 300, 350 and 4000 C; the reaction rate increasing with reaction temperature. The main reaction products identified were ether and n-butanol. The hydrotalcite synthesized with cation sodium presented the highest yield of n-butanoI independent of aluminum content present in the samples. The results of Iow conversions showed significant yield of n-butanoI, and this could indicate that the formation of that product occurs by aldoI condensation and aIso by straight condensation of ethanoI molecule, without acetaldehyde desorption to gas fase. Comparative catalytic tests performed with MgO and AI203 showed acetaldehyde and ethylene predominantly as reaction products. Traces of n-butanoI were identified with MgO when the reaction occurred at 4000 C, and ether was identified with AI203 when the reaction occurred at 3000 C / Doutorado / Desenvolvimento de Processos Químicos / Doutor em Engenharia Química

Submitted by Marlene Santos (marlene.bc.ufg@gmail.com) on 2016-06-15T19:31:26Z No. of bitstreams: 2 Dissertação - Caroline Winter - 2016.pdf: 7433726 bytes, checksum: bf2a1b900a9af4a614fcafcacca772fa (MD5) license_rdf: 19874 bytes, checksum: 38cb62ef53e6f513db2fb7e337df6485 (MD5) / Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2016-06-28T12:15:36Z (GMT) No. of bitstreams: 2 Dissertação - Caroline Winter - 2016.pdf: 7433726 bytes, checksum: bf2a1b900a9af4a614fcafcacca772fa (MD5) license_rdf: 19874 bytes, checksum: 38cb62ef53e6f513db2fb7e337df6485 (MD5) / Made available in DSpace on 2016-06-28T12:15:36Z (GMT). No. of bitstreams: 2 Dissertação - Caroline Winter - 2016.pdf: 7433726 bytes, checksum: bf2a1b900a9af4a614fcafcacca772fa (MD5) license_rdf: 19874 bytes, checksum: 38cb62ef53e6f513db2fb7e337df6485 (MD5) Previous issue date: 2016-03-07 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / The members of flavonoids and chalcones family have attracted great interest because of their pharmacological applications as antibacterial, anti-inflammatory and anticarcinogenicagents, and are commonly synthesized by Claisen-Schmidt condensation between acetophenone and benzaldehyde derivatives. This reaction is usually catalyzed under homogeneous conditions which present, however, several drawbacks such as catalyst recovery and waste disposal problems. This work proposes the use of a variety of heterogeneous catalysts to achieve good results for condensation Claisen-Schmidt reaction in terms of conversion and chalcones selectivity, when compared to the homogeneous catalysis. Two groups of catalysts were tested: metal oxides and activated carbons. Magnesium oxide catalysts were prepared by hydrothermal treatment and magnesium, niobium, lanthanum and titanium oxides by rehydration of commercial precursors, all methods followed and not followed by cesium impregnation. The activated carbons used as catalysts were Babassu, Bahia Coconut, ox bone and Dendê, raw and treated with sodium hydroxide. The catalysts were characterized by scanning and transmission electron microscopy, thermogravimetric analysis, differential thermal analysis, determination of the specific superficial area by the adsorption/desorption of N2 at 77 K method, infrared spectroscopy, X-ray diffraction and temperature-programmed desorption of CO2 and NH3. The basic sites of carbons were quantified by Boehm Method. Finally, the performance of the catalysts was evaluated on the Claisen-Schmidt reaction between Acetophenone and 4-nitrobenzaldehyde, and the conversion was quantified by high performance liquid chromatography. The best catalyst was treated babassu activated carbon, whose conversion achieved was 92,38%. / Os membros da família das chalconas e flavonóides têm despertado um grande interesse devido às suas aplicações como agentes farmacológicos, antibacterianos, anti-inflamatórios e anticarcinogênicos, sendo comumente sintetizados via condensação de Claisen-Schmidt entre derivados de acetofenona e de benzaldeído. Esta reação é catalisada normalmente sob condições homogêneas, que apresentam, no entanto, vários inconvenientes, tais como a recuperação do catalisador e problemas de destinação de resíduos. Neste trabalho foi proposto o uso de uma série de catalisadores heterogêneos para se alcançar bons resultados para a reação de condensação de Claisen-Schmidt, em termos de conversão e seletividade de derivados de chalconas, quando comparados à catálise homogênea. Foram testados dois grupos de catalisadores: óxidos metálicos e carvões ativados. Prepararam-se catalisadores de óxido de magnésio por tratamento hidrotérmico e óxidos de magnésio, nióbio, lantânio e titânio por reidratação de precursores comerciais, todos os métodos seguidos e não seguidos por impregnação de césio. Os carvões ativados utilizados como catalisadores foram de babaçu, coco da Bahia, osso de boi e dendê brutos e tratados com hidróxido de sódio. Os catalisadores foram caracterizados por microscopia eletrônica de varredura e transmissão, análise termogravimétrica, análise térmica diferencial, determinação de área superficial específica por análise textural de adsorção/dessorção de N2 a 77 K, espectroscopia de infravermelho, difração de raios X e dessorção à temperatura programada de CO2 e NH3. Os sítios básicos dos carvões foram quantificados pelo método de Boehm. Finalmente, o desempenho dos catalisadores foi avaliado na reação de Claisen-Schmidt entre Acetofenona e 4-Nitrobenzaldeído, sendo a conversão quantificada por cromatografia líquida de alta eficiência. O melhor catalisador foi o de carvão de babaçu tratado, cuja conversão alcançada foi de 92,38%.

The administration of enantiopure drugs brings advantages such as improved efficacy, more predictable pharmacokinetics and reduced toxicity from the point of view of the pharmaceutical area.[1] For this reason, a tremendous amount of supply and demand for enantiomeric pure compounds has been shown not only in market, but industry and academia.[2-4] According to the industry publication Genetic Engineering and Biotechnology News (GEN) in 2014, 22 billion dollars were accounted for enantiopure form of drugs such as Sovaldi® (Sofosbuvir), Crestor® (Rosuvastatin), and Advair® (fluticasone/salmeterol). The fact that one enantiomer can be pharmacologically effective whereas the other enantiomer can be inactive or display non-desirable activity, chiral resolution and asymmetric synthesis research has broken out in recent years to obtain one desired stereoisomer. Enormous amounts of well-organized and rationalized research results for higher enantiomeric selectivity and efficiency has been reported with diverse chiral ligands and transition metals in academia.[5-10] However novelty-driven results from academic area does not meet the requirement in industry field for the practical issue, especially tedious separation process that require high cost and effort. In addition, methodologies developed with privileged chiral ligands and transition metal complexes leave a concern like undesired residue of trace amount of toxic metals in the products. In this dissertation, two types of heterogeneous asymmetric catalyst were investigated to find the alternative that accommodates industrial requirement to obtain enantiomeric pure compounds and novelty-driven academic demands. Firstly, constructions of rationally designed metal organic frameworks (MOFs) using chiral BINOL-derived phosphoric acid ligands were achieved. Overall, catalytic reactions with ocMOFs showed lower enatioselectivity than their homogeneous counterparts, but one of the MOFs, ocMOF-1, was found to exhibit improved enantioselectivity than its homogeneous counterpart in the context of transfer hydrogenation reaction of benzoxazine. Lower enatioselectivity with ocMOFs was rationalized by the chiral environment change by the formation of frameworks in a computational study. In addition, self-supported heterogenization of chiral BINOL-phosphoric acid was achieved by the Yamamoto coupling reaction, and by using catalytically active ocPOP-1 having nanoscopic channels, enantioselectivity was obtained up to 48% in transfer hydrogenation of N-PMP ketimine. Although extension of substituent groups at 3, 3' positions was expected to bring enhanced steric hindrance and to influence to enantioselectivity positively, lack of spatially well-defined interactions induced by this chiral environment change might have lowered the enantiomeric selectivity of the catalytic reaction using ocPOP-1 than its counterpart.

Le méthanethiol est un intermédiaire clé dans la synthèse de la méthionine, un acide aminé largement utilisé dans l'industrie agro-alimentaire. / Methanethiol is a key intermediate in methionine synthesis, an amino-acid which is widely used in food-processing industry.

Le projet Européen UNIfHY a vu le jour dans une optique de production d’hydrogène à partir de biomasse pour le remplacement des énergies fossiles. La purification des gaz produits par la gazéification de la biomasse permet l’obtention d’hydrogène pur pour une utilisation dans les piles à combustible. Cette thèse s’inscrit dans ce projet avec pour but le développement de catalyseurs Fe/CeO2 et Cu/CeO2 déposés sur des supports de mousse céramique pour la réaction de conversion du gaz à l’eau à haute et basse températures, de manière à augmenter la production d’hydrogène et diminuer la perte de charge dans le système. Les principaux objectifs de la thèse sont la synthèse et les caractérisations des catalyseurs à base de fer et de cuivre, l’optimisation des conditions réactionnelles dans la limite du cadre fixé par le projet, la modélisation cinétique en présence des catalyseurs Fe/CeO2 et Cu/CeO2 et la transposition à grande échelle des catalyseurs pour une utilisation en réacteur pilote. / The UNIfHY European project was launched in an optic of producing hydrogen from biomass to replace fossil fuels. Purification of gases produced by biomass gasification allows obtaining pure hydrogen which can be used in fuel cells. This thesis takes part in this project with the development of Fe/CeO2 and Cu/CeO2 catalysts deposited on ceramic foam supports for high temperature and low temperature water gas shift reaction to increase the production of hydrogen and decrease the pressure drop in the system. The main objectives of this thesis are the synthesis and characterizations of iron and copper based catalysts, the optimization of reaction conditions within the limits of the framework set by the project, the kinetic modeling of the reaction in the presence of Fe/CeO2 and Cu/CeO2 catalysts and the scale-up of catalysts to use them in a pilot reactor.

A l’heure actuelle, la réduction de l’impact environnemental de l’industrie chimique est un enjeu majeur. Pour parvenir à ce but, le concept de Chimie Verte, né dans les années 90, cherche à promouvoir les réactions catalysées et notamment l’utilisation de catalyseurs hétérogènes. L’objectif de cette thèse a été d’utiliser des zéolithes, aluminosilicates microporeux, dopées avec un métal, pour des applications en synthèse organique, et notamment dans une synthèse multi-étapes. Ce type de catalyseur hétérogène est intéressant car il est potentiellement recyclable, facile à séparer du milieu réactionnel et stable.Afin d’atteindre notre objectif, la synthèse totale de l’acortatarine A a été effectuée en utilisant lors d’une étape, une zéolithe dopée avec du cuivre pour former un N-alcynylpyrrole et lors d’une autre étape, une zéolithe dopée avec de l’argent pour effectuer une spirocétalisation. Dans un premier temps, les méthodologies liées à ces deux réactions ont été étudiées puis dans un second temps, en se basant sur les connaissances acquises, la synthèse totale de l’acortatarine A a été effectuée avec succès. Il est à noter que lors de cette synthèse, deux étapes additionnelles ont été réalisées avec des zéolithes acides. A travers cette synthèse nous avons montré que les zéolithes dopées avec des métaux qui entrent pleinement dans le cadre de la Chimie Verte, peuvent être des outils très attractifs dans les synthèses multi-étapes. / Nowadays, reduction of the environmental impact of the chemical industry is a major challenge. To reach this goal, Green Chemistry was born in the 90s where catalysis plays an essential role especially with heterogenous catalysts. The aim of this PhD thesis was to use a support (zeolite) doped with a transition metal in organic synthesis and more specifically in a multi-step synthesis. These heterogeneous catalysts are interesting because they are potentially recyclable, easy to separate from reaction medium and stable. In order to reach our goal, we have performed the total synthesis of acortatarin A performing a step with a copper doped zeolite to form a N-alcynylpyrrole and in another step, a silver doped zeolite was used in a spiroketalization. The methodology linked to these two steps was firstly studied and then gained knowledge was successfully applied in the total synthesis of acortatarin A. Moreover, two additional steps were carried out with acidic zeolites during the synthesis. Through this total synthesis, we have demonstrated that metal-doped zeolites can be very attractiveto perform multi-step synthesis.

Le travail qui est décrit dans ce manuscrit de thèse traite de la chimie des superbases de type proazaphosphatranes, systèmes phosphorés bicycliques très utilisés en catalyse. L’objectif des investigations qui ont été menées à été d’ouvrir de nouvelles voies d’applications de ces catalyseurs. Afin de satisfaire cet objectif, plusieurs stratégies ont été envisagées. D’une part par la mise en confinement de la structure proazaphosphatrane et l’étude de l’influence de ce confinement sur la réactivité intrinsèque du proazaphosphatrane, et d’autre part par la catalyse en conditions bi-phasiques, que ce soit à l’interface entre une phase liquide et un solide ou entre deux phases liquides non-miscibles. Les recherches se sont orientées dans un premier temps sur la synthèse et la caractérisation complète d’un proazaphosphatrane supramoléculaire, obtenu par la fonctionnalisation par un proazaphosphatrane de la cavité supramoléculaire d’un récepteur macrobicyclique. Les séparations semi-préparatives des deux énantiomères d’un intermédiaire et de la molécule phosphorée finale ont également été réalisées, séparations qui ont permis de réaliser l’attribution des configurations absolues des deux structures macrobicycliques. La synthèse d’une famille de catalyseurs de type proazaphosphatrane supportés sur silice mésoporeuse a ensuite été réalisée, suivie de sa caractérisation texturale et structurale par les procédés physico-chimiques habituels, et enfin de sa mise en application dans des réactions d’intérêts de la synthèse organique. En dernier lieu, l’exploitation de la forme acide conjuguée des proazaphosphatranes, dite forme azaphosphatrane, dans des réactions de catalyse par transfert de phase a été entreprise. Il a ainsi put être démontré leur activité en tant qu’agent de transfert dans le cadre de quatre réactions significatives de la catalyse par transfert de phase en version racémique. Ce travail de thèse s’est finalement terminé par une ouverture vers la catalyse par transfert de phase en version asymétrique, par le biais de l’utilisation d’azaphosphatranes chiraux énantiopurs. / The work described in this PhD thesis deals with the chemistry of proazaphosphatrane-type superbases, which are highly reactive bicyclic phosphorous systems largely applied in catalysis. The main goal of these investigations was to devise new applications for their use in catalysis. In this way, several strategies were followed, with an emphasis on their molecular confinement and use in interfacial catalytic systems. In the first part, the manuscript describes the synthesis and characterisation of a supramolecular proazaphosphatrane obtained via the enclosing of a proazaphosphatrane moiety in a hemicryptophane-type macrobicyclic cavity. In parallel, the semi-preparative scale resolution of two macrobicyclic intermediates allowed us to assign their absolute configurations. In the second part, the synthesis and characterisation of a new class of superbases supported on mesoporous silica was achieved. The synthesis was followed by their application in base-catalysed organic reactions. The last part reports the use of their conjugate acids, or azaphosphatranes, in phase transfer catalysis. Their usefulness as achiral phase transfer agents in four relevant reactions was thus determined. The thesis ends with an introduction into asymmetric phase transfer catalysis, using enantiopure azaphosphatranes.

L'objectif de ce travail était double : obtenir des informations sur le lien structure/réactivité dans les nanoalliages et évaluer l'impact de l'addition d'or sur les propriétés catalytiques de métaux actifs en hydrogénation. Des nanoparticules bimétalliques Au-Pd et Au-Rh ont été synthétisées et supportées principalement sur des nanobâtonnets TiO2 rutile, caractérisées par différentes techniques d'analyse (DLS, UV-Vis, HR-(S)TEM, XRD, XPS et CO-FTIR), et évaluées dans deux réactions d'hydrogénation. Les catalyseurs modèles ont été principalement préparés par voie colloïdale suivie d'une immobilisation sur le support et d'un post-traitement consistant à éliminer le surfactant sans détruire la structure des nanoparticules. Les particules Au-Pd (3-5 nm) possèdent une structure alliée de type solution solide. La structure des particules Au-Rh (3-5 nm), système immiscible en volume, est plus hétérogène, avec différentes configurations en fonction du post-traitement effectué : coeur-coquille, ségrégation de phases de type « Janus » et alliage à l'échelle atomique en faible proportion. Les catalyseurs bimétalliques ont été testés en hydrogénation de la tétraline en présence de soufre et en hydrogénation sélective du cinnamaldéhyde, dans les deux cas sous haute pression d'hydrogène, et comparés à leurs homologues monométalliques. En hydrogénation du cinnamaldéhyde, un effet considérable du traitement post-synthèse sur l'activité et sélectivité est mis en évidence. Les catalyseurs fraichement synthétisés montrent une sélectivité élevée en hydrocinnamaldéhyde alors que les traitements de réduction et de calcination-réduction diminuent l'activité pour les échantillons AuRh les plus riches en Rh. En hydrogénation de la tétraline, l'alliage avec l'or a pour effet de diminuer l'activité mais d'améliorer la stabilité des systèmes à base de Pd et Rh en présence de soufre, en augmentant, par effet électronique, la barrière de chimisorption du soufre ou de sulfuration / The objectives of this work were to gain an insight into the structure-selectivity relationships in nanoalloys and to evaluate the impact of gold addition on the catalytic properties of active metals in hydrogenation reactions. For this purpose, bimetallic Au-Pd and Au-Rh nanoparticles were synthesized and supported (mostly) on rutile TiO2 nanorods before being structurally characterized by various techniques (DLS, UV-Vis, HR-(S)TEM, XRD, XPS, and CO-FTIR) and evaluated in two hydrogenation reactions. The model catalysts were mainly prepared using a colloidal method and immobilized on the support. Post-treatments were carried out in order to eliminate the surfactant used during the synthesis, with minimal impact on the nanoparticle structure. The influence of the synthesis parameters on the nanoparticle structure and catalytic properties was evaluated. The Au-Pd particles (3-5 nm) exhibit an alloyed solid solution structure. The structure of the bulk-immiscible Au-Rh particles (3-5 nm) is more heterogeneous, with several structural configurations depending on the post-treatment: core-shell, Janus-type phase segregation, and atomic-scale alloyed structure to a small extent. The catalysts were tested for tetralin hydrogenation in the presence of sulfur (0-100 ppm H2S) and for the selective hydrogenation of cinnamaldehyde, both under high hydrogen pressure. The bimetallic systems were compared to their monometallic counterparts. The post-synthesis treatments have a dramatic impact on activity and selectivity in cinnamaldehyde hydrogenation. The fresh catalysts exhibit a high selectivity toward hydrocinnamaldehyde, whereas reduction and calcination-reduction mainly decrease the activity of Rh-rich Au-Rh samples. For tetralin hydrogenation, gold decreases the activity but improves the stability of Pd and Rh-based systems in the presence of sulfur through electronic effects increasing sulfur chemisorption or sulfidation barriers

Orientador: Celso Valentim Santilli / Banca: Leila Aparecida Chiavacci Favorin / Banca: Eduardo Ferreira Molina / Resumo: Neste trabalho a metodologia sol-gel foi utilizada para a preparação de materiais híbridos orgânico-inorgânicos (HOI) à base de óxido de poli-etileno (PEO), ligado de forma covalente com o agente acoplador 3(isocianatopropil) - trietoxisilano (IsoTREOS) conjugados com um material zeolítico do tipo MFI, visando aplicações como catalisador para a reação de acetilação do glicerol e assim agregar valor a esse coproduto gerado na produção do biodiesel. O objetivo desta dissertação é demonstrar que o sinergismo entre híbridos do tipo siloxano-poliéter e as zeólitas pode ser explorado na produção de hidrogéis com atividade catalítica. As análises por Microscopia Eletrônica de Varredura (MEV) evidenciaram a homogeneidade na dispersão do material zeolítico na matriz híbrida Os difratogramas de raios-X apresentaram os picos característicos da estrutura cristalina da zeolita ZSM-5 após a conjugação com a matriz U-PEO. Os resultados de Calorimetria Diferencial de Varredura (DSC) revelaram que não ocorre uma mudança significativa na temperatura de transição vítrea (Tg), após a conjugação da matriz híbrida com a zeólita e revelaram uma diminuição do pico endotérmico associado à fusão dos domínios cristalinos do PEO1900, indicando uma possível interação matriz-zeólita. As análises por Espectroscopia no Infravermelho com Transformada de Fourier (FTIR) confirmaram a interação entre a matriz híbrida e a zeólita pelo deslocamento das bandas associadas ao oxigênio tipo éter não coordenado. Medid... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: In this work the sol-gel methodology was used for the preparation of organic-inorganic hybrid (HOI) materials based on polyethylene oxide (PEO) - covalently bonded with the coupling agent 3 (isocyanatopropyl) triethoxysilane (IsoTREOS) conjugate with a zeolitic material of the MFI type, aiming at applications as catalyst for glycerol acetylation reaction and thus add value to this byproduct generated in biodiesel production. The objective of this dissertation is to demonstrate that the synergism between siloxane-polyether hybrids and zeolites can be explored in the production of catalytic activity hydrogels. Scanning Electron Microscopy (SEM) analyzes showed homogeneity in the dispersion of zeolite material in the hybrid matrix. XDR patterns showed the characteristic peaks of the ZSM-5 zeolite crystal structure after conjugation with the U-PEO matrix. Differential Scanning Calorimetry (DSC) results revealed that no significant change in glass transition temperature (Tg) occurs after conjugation of hybrid matrix with zeolite and revealed a decrease in endothermic peak associated with fusion of crystalline domains of PEO1900., indicating a possible matrix-zeolite interaction. Fourier Transform Infrared Spectroscopy (FTIR) analyzes confirmed the interaction between the hybrid matrix and zeolite by shifting the bands associated with uncoordinated ether oxygen. Small-angle X-ray Scattering (SAXS) measurements showed that the starting reagents in the solketal production reaction w... (Complete abstract click electronic access below) / Mestre