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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

S?ntese, caracteriza??o e estudo cin?tico da degrada??o de quitosana impregnada em SBA-15

Santos, Adriana Paula Batista dos 15 March 2012 (has links)
Made available in DSpace on 2014-12-17T15:41:59Z (GMT). No. of bitstreams: 1 AdrianaPBS_DISSERT.pdf: 2596487 bytes, checksum: f09071ef3141cb36b73492e4246e301b (MD5) Previous issue date: 2012-03-15 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico / The recent interest in obtaining functionalized nanoporous materials for applications such as heterogeneous catalysts and adsorption of CO2 has increased today. In the latter application, the introduction of amino groups such as present in the chitosan (CS), in the nanoporous materials like SBA-15 to generate specific interactions with CO2 has gained importance. In this work were performed to hydrothermal synthesis of SBA-15 and subsequent impregnation of the CS in the support mesoporous by the method of the wet impregnation. The materials were characterized by TG/DTG, DSC, XRD, SEM, FTIR and adsorption / desorption of N2. The XRD showed that the ordered structure of the support SBA-15 was preserved after the impregnation and calculations have shown that the average pore diameter (Dp) and / or the average wall thickness (wt) have been changed due to introduction of the CS in the samples functionalized. The curves of TG and DSC data corroborates the XRD, indicating the presence of CS in the nanoporous structure of SBA-15, as well as micrographs of samples, which allowed the display state of aggregation of the material obtained. The characteristics of bands absorption in the region of the CS in the FTIR were identified and interpreted in the samples functionalized, confirming the further characterization. Measurements showed that the BET surface area decreases in the functionalized samples, indicating the successive incorporation of the polymer in the nanoporous support. The activation energy apparent (Ea) for the process of thermal degradation of CS in the impregnated support was determined by the methods of kinetic freedom Vyazovkin and Ozawa-Flynn-Wall with the results indicating that the sample functionalized CS/SBA-15 2,5 % was decrease of the Ea in their degradation of about 10% compared to 1,0 % CS/SBA-15 sample / O recente interesse em se obter materiais nanoporosos funcionalizados para aplica??es como catalisadores heterog?neos e na adsor??o de CO2 tem aumentado atualmente. Nesta ?ltima aplica??o, a introdu??o de grupos aminas, como os presentes na quitosana (CS), em materiais nanoporosos do tipo SBA-15 para gerar intera??es espec?ficas com o CO2 tem ganhado import?ncia. Assim, neste trabalho foram realizadas a s?ntese hidrot?rmica do SBA- 15 e posterior impregna??o da CS no suporte mesoporoso atrav?s do m?todo de impregna??o por via ?mida. Os materiais obtidos foram caracterizados por meio de TG/DTG, DSC, DRX, MEV, FTIR e adsor??o/dessor??o de N2. Os resultados de DRX indicaram que a estrutura ordenada do suporte SBA-15 foram preservada ap?s a impregna??o e os c?lculos mostraram que o di?metro m?dio do poro (Dp) e/ou espessura m?dia da parede (wt) foram alterados devido a introdu??o da CS nas amostras funcionalizadas. As curvas de TG e DSC corroboraram com os dados de DRX, indicando a presen?a da CS na estrutura mesoporosa do SBA-15, assim como as micrografias das amostras funcionalizadas, que possibilitou visualizar o estado de agrega??o do material obtido. As bandas caracter?sticas de absor??o da CS da regi?o IV foram identificadas e interpretadas nas amostras funcionalizadas, confirmando as outras caracteriza??es. As medidas de BET mostraram que a ?rea superficial diminui nas amostras funcionalizadas, indicando a sucessiva incorpora??o do pol?mero no suporte nanoporoso. A energia de ativa??o aparente (Ea) do processo de degrada??o t?rmica da CS impregnada no suporte foi determinada por meio dos m?todos de cin?tica livre de Vyazovkin e de Ozawa-Flynn-Wall com os resultados indicando que a amostra funcionalizada CS/SBA-15 2,5 % teve uma diminui??o da Ea para a sua degrada??o de aproximadamente de 10% em rela??o a amostra de CS/SBA-15 1,0 %

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