Síntese e caracterização de híbridos inorgânico-orgânicos funcionalizados com tiouréia e 2,2’-dipiridilamina: aplicação em adsorção de íons metálicos, pré-concentração e catálise
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Data
2013-02-28
Autores
Vieira, Eduardo Guimarães [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
Este trabalho descreve a síntese e caracterização da sílica gel 60 Å da Merck (SGP), com tamanho de partícula de 0,063-0,200 mm (70-230 mesh ASTM) funcionalizada com tiouréia-propil (SG-Pr-TIOU) e a síntese e caracterização da sílica gel e do silsesquioxano quimicamente modificados com 2,2’-dipiridilamina-propil grupos SG-Pr-DPA e T8-Pr-DPA respectivamente. Os materiais SG-Pr-TIOU e SG-Pr-DPA foram caracterizados por: espectroscopia na região do infravermelho (FTIR), ressonância magnética nuclear 29Si e 13C no estado sólido (RMN), microscopia eletrônica de varredura (MEV), análise elementar e análise de textura, já o nanomaterial T8-Pr-DPA foi caracterizado por: espectroscopia na região do infravermelho (FTIR), ressonância magnética nuclear 29Si e 13C no estado sólido (RMN) e análise elementar. Nos estudos de batelada determinou-se a dose de adsorvente na solução, efeito do pH e o tempo de equilíbrio, na qual para o material SG-Pr-TIOU a capacidade máxima de adsorção ocorreu em 60 mg de adsorvente em pH = 6 e o equilíbrio de adsorção foi alcançado em 30 minutos para todos os solventes e íons metálicos, enquanto que para o SG-Pr-DPA os resultados foram 10 mg, pH 5-6 e 14 minutos respectivamente, já para o T8-Pr-DPA 10 mg, pH 6 e 10 minutos respectivamente. O efeito do solvente na capacidade de adsorção deve a seguinte ordem cetônico > etanólico > aquoso. O efeito dos contra-íons Cl-, Br- e ClO4- foram estudados para os três materiais, na qual observou-se que para os três adsorventes a capacidade de adsorção seguiu a ordem: Cl- > Br- > ClO4-. Os modelos de Langmuir e pseudo-segunda-ordem foram os mais apropriados para descrever os dados de adsorção e cinética respectivamente do material SG-Pr-TIOU, enquanto que para os materiais SG-Pr-DPA e T8-Pr-DPA os modelos de Langmuir...
This work describes the synthesis and characterization of the silica gel 60 Å Merck (SGP), with particle size 0.063-0.200 mm (70-230 mesh ASTM) functionalized with thiourea-propyl (SG-Pr-THIO) and the synthesis and characterization of the silica gel and silsesquioxane chemically modified with 2,2'-dipyridylamine propyl groups SG-Pr-DPA and T8-Pr-DPA respectively. The materials SG-Pr-THIO and SG-Pr-DPA were characterized by infrared spectroscopy (FTIR), nuclear magnetic resonance 29Si and 13C solid state (NMR), scanning electron microscopy (SEM), elemental analysis and texture analysis, where as the T8-Pr-DPA was characterized by infrared spectroscopy (FTIR), nuclear magnetic resonance 29Si and 13C solid state (NMR) and elemental analysis. In the studies batch was determined dose of adsorbent in the solution, the effect of pH and time of equilibrium, in which for material to SG-Pr-THIO the maximum adsorption capacity was 60 mg of adsorbent at pH = 6 and the equilibrium adsorption was achieved in 30 minutes for all solvents and metal ions, while for the SG-Pr-DPA, results were 10 mg, pH 5-6 and 14 minutes respectively, while for T8-Pr-DPA 10 mg, pH 6 and 10 minutes respectively. It were studied also the maximum adsorption capacity for the solvents, where the maximum capacity occurred in acetone > ethanol > water. The effect of the counter ions Cl-, Br- and ClO4-were studied for the three materials, in which it was observed that for the three adsorbents for the adsorption capacity followed the order: Cl- > Br- > ClO4-. The Langmuir and pseudo-second-order models were the most suitable to describe of adsorption and kinetic data respectively of the SG-Pr-THIO, whereas for materials SG-Pr-DPA and T8-Pr-DPA Elovich and Langmuir models were the most suitable to describe the data of adsorption and kinetic. The values of free energy (E) of... (Complete abstract click electronic access below)
This work describes the synthesis and characterization of the silica gel 60 Å Merck (SGP), with particle size 0.063-0.200 mm (70-230 mesh ASTM) functionalized with thiourea-propyl (SG-Pr-THIO) and the synthesis and characterization of the silica gel and silsesquioxane chemically modified with 2,2'-dipyridylamine propyl groups SG-Pr-DPA and T8-Pr-DPA respectively. The materials SG-Pr-THIO and SG-Pr-DPA were characterized by infrared spectroscopy (FTIR), nuclear magnetic resonance 29Si and 13C solid state (NMR), scanning electron microscopy (SEM), elemental analysis and texture analysis, where as the T8-Pr-DPA was characterized by infrared spectroscopy (FTIR), nuclear magnetic resonance 29Si and 13C solid state (NMR) and elemental analysis. In the studies batch was determined dose of adsorbent in the solution, the effect of pH and time of equilibrium, in which for material to SG-Pr-THIO the maximum adsorption capacity was 60 mg of adsorbent at pH = 6 and the equilibrium adsorption was achieved in 30 minutes for all solvents and metal ions, while for the SG-Pr-DPA, results were 10 mg, pH 5-6 and 14 minutes respectively, while for T8-Pr-DPA 10 mg, pH 6 and 10 minutes respectively. It were studied also the maximum adsorption capacity for the solvents, where the maximum capacity occurred in acetone > ethanol > water. The effect of the counter ions Cl-, Br- and ClO4-were studied for the three materials, in which it was observed that for the three adsorbents for the adsorption capacity followed the order: Cl- > Br- > ClO4-. The Langmuir and pseudo-second-order models were the most suitable to describe of adsorption and kinetic data respectively of the SG-Pr-THIO, whereas for materials SG-Pr-DPA and T8-Pr-DPA Elovich and Langmuir models were the most suitable to describe the data of adsorption and kinetic. The values of free energy (E) of... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Tiouréia, Adsorção, Catalise, Thiourea
Como citar
VIEIRA, Eduardo Guimarães. Síntese e caracterização de híbridos inorgânico-orgânicos funcionalizados com tiouréia e 2,2’-dipiridilamina: aplicação em adsorção de íons metálicos, pré-concentração e catálise. 2013. 151 f. Dissertação (mestrado) - Universidade Estadual Paulista Júlio de Mesquita Filho, Faculdade de Engenharia de Ilha Solteira, 2013.