Propriedades analíticas e eletroanalíticas de um silsesquioxano nanoestruturado organofuncionalizado
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2011-01-20
Autores
Soares, Layciane Aparecida [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
O presente trabalho apresenta a preparação de um silsesquioxano nanoestruturado, o cloropropilsilsesquioxano (S) que foi organofuncionalizado com os seguintes agentes modificadores: 4-amino-3-hidrazinico-5-mercapto-1,2,4-triazol (Purpald®) e o 4-amino-5-4(piridil)-4H-1,2,4-triazol-3-tiol (APTT), os materiais obtidos dessa funcionalização foram descritos como SP e SA, respectivamente. Os materiais SP e SA foram caracterizados por diversas técnicas espectroscópicas: Espectroscopia na região do infravermelho (FT-IR), Ressonância magnética nuclear 29Si e 13C no estado sólido (RMN), Difração de Raios- X (DRX), Espectroscopia de Energia Dispersiva de Raios X (EDX), Termogravimetria e Análise Térmica Diferencial (TG – DTA). Após a devida caracterização, realizaram-se estudos de adsorção de íons metálicos (Cu2+, Cd2+ e Ni2+) nos sítios ativos do SA, porém, curiosamente não se observou a mesma capacidade de sorção pelo SP. Diferentes meios foram estudados no processo de adsorção dos íons metálicos supracitados: aquoso, etanólico 99% e etanólico 42%, determinando-se o tempo de equilíbrio de adsorção, que para ambos os meios e metais esse tempo máximo foi em média 35 min. Determinado o tempo de equilíbrio de adsorção dos íons metálicos em cada sistema, determinou-se a capacidade específica de sorção (Nfmax) através de isotermas de adsorção. Para o Cu2+, os valores de Nf foram: meio aquoso (3,09 × 10-4 mol g-1), etanólico 42% (1,03 × 10-4 mol g-1) e etanólico 99% (1,86 × 10-4 mol g-1), com concentrações de íons Cu2+ variando de 1,74 a 29,64 mol L-1. Os valores encontrados para o Ni2+ foram: em meio aquoso (2,11 × 10-4 mol g-1), etanólico 42% (0,97 × 10-4 mol g-1) e etanólico 99% (1,05 × 10-4 mol g-1), com concentrações de íons Ni2+ variando de 2,25 a 33,18 mol L-1. Para os íons cádmio não foram...
This work presents the preparation of a nanostructured silsesquioxane, the cloropropilsilsesquioxano (S) that was organofunctionalised with the following modifying agents: 4-amino-3-hydrazino 5 - mercapto 1,2,4 triazole (Purpald ®) and 4- amino-5-4 (pyridyl)-4H-1,2,4-triazole-3-thiol (APTT), the materials obtained of the functionalization were described as SP and SA, respectively. The materials SA and SP were characterized by various spectroscopic techniques such as spectroscopy in the region of infrared (FTIR), nuclear magnetic resonance 29Si and 13C solid-state (NMR), X-ray diffraction (XRD), Energy Dispersive Spectroscopy Rays (EDS), Thermogravimetry and Differential Thermal Analysis (TG - DTA). After proper characterization, were carried studies on adsorption of metallic ions such as Cu2+, Ni2+ and Cd2+ in the active sites of SA, but curiously did not observe the same sorption capacity of the SP. Different methods were studied in the adsorption of metal ions above: aqueous, 99% ethanolic and 42% ethanolic, determining the adsorption equilibrium time, which for both means and metals the maximum time averaged 35 min. After determining the adsorption equilibrium time of metal ions in each system, we determined the specific sorption capacity (Nfmax) through adsorption isotherms. For Cu2+, the values of Nf were: aqueous solution (3.09 × 10-4 mol g-1), 42% ethanolic (1.03 × 10-4 mol g-1) and 99% ethanolic (1.86 × 10-4 mol g-1), with Cu2 + ion concentrations ranging from 1.74 to 29.64 mol L-1. The values obtained for the Ni2+ were: aqueous solution (2.11 × 10-4 mol g-1), 42% ethanolic (0.97 × 10-4 mol g-1) and 99% ethanolic (1.05 × 10-4 mol g-1), with Ni2 + ion concentrations ranging from 2.25 to 33.18 mol L-1. For the cadmium ions were not observed saturation of adsorption sites in the concentration range studied, not getting the maximum... (Summary complete electronic access click below)
This work presents the preparation of a nanostructured silsesquioxane, the cloropropilsilsesquioxano (S) that was organofunctionalised with the following modifying agents: 4-amino-3-hydrazino 5 - mercapto 1,2,4 triazole (Purpald ®) and 4- amino-5-4 (pyridyl)-4H-1,2,4-triazole-3-thiol (APTT), the materials obtained of the functionalization were described as SP and SA, respectively. The materials SA and SP were characterized by various spectroscopic techniques such as spectroscopy in the region of infrared (FTIR), nuclear magnetic resonance 29Si and 13C solid-state (NMR), X-ray diffraction (XRD), Energy Dispersive Spectroscopy Rays (EDS), Thermogravimetry and Differential Thermal Analysis (TG - DTA). After proper characterization, were carried studies on adsorption of metallic ions such as Cu2+, Ni2+ and Cd2+ in the active sites of SA, but curiously did not observe the same sorption capacity of the SP. Different methods were studied in the adsorption of metal ions above: aqueous, 99% ethanolic and 42% ethanolic, determining the adsorption equilibrium time, which for both means and metals the maximum time averaged 35 min. After determining the adsorption equilibrium time of metal ions in each system, we determined the specific sorption capacity (Nfmax) through adsorption isotherms. For Cu2+, the values of Nf were: aqueous solution (3.09 × 10-4 mol g-1), 42% ethanolic (1.03 × 10-4 mol g-1) and 99% ethanolic (1.86 × 10-4 mol g-1), with Cu2 + ion concentrations ranging from 1.74 to 29.64 mol L-1. The values obtained for the Ni2+ were: aqueous solution (2.11 × 10-4 mol g-1), 42% ethanolic (0.97 × 10-4 mol g-1) and 99% ethanolic (1.05 × 10-4 mol g-1), with Ni2 + ion concentrations ranging from 2.25 to 33.18 mol L-1. For the cadmium ions were not observed saturation of adsorption sites in the concentration range studied, not getting the maximum... (Summary complete electronic access click below)
Descrição
Palavras-chave
Adsorção, Voltametria, Silsesquioxano, Funcionalização, Voltametria cíclica, Eletrodo quimicamente modificado, Silsesquioxane, Functionalization, Adsorption, Cyclic voltammetry, Chemically modified electrode
Como citar
SOARES, Layciane Aparecida. Propriedades analíticas e eletroanalíticas de um silsesquioxano nanoestruturado organofuncionalizado. 2011.. 130 f. Dissertação (mestrado) - Universidade Estadual Paulista, Faculdade de Engenharia de Ilha Solteira, 2011..