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Síntese, caracterização de complexos de Base de Schiff com níquel (II) ancorados no material mesoporoso SBA-15

Síntese, caracterização de complexos de Base de Schiff com níquel (II) ancorados no material mesoporoso SBA-15

Maia, Danielle de Oliveira; Araújo, Aruzza Mabel de Morais; Guedes, Ana Paula de Melo Alves; Gondim, Amanda Duarte; Araujo, Antonio Souza de; Lemos, Francisco das Chagas Dantas de; Dockal, Edward Ralph;

Completo:

SBA-15 são materiais mesoporosos, que possuem uma rede de canais e poros de tamanho bem definido na escala nanométrica, além de outras características, tais como, elevada estabilidade térmica e área superficial. Essa arquitetura particular de poros torna esses materiais promissores na área de ancoramento de uma variedade de compostos na matriz da sílica resultando em aplicações nas diversas áreas, dentre elas, na catálise. Nesse trabalho, foram sintetizados complexos de Base de Schiff com níquel (II) para serem ancorados na SBA-15 funcionalizada com 3-cloropropiltrimetóxisilano realizando um estudo da estabilidade térmica desses compostos. Após a síntese dos complexos, estes foram caracterizados por análise elementar (CHN), espectroscopia de absorção na região do infravermelho e análises térmicas (TG/DTG). A análise elementar sugere que os complexos apresentam as seguintes fórmulas químicas gerais: [Ni(C18H19N3O2)].2CH3COO.H2O, [Ni(C20H23N3O2)(2Cl)].2H2O, sendo L1= C18H19N3O2, L2= C20H23N3O2. Após caracterização dos complexos, confirmando a coordenação metal – ligante, estes foram ancorados no material mesoporoso. A caracterização desses materiais foi realizada por difração de raios - X, adsorção e dessorção de N2 e análises térmicas (TG/DTG). No DRX foram observados três picos principais de difração, cujos índices de Miller são (100), (110) e (200), mostrando que mesmo após a ancoragem, os materiais mesoporosos não perderam suas características estruturais. Através da adsorção e dessorção de N2, foram observadas que os materiais apresentaram isoterma do tipo IV e histerese do tipo H1 característicos dos materiais mesoporos. Na espectroscopia de absorção na região do infravermelho, os materiais ancorados apresentaram bandas características dos ligantes (Base de Schiff) e da sílica evidenciando o sucesso da ancoragem. Na análise térmica, foram observadas a decomposição de água adsorvida, água coordenada, aminas, aromáticos, ligantes, cloropropiltrimetóxisilano e também um aumento na estabilidade térmica (eliminação dos ligantes) das sílicas ancoradas [Ni(L1)]SBA-15 e [Ni(L2)]SBA-15 quando comparado aos complexos livres, evidenciando o sucesso da ancoragem dos complexos na peneira molecular.

Completo:

SBA-15 materials are mesoporous, having a network of channels and well defined pore size in the nanometer range, as well as other features such as high thermal stability and surface area. This particular pore architecture makes these promising materials in the anchoring area of a variety of compounds in the silica matrix resulting in applications in several fields, among them, in catalysis. In this work, they synthesized Schiff Base complexes of nickel (II) to be anchored in the SBA-15 functionalized with 3-chloropropyltrimethoxysilane conducting a study of thermal stability of these compounds. After synthesis of the complexes, they were characterized by elemental analysis (CHN), absorption spectroscopy in the infrared region and thermal analysis (TG / DTG). Elemental analysis suggests that the complexes have the following general chemical formulas: [Ni(C18H19N3O2)]2CH3COO.H2O, [Ni(C20H23N3O2)(2Cl)] 2H2O, being C18H19N3O2 = L1, L2 = C20H23N3O2. After characterization of the complex, confirming the coordinating metal - ligand, these were anchored in the mesoporous material. The characterization of these materials was carried out by diffraction of X - ray adsorption and desorption of N2 and thermal analysis (TG / DTG). XRD analysis revealed three main diffraction peaks, whose Miller indices are (100), (110) and (200), showing that even after the anchoring, the mesoporous materials do not lose their structural characteristics. By N2 adsorption and desorption it was observed that the materials had type IV isotherm and type H1 hysteresis characteristic of mesoporous materials. In absorption spectroscopy in the infrared region, the materials showed characteristic bands of docked ligand (Schiff Base) and silica demonstrating the success of the anchor. In the thermal analysis, there were observed the decomposition of adsorbed water, coordinated water, amines, aromatics, ligands, chloropropyltrimethoxysilane, and also an increase in thermal stability (removal of ligands) of the silicas anchored [Ni(L1)] SBA-15 and [Ni(L2)] SBA-15 compared to free complexes, demonstrating the successful anchoring of complex molecular sieve.

Palavras-chave: SBA-15; Base de Schiff; Materiais Mesoporosos; Termogravimetria; DRX,

Palavras-chave: SBA-15; Schiff base; Mesoporous materials; thermogravimetry; DRX,

DOI: 10.5151/chenpro-5erq-am7

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Como citar:

Maia, Danielle de Oliveira; Araújo, Aruzza Mabel de Morais; Guedes, Ana Paula de Melo Alves; Gondim, Amanda Duarte; Araujo, Antonio Souza de; Lemos, Francisco das Chagas Dantas de; Dockal, Edward Ralph; "Síntese, caracterização de complexos de Base de Schiff com níquel (II) ancorados no material mesoporoso SBA-15", p. 665-674 . In: Anais do V Encontro Regional de Química & IV Encontro Nacional de Química [=Blucher Chemistry Proceedings].. São Paulo: Blucher, 2015.
ISSN 2318-4043, DOI 10.5151/chenpro-5erq-am7

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