Neste trabalho foi realizada a síntese da SBA-15, a funcionalização com o agente sili- lante 3 – cloropropiltrimetóxisilano, além da síntese dos complexos e a ancoragem destes no suporte SBA-15. Com os resultados obtidos pode-se concluir que:
A formação da SBA-15, foi confirmada através das análises de difração de raios-X, em que foram observados os três picos de difração cujos Índices de Miller são (100), (110) e (200), característicos de materiais mesoporosos, a elevada área superficial (517, 47 m2/g), volume de poros (0,74 cm3/g) na análise de adsorção e dessorção de N2, na espectroscopia de absorção na região do infravermelho foram observadas bandas características da sílica em 3449 cm-1 referentes às vibrações de estiramento dos grupos hidroxilas internos e externos, estiramentos simétrico e assimétrico Si-O-Si em 1085 e 808 cm-1, respectivamente e defor- mação angular em 468 cm-1 e a eliminação da água fisissorvida em 92°C na análise termo- gravimétrica (TG/DTG).
A comprovação de que o material foi funcionalizado com o agente sililante 3- cloropropiltrimetóxisilano se deu através do difratograma de raios-x, em que foram observa- dos três picos característicos dos materiais mesoporosos com reduções na intensidade dos picos em maior ângulo provavelmente causadas devido ao efeito do preenchimento do poro dos canais da SBA-15. As porcentagens dos elementos, sílica (92%) e Cloro (8%) presentes no material. A diminuição na área superficial (333,4 m2/g) e no volume de poros (0,46 cm3/g) na adsorção e dessorção de N2 comprovam o sucesso da organofuncionalização. A reação en- tre Si-OH e o cloropropiltrimetóxisilano ficou evidenciada com o decréscimo na intensidade da banda de absorção em 3469 cm-1 e a presença da banda em 2954 cm-1 referente ao estira- mento C-H. A decomposição do material orgânico em 300 °C atribuída à molécula orgânica ancorada na superfície do material na análise termogravimétrica (TG/DTG).
Foi possível o estudo e preparação dos complexos com Base de Schiff com níquel (II):
Ni(L1), em que L1 = dietilenotriamina, Ni(L2), sendo L2 = 3,3’ iminobispropilamina e
[Ni(L3)] em que L3 = N-(2-aminoetil)-1,3- propanodiamina). Após sintetizados os complexos foram caracterizados para constatar a formação da Base de Schiff e da coordenação do ligante ao metal. A análise elementar (CHN) sugeriu a fórmula molecular para os complexos:
[Ni(C18H19N3O2)].2CH3COO.H2O, [Ni(C20H23N3O2)(2Cl)].2H2O,
[Ni(C19H18N3O2(2Cl)].3H2O, sendo L1= C18H19N3O2, L2= C20H23N3O2 e L3 = C19H18N3O2; Nos espectros de absorção na região do UV-visível dos complexos nas concentrações 1×10-3
mol.L-1 e 1×10-2 mol.L-1 em DMSO, a coordenação metal –ligante foi constatada pela presen- ça das bandas de transferência de carga na região de 369 – 391 nm e bandas d-d em 569 e 862 nm. Nos espectros de absorção na região do infravermelho as bandas de deformação axial C=N que (caracteriza a Base de Schiff), C-O e C=C se encontram deslocadas para menores números de onda quando comparada a dos ligantes evidenciando a formação da Base de Schiff e coordenação do metal – ligante.
A ancoragem dos complexos na SBA-15 funcionalizada com cloropropiltrimetóxisilano ocorreu através de uma reação de substituição nucleofílica. Após a ancoragem os materiais foram caracterizados por: Difração de raios-X, em que foram observados os três picos de di- fração cujos índices de Miller são (100), (110) e (200), característicos de materiais mesoporo- sos, mostrando que mesmo após a ancoragem, os materiais não perderam suas características estruturais. As porcentagens dos elementos no [Ni(L1)]SBA-15 (4,4 % níquel, 95,6 % síli- ca), [Ni(L2)]SBA-15 (8,6 % níquel, 85,9 % sílica e 5,5 % cloro) e [Ni(L3)] SBA-15 (2,5 % níquel, 92,3 % sílica e 5,2% cloro), mostraram que os complexos foram ancorados na sílica. Na análise de adsorção e dessorção de N2 dos materiais sintetizados foram obtidas isotermas do tipo IV, histereses tipo H1, característicos de materiais mesoporosos. O decréscimo na área superficial, volume de poros, diâmetro de poros quando comparadas com a da SBA-15 con- firmam a presença de complexos nos poros da sílica. Nas curvas termogravimétricas TG/DTG da SBA-15, SBA-15 funcionalizada, dos complexos livres e dos complexos ancorados foram observados eventos de perda de água fisissorvida, água coordenada, aminas, aromáticos, li- gantes.
Nas análises termogravimétricas (TG/DTG) foi observado um aumento da estabilidade térmica dos materiais ancorados com complexos quando comparado aos complexos livres, pela saída dos ligantes em 671°C [Ni(L1)]SBA-15, 666°C [Ni(L2)]SBA-15 e 554°C [Ni(L3)]SBA-15, confirmando a presença do complexo nos poros da sílica, nos complexos livres [Ni(L1)], [Ni(L2)] e [Ni(L3)], são observadas a temperaturas menores 489, 507 e 453°C, respectivamente.
PROPOSTA PARA TRABALHOS FUTUROS
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