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Dalton Trans. 2010 Mar 21;39(11):2842-54. doi: 10.1039/b920853d. Epub 2010 Feb 5.

Superparamagnetic gamma-Fe2O3@SiO2 nanoparticles: a novel support for the immobilization of [VO(acac)2].

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REQUIMTE, Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre, s/n, 4169-007, Porto, Portugal.


This work reports a detailed investigation about the physicochemical properties of superparamagnetic gamma-Fe(2)O(3) nanomaterial synthesized by the co-precipitation method and coated with two silica shells, and its application as support for the immobilization of oxovanadium(IV) acetylacetonate ([VO(acac)(2)]). The influence of the silica coatings on the surface composition and physicochemical interactions of the core-shell nanocomposites is discussed based on the combination of several techniques: electron microscopy techniques (SEM and TEM with EDS), DLS, powder XRD, XPS, FTIR and magnetic characterization. The identity of the iron oxide, gamma-Fe(2)O(3), was confirmed by XPS, FTIR and by the Rietveld refinement of the PXRD pattern. The results obtained by electron microscopy techniques, XRD and magnetization indicated that the gamma-Fe(2)O(3) nanoparticles are superparamagnetic and present an average size of approximately 6.5 nm. The first silica coating leads to a core-shell nanomaterial with an average particle size of 21 nm and upon the second coating, the average size increases to 240 nm. Magnetic measurements revealed that the silica-coated nanomaterials maintain the superparamagnetic state at room temperature, although with an expected reduction of the magnetization saturation due to the increase of the silica shell thickness. Furthermore, a numerical fit of the temperature dependence of magnetization was performed to determine the core size distribution and the effect of the silica coatings on the dipolar magnetic interactions. [VO(acac)(2)] was covalently immobilized on the surface of the silica-coated magnetic nanoparticles functionalized with amine groups, as confirmed by chemical analysis and XPS. In a proof-of-principle experiment, we demonstrated the catalytic performance of the novel magnetic hybrid nanomaterial in the epoxidation of geraniol, which presented high selectivity towards the 2,3-epoxygeraniol product and easy recovery by magnetic separation.

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