Oxi̇me deri̇vati̇ves new precursors syntheses used i̇n supercri̇ti̇cal deposi̇ti̇on
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Abstract (EN)
In the thesis, new vic-oxime derivative ligand and metal complexes (precursors) have been prepared and used for Pd deposition on SBA-15 based silica, which can be used for supercritical carbon dioxide deposition technique. For this purpose, the oxime compound is coupled with fluorine alkyl group and Pd (II) complexes of the ligands obtained are prepared. The solubilities of the synthesized complexes (precursor) in scCO2 were examined at different temperatures and pressures. In the light of the results obtained, the effect of solubility of electronic and steric effects of substituent groups on the ligand was investigated. The effect on the deposition of amphi isomer, which is more unstable than the stable isomer and anti isomer in oximes, is discussed. The structures of synthesized ligand and metal complexes were elucidated by analytical methods such as FT-IR, 1H, 19F NMR, elemental analysis, mass spectroscopy, magnetic susceptibility, UV-Vis. Silica supported metal nanoparticles' surfaces were analyzed by ICP-OES for determination of % Pd, TEM and SEM for determination of particle size and distribution and XRD for determination of metal forms that have been present. In the last step of the project, silica supported metal nanoparticles' catalytic activity was tested at Suzuki-Miyaura reactions over bromobenzene and phenylboronic acid reactions and products that have been obtain were analyzed by gas chromatography (GC). When the obtained data were analyzed it was concluded that the conversion efficiencies of the catalysts obtained from the complexes of the anti-vic-dioximines were better than the catalysts obtained from the amphi-forms. Catalyst yields were determined to be between 60-100% in 5 hours.
Author
Özge Atış
How to Cite
Özge Atış (Master Thesis). Oxi̇me deri̇vati̇ves new precursors syntheses used i̇n supercri̇ti̇cal deposi̇ti̇on, 2018, Çukurova University.
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