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Synthesis of Vic-Dioxime Palladium (II) Complex: Precursor for Deposition on SBA-15 in ScCO2

Authors: Asım Egitmen, Aysen Demir, Burcu Darendeli, Fatma Ulusal, Bilgehan Güzel


Synthesizing supercritical carbon dioxide (scCO2) soluble precursors would be helpful for many processes of material syntheses based on scCO2. Ligand (amphi-(1Z, 2Z)-N-(2-fluoro-3-(trifluoromethyl) phenyl)-N'-hydroxy-2-(hydroxyimino) were synthesized from chloro glyoxime and flourus aniline and Pd(II) complex (precursor) prepared. For scCO2 deposition method, organometallic precursor was dissolved in scCO2 and impregnated onto the SBA-15 at 90 °C and 3000 psi. Then the organometallic precursor was reduced with H2 in the CO2 mixture (150 psi H2 + 2850 psi CO2). Pd deposited support material was characterized by ICP-OES, XRD, FE-SEM, TEM and EDX analyses. The Pd loading of the prepared catalyst, measured by ICP-OES showed a value of about 1.64% mol/g Pd of catalyst. Average particle size was found 5.3 nm. The catalytic activity of prepared catalyst was investigated over Suzuki-Miyaura C-C coupling reaction in different solvent with K2CO3 at 50 oC. The conversion ratio was determined by gas chromatography.

Keywords: Nanoparticle, nanotube, oximes, precursor, supercritical CO2.

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