Synthesis of Vic-Dioxime Palladium (II) Complex: Precursor for Deposition on SBA-15 in ScCO2
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.
Digital Object Identifier (DOI): doi.org/10.5281/zenodo.1127468Procedia APA BibTeX Chicago EndNote Harvard JSON MLA RIS XML ISO 690 PDF Downloads 838
 Y. Zhang, C. Erkey, “Preparation of supported metallic nanoparticles using supercritical fluids: a review,” J. Supercrit. Fluids, vol. 38, pp. 252, 2006.
 C. Erkey, “Preparation of metallic supported nanoparticles and films using supercritical fluid deposition,” J. Supercrit. Fluids, vol. 47, pp. 517, 2009.
 X.R. Ye, Y. Lin, C.M. Wai, “Decorating catalytic palladium nanoparticles on carbon nanotubes in supercritical cabon dioxide,” Chem. Commun., vol. 5, pp. 642, 2003.
 S.E. Bozbag, C. Erkey, “Supercritical deposition: Current status and perspectives for the preparation of supported metal nanostructures” J. Supercrit. Fluids, vol. 96, pp. 298, 2015.
 Lin, Chi-Kai, “Novel synthesis and characterization of precious-metal nanocatalysts for clean energy applications,” N. IL. Uni., pp. 128, 2011.
 S.K. Morley, P.C. Marr, P.B. Webb, A.R. Berry, F.J. Allison, G. Moldovan, P.D. Brown, S.M. Howdle, “Clean preparation of nanoparticulate metals in porous supports: a supercritical route,” J. Mater. Chem., vol. 12, pp. 1898, 2002.
 A. Bayrakceken, U. Kitkamthorn, M. Aindow and C. Erkey, “Decoration of multi-wall carbon nanotubes with platinum nanoparticles using supercritical deposition with thermodynamic control of metal loading” Scripta Materialia, 56, 101–103, 2007
 J. Baoa, H. Tianb, R. Tang, “Synthesis and characterization a novel europium(III)-β-diketonate complex with carbazole and triphenylamine moieties” Inorganica Chimica Acta, vol.401, pp.19–23, 2013.
 A.L. Dantas, P.D. Alves, D. Arando, M. Schmal, “Characterization of carbon supported Pd catalysts: Influence of electronic and particle size effects using reaction probes” Appl. Catal., vol 277, pp. 71-81, 2004.
 Hunt A. J., Budarin V. L., Comerford J. W., Parker H. L., Lazarov V. K., Breeden S.W., Macquarrie D. J., Clark J. H.. "Deposition of Palladium Nanoparticles in SBA-15 Templated Silica Using Supercritical Carbon Dioxide" Materials Letters vol.116, pp. 408–411, 2014.
 Cotugno, P., M. Casiello, A. Nacci, P. Mastrorilli, M. M. Dell’Anna and A.Monopoli. "Suzuki coupling of iodo and bromoarenes catalyzed by chitosan-supported Pd-nanoparticles in ionic liquids" Journal of Organometallic Chemistry vol. 752: pp.1-5, 2014.