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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Design of highly selective platinum nanoparticle catalysts for the aerobic oxidation of KA-Oil using continuous-flow chemistry Arran M. Gill , Christopher Hinde , Rowan K. Leary , Matthew Potter , Andrea Jouve , Peter Wells , Paul A. Midgley , John M. Thomas , Robert Raja Chemsuschem DOI: 10.1002/cssc.201501264 Diamond Proposal Number(s): [8071] Show Abstract ▼ Abstract: Highly active and selective aerobic oxidation of KA-oil to cyclohexanone (precursor for adipic acid and ɛ-caprolactam) has been achieved in high yields using continuous-flow chemistry by utilizing uncapped noble-metal (Au, Pt & Pd) nanoparticle catalysts. These are prepared using a one-step in situ methodology, within three-dimensional porous molecular architectures, to afford robust heterogeneous catalysts. Detailed spectroscopic characterization of the nature of the active sites at the molecular level, coupled with aberration-corrected scanning transmission electron microscopy, reveals that the synthetic methodology and associated activation procedures play a vital role in regulating the morphology, shape and size of the metal nanoparticles. These active centers have a profound influence on the activation of molecular oxygen for selective catalytic oxidations.	Feb 2016
B18-Core EXAFS	Utilizing benign oxidants for selective aerobic oxidations using heterogenized platinum nanoparticle catalysts Christopher Hinde , Arran M. Gill , Peter Wells , T. S. Andy Hor , Robert Raja Chempluschem DOI: 10.1002/cplu.201500195 Diamond Proposal Number(s): [8071] Show Abstract ▼ Abstract: By using platinum nanoparticle catalysts that are generated in situ by extrusion from a porous copper chlorophosphate framework, the role of oxidants in the selective oxidation of benzyl alcohol to benzaldehyde was evaluated, with a view to establishing structure–property relationships. With a detailed study of the kinetic properties of the oxidation reaction, it has been determined that the aerobic oxidation pathways progress with lower levels of product selectivity and higher activation energies (72.4 kJ mol−1) than the peroxide-based ones (23.6 kJ mol−1); affording valuable insights in the design of solid catalysts for selective oxidation reactions. Furthermore, through the use of X-ray absorption spectroscopy, the effect of calcination temperature on the degree of extrusion and its influence on nanoparticle formation have been evaluated, leading to the establishment of structure–activity correlations between the observed activation energies and the proportion of nanoparticle species generated.	Jun 2015
B18-Core EXAFS	Elucidating structure-property relationships in the design of metal nanoparticle catalysts for the activation of molecular oxygen Christopher Hinde , Davide Ansovini , Peter Wells , Gillian Collins , Sivan Van Aswegen , Justin D. Holmes , T. S. Andy Hor , Robert Raja Acs Catalysis 5 (6), 3807 - 3816 DOI: 10.1021/acscatal.5b00481 Diamond Proposal Number(s): [8071] Show Abstract ▼ Abstract: A novel synthetic strategy for the design of metal nanoparticles by extrusion of anionic chloride precursors from a porous copper chlorophosphate framework has been devised for the sustainable aerobic oxidation of vanillyl alcohol (4-hydroxy-3-methoxybenzyl alcohol) to vanillin (4-hydroxy-3-methoxybenzaldehyde) using a one-step, base-free method. The precise nature of the Au, Pt, and Pd species has been elucidated for the as-synthesized and thermally activated analogues, which exhibit fascinating catalytic properties when subjected to diverse activation environments. By employing a combination of structural and spectroscopic characterization tools, it has been shown that analogous heat treatments have differing effects on extrusion of a particular metal species. The most active catalysts in this series of materials were the extruded Pt nanoparticles that were generated by reduction in H2, which exhibit enhanced catalytic behavior, when compared to its Au or Pd counterparts, for industrially significant, aerobic oxidation reactions.	Jun 2015

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