Synthesis of high surface area CuMn2O4 by supercritical anti-solvent precipitation for the oxidation of CO at ambient temperature

Z.-R. Tang; S. A. Kondrat; C. Dickinson; J. K. Bartley; A. F. Carley; S. H. Taylor; T. E. Davies; M. Allix; M. J. Rosseinsky; J. B. Claridge; Z. Xu; S. Romani; M. J. Crudace; G. J. Hutchings

doi:10.1039/C1CY00064K

Synthesis of high surface area CuMn₂O₄ by supercritical anti-solvent precipitation for the oxidation of CO at ambient temperature

Z.-R. Tang,^a S. A. Kondrat,^a C. Dickinson,^b J. K. Bartley,^a A. F. Carley,^a S. H. Taylor,^a T. E. Davies,^a M. Allix,^b M. J. Rosseinsky,^b J. B. Claridge,^b Z. Xu,^b S. Romani,^b M. J. Crudace^c and G. J. Hutchings*^a

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^a Cardiff Catalysis Institute, School of Chemistry, Cardiff University, Main Building, Park Place, Cardiff, UK

^b Department of Chemistry, University of Liverpool, Crown Street, Liverpool, UK

^c Molecular Products Limited, Mill End, Thaxted, Essex, UK

Abstract

A series of high surface area nanocrystalline copper manganese oxide catalysts have been prepared by supercritical anti-solvent (SAS) precipitation using CO₂ and tested for the ambient temperature oxidation of CO. The catalysts were prepared by precipitation from an ethanol/metal acetate solution and the addition of small quantities of water was found to result in a mixed acetate precursor with surface areas >200 m² g⁻¹, considerably higher than those prepared by conventional precipitation methods. The surface area of the final calcined mixed oxide was found to be dependent upon the initial water concentration. XRD and FT-IR analysis indicated that the addition of water promoted the formation of carbonate species in the amorphous acetate precursor, with high resolution TEM and STEM showing the material to consist of spherical agglomerations of fibrous strings of ca. 30 nm length. This is in contrast to the material prepared in the absence of water, using the same SAS methodology, which typically yields quasi-spherical particles of 100 nm size.

Catalysis Science & Technology

Synthesis of high surface area CuMn₂O₄ by supercritical anti-solvent precipitation for the oxidation of CO at ambient temperature

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Synthesis of high surface area CuMn₂O₄ by supercritical anti-solvent precipitation for the oxidation of CO at ambient temperature

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