Hydrogenation of aqueous glucose solution was performed in batch and continuous reactors using supported nickel and ruthenium catalysts. Preparation methods were precipitation, impregnation, solgel and template syntheses, and SiO 2 , TiO 2 , Al 2 O 3 and carbon were used as support materials. A procedure for the one-step synthesis of templated metal on support catalysts was established. The influence of support material and preparation methods was studied and the results were compared with those of an industrial nickel catalyst. In a detailed study taking more than 1100 h time on stream we investigated the deactivation of the industrial catalyst and a supported ruthenium catalyst, and evaluated the deactivation mechanisms. As yet unpublished side products of the glucose hydrogenation were identified and a scheme of the reaction network was set up.
Metal stearate‐stabilized Cu nanoparticles, synthesized by an efficient one‐step process, were applied in the continuous liquid‐phase synthesis of methanol. After optimizing the reduction procedure, twofold higher rates of methanol formation were found for Cu–Zn colloids, compared to the conventional ternary Cu/ZnO/Al2O3 catalyst applied as fine powder in the liquid phase. Structural changes were investigated as a function of time on stream; after reduction in H2, spherical, well‐separated 5–10 nm Cu particles stabilized by a Zn stearate shell were found. Under catalytic high‐pressure conditions Zn stearate was hydrolyzed forming ZnO. High‐resolution transmission electron microscopy revealed the presence of triangular ZnO prisms with truncated edges. Applying optimized synthesis conditions these triangularly shaped ZnO particles were found to be mostly attached to the spherical Cu particles. The catalytic results and the structural and spectroscopic characterization suggest that these ZnO particles act as a reservoir, releasing ZnOx species, which diffuse onto the Cu particles and promote the catalytic activity.
A highly efficient one-step process to generate Cu-Zn colloids was developed, in which the colloidal particles were synthesized from Cu and Zn stearates by reduction with H(2) in a continuously operated stirred tank reactor. The resulting spherical, well separated particles have a size of 5-10 nm, consisting of a crystalline Cu(0) core (fcc) stabilized by a Zn stearate shell without long-range order. In situ attenuated total reflection FTIR spectroscopy was used to monitor the shift of the C-O stretching vibration of adsorbed CO as a function of temperature and pressure. The absence of the CO rotation-vibration bands of dissolved CO allowed us to obtain FTIR spectra at a CO pressure of 1.0 MPa at 473 K resulting in three shifted CO bands at 2030-2025, 1979-1978, and 1920 cm(-1). These bands indicate the presence of reduced coadsorbed Zn species on the metallic Cu surface. Cyclic CO adsorption experiments demonstrated the dynamics of the interaction between the Cu core and the Zn stearate shell.
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