Catalysis of Organic..

Cao, White, Wang and Frye 291Experimental SectionCordierite monolith (400cpi) (Corning, Inc) was used as a substrate. The opening ofeach channel has 1x1 mm of dimension. The monolith was pre-machined to fit into astainless steel tubular reactor with 1.27cm of diameter and 52.8cm of length. Themonolith substrate was first treated with 10wt% HNO 3 for 1 hour at 80°C followedby washing with DI H 2 O. This served to both clean the monolith and rehydrate thesurfaces. The monolith was then dried at 50°C overnight. TiO 2 contained Tyzor LAmaterial (Dupont) was applied as catalyst support which was coated onto themonolith, The TiO 2 concentration in Tyzor was 2.2M. Tyzor coating was appliedsequentially with inter-drying steps and calcinations at 350°C. The total TiO 2 loadingis 5.2g. The coating thickness is 25μm. Ni(NO 3 ) 2 . 6H 2 O and HReO 4 were theprecursors of the active metals. Aqueous phase solution containing 8.6wt% Ni and1.22wt% Re was impregnated into the TiO 2 coating on the monolith. The catalystwas then calcined at 300°C for 3 hours. The final composition was 18% Ni/ 2.6%Re/TiO 2 .The monolith catalyst was snugly fit into a tubular reactor with a jacked heatexchanger. The catalyst was activated by flowing hydrogen across the bed atatmospheric pressure, and the bed was heated to 285°C and held for 8 hours. Thereactor was then cooled under hydrogen. The reactor was then raised to 1200 psigand 210°C. 25wt% sorbitol, 2.1wt% NaOH aqueous solution was pumped into thesystem with flowrates of 25-100 ml/hr. Hydrogen flow was regulated by a mass flowcontroller to keep the H 2 / Sorbitol molar ratio of 8.9 The reactor pressures wasmaintained at 1200 psig by a dome-loaded back pressure regulator.AcknowledgementsThis work was funded by Laboratory Directed Research and Development (LDRD)Program at Pacific Northwest National Laboratory. Pacific Northwest NationalLaboratory is operated by Battelle Memorial Institute for US Department of Energy.References1. T. A. Werpy, J. G. Frye, A. H. Zacher and D. J. Miller, US Pat. 6,841,085, toBattelle Memorial Institute and Michigan State University (2005).2. D. C. Elliott, U.S. Pat. Appl. 2002,169,344, Battelle Memorial Institute (2002).3. T. A. Werpy, J. G. Frye, A. H. Zacher and D. J. Miller, US Pat. 6,479,713, toBattelle Memorial Institute and Michigan State University (2002).4. S. P. Chopade, D. J. Miller, J. E. Jackson, T. A. Werpy, J. G. Frye, A. H.Zacher, US Pat. 6,291,725, to Michigan State University and Battelle MemorialInstitute (2000).