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Boreskov Institute of Catalysis of the Siberian Branch of Russian ...

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OP-I-16KINETICS IN THE HYDROGENATION OF β-SITOSTEROLTO β-SITOSTANOL OVER DIFFERENT Pd CATALYSTSP. Mäki-Arvela, G. Martin, A. Tokarev, N. Kumar, J. Hemming, B. Holmbom,T. Salmi, D.Yu. MurzinProcess Chemistry Centre, Åbo Akademi University, FI-20500 Turku/Åbo, FinlandIntroductionNowadays, one <strong>of</strong> <strong>the</strong> most important problem for human health is high concentration <strong>of</strong>fats in food. Therefore, a lot <strong>of</strong> attention has been devoted to β-sitostanol, which was proved toinhibit cholesterol absorption [1], and is thus a constituent <strong>of</strong> some margarines available on <strong>the</strong>consumer market. The aim <strong>of</strong> <strong>the</strong> present work was to evaluate <strong>the</strong> catalytic activity <strong>of</strong> severalmaterials in <strong>the</strong> hydrogenation <strong>of</strong> β-sitosterol, which is a product from pulping industry, in orderto achieve a high selectivity towards β-sitostanol and to determine <strong>the</strong> reaction kinetics over <strong>the</strong>most promising catalyst. The main reaction scheme is presented in Fig 1.C 2H 5C 2H 5Fig. 1. Reaction scheme for β-sitosterol hydrogenation.ExperimentalThe kinetic experiments were performed in a shaking reactor using 1-propanol as asolvent. The volume <strong>of</strong> <strong>the</strong> liquid phase was 110 mL and <strong>the</strong> pressure was set to4 bar. The raw material according to results obtained from GC-MS analysis were:82 wt.% β-sitosterol, about 7 wt.% campesterol, 9 wt.% β-sitostanol and 1 wt.% campestanol.The β-sitosterol hydrogenation was carried out in <strong>the</strong> presence <strong>of</strong> 1-propanol, and severalsupported Pd catalysts. The samples were withdrawn periodically from <strong>the</strong> reactor whichoperated at 60°C to 80°C. After addition <strong>of</strong> an internal standard solution consisting <strong>of</strong>heneicosanoic acid and betulinol, <strong>the</strong> reaction mixture was evaporated under nitrogen andsilylated at 60°C for 45 min with BSTFA-TMCS-pyridine solution and analyzed by a GCequipped with an HP-1 column. Several catalyst characterization methods (COchemisorption,nitrogen adsorption, XRD) were applied. Fur<strong>the</strong>rmore, rapid UV analyseswere applied for <strong>the</strong> reaction mixtures, being prior calibrated using GC analyses.56

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