原位谱学表征技术进展.pptVIP

原位谱学表征技术进展 Outline Why in-situ spectroscopy Progress of in-situ spectroscopy IR UV-Vis EPR NMR Outlook: Future of in-situ spectroscopy Why in-situ spectroscopy Real catalysts Practical condition: continuous flow high temperature high pressure Many catalytic reaction don’t be understood well In situ IR reactor cell H.G.Karge, W.Nieβen, Catal.Today 8 (1991) 451 Pressure: vacuum or 1 bar Temperature: up to 923K Progress of in-situ IR spectroscopy G.Mirth et al. Appl.Spectrosc. 48 (1994) 194 Pressure: up to 5 bar Temperature: 300 to 870K In situ IR reactor cell Pressure: 10-5 torr to 15 bar Temperature: RT to 723K Commercial in situ IR cell Provided by ISRI,USA Commercial in situ IR reactor cell Example of application of in-situ FTIR Preparation of solid catalysts Ir(CO)2(acac) Ir4(CO)12 NaY CO Intermediate:Ir2(CO)8 No intermediate F.Li etal. J.Phys.Chem.B, 108(2004)11259 NaY300 NaY25 Example of application of in-situ FTIR 1479cm-1: benzene vibration 1492cm-1,1386cm-1: cumene 1600cm-1:coke M.Breuninger et al.Chem.Ing.Tech.73 (2001) 869 + H-EU-1 448K Heterogeneously catalyzed reaction process Example of application of in-situ FTIR Time resolved In-situ ATR-FTIR (Attenuated Total reflection ) In-situ ATR-FTIR and DEMS setup M.Heinen et al.Electrochimica Acta 52(2007)5634 Example of application of in-situ FTIR M.Heinen et al.Electrochimica Acta 52(2007)5634 Scheme of an UV-Vis/NIR setup 200-500nm is of special intrest for an in-situ UV-Vis spectroscopic detection of hydrocarbons with conjugated double bands and unsaturated carbenium ions Progress of in-situ UV-Vis spectroscopy J.Mehlsheimer et al.Phys.Chem.Chem.Phys.5(2003) 4366 Example of application of in situ UV-Vis spectroscopy UV-Vis spectra recorded during the conversion of isobutane and 1-butene(9:1) on zeolite LaH-Y at reaction temperatures of 523-773K 315nm:monoenyl carbenium ions 370nm:dienyl carbenium ions I.Kiricsi et al. Chem.Rev.99 (1999) 2085 A. Brückner et al. Stud.Surf