High-throughput reactor system with individual temperature control for the investigation of monolith catalysts

Dellamorte, Joseph C.; Vijay, Rohit; Snively, Christopher M.; Barteau, Mark A.; Lauterbach, Jochen
July 2007
Review of Scientific Instruments;Jul2007, Vol. 78 Issue 7, p072211
Academic Journal
A high-throughput parallel reactor system has been designed and constructed to improve the reliability of results from large diameter catalysts such as monoliths. The system, which is expandable, consists of eight quartz reactors, 23.5 mm in diameter. The eight reactors were designed with separate K type thermocouples and radiant heaters, allowing for the independent measurement and control of each reactor temperature. This design gives steady state temperature distributions over the eight reactors within 0.5 °C of a common setpoint from 50 to 700 °C. Analysis of the effluent from these reactors is performed using rapid-scan Fourier transform infrared (FTIR) spectroscopic imaging. The integration of this technique to the reactor system allows a chemically specific, truly parallel analysis of the reactor effluents with a time resolution of approximately 8 s. The capabilities of this system were demonstrated via investigation of catalyst preparation conditions on the direct epoxidation of ethylene, i.e., on the ethylene conversion and the ethylene oxide selectivity. The ethylene, ethylene oxide, and carbon dioxide concentrations were calibrated based on spectra from FTIR imaging using univariate and multivariate chemometric techniques. The results from this analysis showed that the calcination conditions significantly affect the ethylene conversion, with a threefold increase in the conversion when the catalyst was calcined for 3 h versus 12 h at 400 °C.


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