Design and applications of an in-house developed high pressure/high temperature transmission FTIR reaction cell are presented. By coupling with a mass spectrometer online analysis of product formation is possible enabling operando FTIR spectroscopic studies. The cell, made of stainless-steel, has been designed to be operable at pressures up to 30 bar and temperatures between 22°C and 300°C. Long-time tests, with no signs of damage of the cell and windows have been conducted at 15 bar and 250°C. The performance of the cell was tested by studying three types of CO 2 hydrogenation reactions (CO 2 Fischer-Tropsch synthesis, CO 2 methanation, CO 2 conversion to dimethyl ether) on selected catalyst systems by varying temperature and pressure. The operando spectroscopic measurements revealed reliable data which reflect the same trends as found by respective catalytic tests.
Shortly after starting our project on CO 2 hydrogenation, we realized that our existing IR cells, designed only for normal pressure, did not deliver relevant results in reactions that require elevated pressure. The crucial point was to ensure comparability of catalytic data measured both in spectroscopic investigations and in catalytic tests. This needs an analytical cell that operates like a traditional catalytic reactor, but also fulfils the requirements for infrared spectroscopy. As a suitable transmission FTIR reactor was not available from commercial suppliers, we decided to develop it on our own. This was done in close cooperation between our experts in FTIR spectroscopy Jana Weiß, Christoph Kubis and Ursula Bentrup, our chemical engineer Christine Rautenberg and our precision mechanics Thomas Rall, who have inspired each other with clever ideas and craftsmanship. The result is the joint success of all, that has produced a cell with many advantages: It can be run at higher pressure and temperature under changing gas atmospheres. The cell is small, compact, easy to handle, fits into different spectrometers and can be used for a wide variety of solid-gas reactions. Due to the low dead volume the obtained spectroscopic results are directly related to the catalytic performance which is a must for reliable mechanistic studies.Invited for this month's cover is the group of Angelika Brücker at the Leibniz Institute for Catalysis in Rostock (Germany). The cover picture shows a self-developed stainless-steel reaction cell for operando transmission FTIR studies of heterogeneous catalytic gas-phase reactions at pressures up to 30 bar and temperatures up to 300°C, which is connected to a mass spectrometer for online product analysis. The performance of the cell has been tested in three types of CO 2 hydrogenation reactions (CO 2 Fischer-Tropsch synthesis, CO 2 methanation, CO 2 conversion to dimethyl ether) on various solid catalysts implemented as self-supporting wafers. Catalytic data obtained with this cell showed the same trends as those measured in a fixed-bed plug-flow reactor, thus confirming their reliability. Read the full text of their Full Paper at 10.1002/cmtd.202100024.
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