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Abstract
In situ characterization of catalysts provides important information on the catalyst and the understanding of its activity and selectivity for a specific reaction. TPX techniques for catalyst characterization reveal the role of the support on the stabilization and dispersion of the active sites. However, these can be altered at high temperature since sintering of active species can occur as well as possible carbon deposition through the Bosch reaction, which hinders the active species and deactivates the catalyst. In situ characterization of the spent catalyst, however, may expose the causes for catalyst deactivation. For example, a simple TPO analysis on the spent catalyst may produce CO and CO2 via a reaction with O2 at high temperature and this is a strong indication that deactivation may be due to the deposition of carbon during the Sabatier reaction. Other TPX techniques such as TPR and pulse chemisorption are also valuable techniques when they are applied in situ to the fresh catalyst and then to the catalyst upon deactivation.
Highlights
The in-situ Catalyst Characterization System (ICCS) [1,2] from Micromeritics and the Cirrus MKS [3] mass spectrometer prove to be a very powerful system when combined with the Micromeritics Flow Reactor (FR) [1]
A necessary technique often used is temperature programmed reactions (TPX) [4]. This technique reveals important properties of the catalyst, such as the effects of the support material in stabilizing the active species to minimize sintering, a quantitative analysis to determine the quantity of the oxide used as active species, the active particle size that can be estimated by the mechanism of reduction shown by the TPR profile, etc
One peak is at about 150 ◦C which could be related to some consumption of O2 as shown by the mass spectrum (Figure 13), and another peak is at about 450 ◦C which was not identified by the mass spectrum and could be related to the oxidation of some remaining salt traces that were used for the preparation of the catalyst
Summary
The in-situ Catalyst Characterization System (ICCS) [1,2] from Micromeritics and the Cirrus MKS [3] mass spectrometer prove to be a very powerful system when combined with the Micromeritics Flow Reactor (FR) [1]. For better interpretation of the results especially on the TPO profile of the spent catalyst, a fresh sample of the catalyst was reduced through TPR up to 650 ◦C (Figure 11).
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