ICCU-methanation using a vertical stainless steel tubular reactor

“CO2 adsorption and hydrogenation cycles were carried out in a vertical stainless steel tubular reactor inside a 3-zone tube furnace. The reactor was filled with 1.0 g of pelletized (0.3–0.5 mm) fresh formulation, where the operating temperature was continuously measured through a thermocouple placed in the centre of the catalytic bed. Prior to the catalytic test, fresh samples were in-situ reduced with a stream composed of 10% H2/Ar leading to the conformation of the final DFM due to the controlled reduction of perovskite-based formulation. With that aim, the temperature was progressively increased from room temperature to 650, 550 or 800 °C (2 h) for bulk and ceria- and alumina-supported samples, respectively. Note that the reduction temperature for each support was already optimized in a previous study [39].

Once the DFM was obtained, CO2 adsorption and hydrogenation experiments were carried out, increasing the reaction temperature progressively from 280 to 520 °C, in steps of 40 °C. During the adsorption period (60 s), the feed composition was 10% CO2/Ar. Then, this step was followed by a purge with Ar (120 s) to remove weakly adsorbed CO2 and prevent mixing of streams. Finally, CO2 was replaced by a 10% of H2 during the hydrogenation (methanation) period (120 s). Before starting the following CO2 adsorption period, the catalyst and the system were again purged with Ar for 60 s. The catalytic tests were carried out with a total flow rate of 1200 mL min−1. This flow corresponds to space velocities of around 45,000 and 140,000 h−1 for ceria- and alumina-supported samples, respectively. CO2, CH4, CO and H2O were continuously quantified by a MKS MultiGas 2030 FT-IR analyser.”

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