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Industrial & Engineering Chemistry Research ■ pubs.acs.org/IECR Article AUTHOR INFORMATION Corresponding Author Robert A. Marriott − Chemistry Department, University of Calgary, Calgary, Alberta T2L 1N4, Canada; orcid.org/ 0000-0002-1837-8605; Email: rob.marriott@ucalgary.ca Authors John H. Jacobs − Chemistry Department, University of Calgary, Calgary, Alberta T2L 1N4, Canada Connor E. Deering − Chemistry Department, University of Calgary, Calgary, Alberta T2L 1N4, Canada Kevin L. Lesage − Chemistry Department, University of Calgary, Calgary, Alberta T2L 1N4, Canada Mitchell J. Stashick − Chemistry Department, University of Calgary, Calgary, Alberta T2L 1N4, Canada Complete contact information is available at: https://pubs.acs.org/10.1021/acs.iecr.1c00469 Author Contributions J.H.J. drafted the initial manuscript, collected data, and performed the data analysis. C.E.D. contributed to the building and design of the instrument and collected data. K.L.L. contributed to the building and design of the instrument. M.J.S. contributed to the data analysis. R.A.M. conceived the presented idea, contributed to the design of the instrument, supervised the findings of this work, and is the corresponding author. All authors have discussed the results and contributed to the final manuscript. Notes The authors declare no competing financial interest. The data that supports the findings of this study are available within the article and its supporting information. ■ Finally, both Figures 9 and 10 show the successful test of this instrument and the utility for comparing long-term (high- cycle) performance between different desiccant materials. Something noteworthy from the analysis of zeolites 4A and 13X is that the change in uptake capacity as measured by the TGA was statistically insignificant for the first 600 cycles with the results falling within the 95% confidence interval of the initial uptake. After 2000 cycles, the uptake capacity of zeolites 4A and 13X decreased by 0.947 mmol g−1 (6.7%) and 2.58 mmol g−1 (19.1%) from the initial uptakes of 13.5 ± 0.4 and 13.6 ± 1 mmol g−1, respectively. In this case, a higher regeneration temperature or the addition of a binder may show a difference in material performance. Again, laboratory studies on the degradation in the adsorption uptake of adsorbents are important for industrial applications.20 In the literature, the most a MOF has been thermally cycled in the range of 160 cycles.21 When compared to adsorbents industrially in TSA processes such as zeolites 4A and 13X, if only 160 cycles are conducted then there would be insufficient data for the performance of these materials on an industrial timescale. 5. CONCLUSIONS This work reports an effective method for the continuous and rapid TSA cycling of adsorbent materials. We have introduced an instrument capable of continuously cycling eight adsorbents at a rate of 250 h per 1000 cycles. From the results of cycling zeolites 4A and 13X, it is clear that the instrument introduced in this publication is capable of cycling adsorbent materials for thousands of cycles, while the analysis of the breakthrough curves produces results consistent with the TGA results. The rapid cycling of this instrument gives results for the change in the uptake capacity of zeolites 4A and 13X over 2000 cycles. These results indicate that TSA cycling of <600 is insufficient for the adsorbents shown when no binder was added and when regeneration was at 280 °C with dry gas. If further insights into the longevity of different gas desiccants and different regeneration conditions are to be obtained, then continuous cycling on the scale of thousands of cycles must be conducted. While the results of these early experiments begin to elucidate the performance of zeolites 4A and 13X for multiple cycles, we note that this particular commissioning has included a single cycling method for consistent side-by-side testing, whereas the instrument is capable of many other cycling modes/methods. There are limitations in this initial commissioning study regarding the contact time of the materials to water vapor and heat, i.e., perhaps one material would outperform another given larger water loading. To address these issues, further studies into wet gas regeneration (keeping a wet gas feed throughout the adsorption and desorption cycle), various regeneration times, longer adsorp- tion times, wet gas composition, and regeneration temperature need to be conducted for future studies. Furthermore, investigations into how the rate of heating during the regeneration and different gas compositions during the cycling of materials would give better mechanistic insights into the d■egradation of the materials. ASSOCIATED CONTENT *sı Supporting Information The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.iecr.1c00469. Tabulated data discussed in this work (PDF) ACKNOWLEDGMENTS 7493 The funding for this research was provided through the Natural Science and Engineering Research Council of Canada (NSERC) and Alberta Sulphur Research Ltd. (ASRL) Industrial Research Chair in Applied Sulfur Chemistry. ■ (1) Kohl, A. L.; Nielsen, R. B. Gas Purification, 5th ed.; Gulf Pub: Huoston, Texas, 1997. (2) Ward, Z. T.; Marriott, R. A.; Sum, A. K.; Sloan, E. D.; Koh, C. A. Equilibrium Data of Gas Hydrates Containing Methane, Propane, and Hydrogen Sulfide. J. Chem. Eng. Data 2015, 60, 424−428. (3) Zarinabad, S.; Samimi, A. Problems of Hydrate Formation in Oil and Gas Pipes Deals. J. Am. Sci. 2012, 88, 1007−1010. (4) Gandhidasan, P.; Al-Farayedhi, A. A.; Al-Mubarak, A. A. Dehydration of Natural Gas Using Solid Desiccants. Energy 2001, 26, 855−868. (5) Popoola, L.; Grema, A.; Latinwo, G.; Gutti, B.; Balogun, A. Corrosion Problems during Oil and Gas Production and Its Mitigation. Int. J. Ind. Chem. 2013, 4, 35. (6) Bui, M.; Adjiman, C. S.; Bardow, A.; Anthony, E. J.; Boston, A.; Brown, S.; Fennell, P. S.; Fuss, S.; Galindo, A.; Hackett, L. A.; Hallett, J. P.; Herzog, H. J.; Jackson, G.; Kemper, J.; Krevor, S.; Maitland, G. C.; Matuszewski, M.; Metcalfe, I. S.; Petit, C.; Puxty, G.; Reimer, J.; Reiner, D. M.; Rubin, E. S.; Scott, S. A.; Shah, N.; Smit, B.; Trusler, J. P. M.; Webley, P.; Wilcox, J.; Mac Dowell, N. Carbon Capture and Storage (CCS): The Way Forward. Energy Environ. Sci. 2018, 11, 1062−1176. (7) Wu, Y.; Carroll, J. J.; Li, Q. Gas Injection for Disposal and Enhanced Recovery; Scrivener Publishing: Salem, Massachusetts, 2014. https://doi.org/10.1021/acs.iecr.1c00469 REFERENCES Ind. Eng. Chem. Res. 2021, 60, 7487−7494PDF Image | Rapid Cycling Thermal Swing Adsorption Apparatus
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