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pubs.acs.org/IECR Rapid Cycling Thermal Swing Adsorption Apparatus: Commissioning and Data Analyses for Water Adsorption of Zeolites 4A and 13X Over 2000 Cycles John H. Jacobs, Connor E. Deering, Kevin L. Lesage, Mitchell J. Stashick, and Robert A. Marriott* Cite This: Ind. Eng. Chem. Res. 2021, 60, 7487−7494 ACCESS Metrics & More Read Online Article Recommendations *sı Supporting Information ABSTRACT: Evaluation of adsorbent integrity over thousands of cycles is necessary to establish the service time and sustainability of adsorbents employed in industrial dehydration. Herein, an adsorption apparatus for rapidly cycling multiple adsorbents through a thermal swing adsorption process is introduced with results for 2000 cycles. This apparatus has eight sample cells arranged in parallel, which are embedded in an aluminum block for rapid heating and cooling. At the outlet of each cell, the water content and temperatures are measured using capacitance relative humidity sensors, which incorporate resistance thermometers. The analysis of the breakthrough curves generated for each adsorbent gives inference into the change in water uptake capacity over continuous cycling. To handle the large sets of data generated by this instrument, an automated analysis program was implemented. To demonstrate the functionality of the instrument, zeolites 4A and 13X were cycled in a thermal swing process over 2000 cycles and the change in the uptake capacity was monitored by the analysis of the breakthrough plots for each cycle. Furthermore, the results of the breakthrough analyses were verified with the thermogravimetric analysis of the adsorbents. From these experiments, zeolites 4A and 13X were observed to lose 7 ± 3 and 19 ± 7% of the adsorption capacity, respectively. 1. INTRODUCTION Dehydration is critical within natural gas processing to prevent hydrate formation and corrosion of pipelines and processing facilities.1−5 The same can be true for carbon capture and storage, as well as acid gas injection applications.6−8 Often, dehydration occurs with either glycol absorption or solid adsorption technology.9−13 The most common solid adsorp- tion process used in industry for the dehydration of natural gas is thermal swing adsorption (TSA).14 During TSA, it is common for two or three beds to be used, where the first bed adsorbs water from the raw natural gas and the second bed is either being thermally regenerated and cooled or is regenerated while the third bed is being cooled. These conditioning systems are designed to operate uninterruptedly for a minimum of 3−5 years.14−16 The estimation of the lifetime for adsorbents during a TSA process is typically based on the historical loss of capacity and has been attributed to the blocking of the pores by either a collapse of the crystal structure17,18 or due to16contaminants such as coke19 or condensed hydrocarbons. If it is assumed that a full cycle (adsorption, regeneration, and cooling) takes 24 h,14 then 5 years of operation would require that an adsorbent is cycled more than 1825 times. Thus, laboratory evaluation of desiccant materials should ideally include thousands of cycles for validation before implementation. However, when one searches the literature, it is difficult to find laboratory adsorbent tests, which have been cycled more than 30 times. To our knowledge, with the © 2021 The Authors. Published by American Chemical Society TSA technique, most cycles reported on an adsorbent were published by Belding et al., who studied desiccants for cooling systems with approximately 50 000 cycles on zeolite 13X, silica gel, and activated alumina.20 Most cycles reported on zeolite 4A in the literature were presented in the work of Ruthven where 725 TSA cycles were conducted on zeolites 4A and 13X. In the last 24 years, the most cycles reported in the work of 7487 https://doi.org/10.1021/acs.iecr.1c00469 Ind. Eng. Chem. Res. 2021, 60, 7487−7494 Masala et al. on an adsorbent was on the metal−organic 21 framework (MOF) UTSA-16. This MOF was studied for its carbon capture capabilities, where the uptake for CO2 was monitored over 160 TSA cycles. Both the work of Ruthven and Belding et al. use ex situ measurements to quantify the change in adsorption capacity, where the number of data points obtained is limited. Ruthven reported up to four points over 725 cycles and Belding et al. reported six data points over 50 000 cycles. With regards to the application of this data, De Marco et al.22 recently used the Wiener process to estimate the remaining useful life of an absorbent material. The Weiner process is a degradation model,23,24 which has typically been used to describe batteries after continuous charging and discharging.25 By calibrating with 160 TSA cycles, De Marco et Article February 1, 2021 April 20, 2021 April 22, 2021 Received: Revised: Accepted: Published: May 4, 2021 Downloaded via 50.93.222.59 on June 28, 2022 at 12:35:14 (UTC). See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.PDF Image | Rapid Cycling Thermal Swing Adsorption Apparatus
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