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Industrial & Engineering Chemistry Research al.22 demonstrated that this modeling could also be applied to adsorption systems. An industrially relevant number of cycles (>2000) could be used to validate these types of degradation models. Based on the publications listed above, one study showed the cycling of adsorbents that matches the current number of desired cycles. This lack of literature for the cycling of adsorbents for an industrially relevant number of cycles highlights the need for more data. The impetus for this study was to build an apparatus to cycle adsorbents on a scale that is relevant to the industrial lifetime of an adsorbent used for dehydrating natural gas (based on the number of cycles versus time on stream or time at temperature). Obviously, to achieve these many cycles, the laboratory test cycle time needs to be short. Herein, we report a new breakthrough apparatus that can meet the above goal (Figure 1). This instrument Figure 1. Image of the breakthrough apparatus for cycling adsorbents. measures water vapor breakthrough curves for eight adsorbent samples simultaneously. The analysis of these breakthrough profiles gives insights into the change in water uptake capacity over continuous cycling. The measurement of the adsorbents periodically with thermogravimetric analysis (TGA) was used to validate the analysis of the breakthrough curves. In this work, we have reported the details of the apparatus and data analysis, along with the results of the change in water uptake over 2000 cycles for zeolites 4A and 13X. The average time for each adsorption cycle reported in this work was 800 s. Due to this short collection time, data equivalent to years of industrial cycling was collected within weeks on a laboratory scale. 2. EXPERIMENTAL SETUP 2.1. Materials. The synthesis and characterization of the zeolite 4A and 13X materials are reported in our previous pubs.acs.org/IECR Article publications.11,12 An in-house EMD Millipore system was used to purify double distilled water to a resistivity of 18 MΩ·cm. Liquid carbon dioxide (CO2, 99.95%) was purchased from Messer and used as received (vapor withdrawal). Liquid nitrogen (N2, 99.998%) and helium (He, 99.9990%, Alphagaz 1) were purchased from Air Liquide and used as received. 2.2. Rapid Thermal Swing Cycling Apparatus. The measurements for these experiments were conducted using an in-house built TSA apparatus with schematics shown in Figures 2 and 3. For these experiments, off-gas from liquid N2 Figure 2. Schematic of the gas manifold for the wet gas feed and the dry gas feed. PRT indicates a 100 Ω platinum resistance thermometer (four wires). 7488 Figure 3. Schematic of the adsorption cells detailing the insertion of the cells into the aluminum block. PRT indicates a 100 Ω platinum resistance thermometer (two wires). and liquid CO2 dewars were used as the source of the gas flowing into the instrument. Liquid sources of N2 and CO2 were chosen to maximize the time between replacement of the gas supply. At the flow rates reported herein, approximately 240 L of liquid N2 and CO2 were used every 7 days (24 h operation for 1 week). The gaseous flow rates of N2 and CO2 were controlled using a VICI Condyne (Model 202) flow controller (flow control valve, FCV). The flow rates from the FCV were measured using a Honeywell American Meter (DTM-200A) dry gas meter. Both the N2 and CO2 gas flows were split to flow to the water saturator and dry gas channels (Figure 2). For these experiments, the flow rate to the Nafion water saturator was adjusted to 1.68 ± 0.05 SL min−1 (T = 20 °C, p = 101 kPa) of N2. After leaving the saturator, 0.72 ± 0.05 SL min−1 of CO2 was added to the water-saturated gas flow to https://doi.org/10.1021/acs.iecr.1c00469 Ind. Eng. Chem. Res. 2021, 60, 7487−7494PDF Image | Rapid Cycling Thermal Swing Adsorption Apparatus
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