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Rapid Cycling Thermal Swing Adsorption Apparatus: Commissioning and Data Analyses for Water Adsorption of Zeolites 4A and 13X Over 2000 Cycles
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  • John H. Jacobs
    John H. Jacobs
    Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    More by John H. Jacobs
  • Connor E. Deering
    Connor E. Deering
    Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    More by Connor E. Deering
  • Kevin L. Lesage
    Kevin L. Lesage
    Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
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  • Mitchell J. Stashick
    Mitchell J. Stashick
    Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    More by Mitchell J. Stashick
  • Robert A. Marriott*
    Robert A. Marriott
    Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    *Email: [email protected]
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    Orcidhttp://orcid.org/0000-0002-1837-8605
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Industrial & Engineering Chemistry Research

Cite this: Ind. Eng. Chem. Res. 2021, 60, 19, 7487–7494
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https://doi.org/10.1021/acs.iecr.1c00469
Published May 4, 2021

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Abstract

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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.

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1. Introduction

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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 adsorption 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 structure (17,18) or due to contaminants such as coke (19) or condensed hydrocarbons. (16)
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 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 Masala et al. on an adsorbent was on the metal–organic framework (MOF) UTSA-16. (21) 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 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 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.

Figure 1

Figure 1. Image of the breakthrough apparatus for cycling adsorbents.

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2. Experimental Setup

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2.1. Materials

The synthesis and characterization of the zeolite 4A and 13X materials are reported in our previous 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 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 give a total flow of 2.40 SL min–1 and a N2/CO2 composition of 70:30. The dry gas feed was composed of N2/CO2 at a ratio of 70:30 at a flow rate of 2.40 ± 0.05 SL min–1.

Figure 2

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).

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Figure 3

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).

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To add water to N2(g), a Nafion water saturator was built (Figure 4). The saturator was composed of Nafion tubes, through which flowed the N2 gas, placed inside a stainless-steel tube that was filled with water. An eluent delivery bottle is used to fill the steel tube with purified double distilled water. To ensure there was no pressure gradient across the Nafion, the high-performance liquid chromatography (HPLC) eluent delivery bottle was pressurized by the gas feeding into the water saturator. At the end of the steel tube, a valve was installed to allow for the controlled drainage of water from the tube during the set up of the experiments. The Nafion water saturator was preferred over a bubble column due to the Nafion polymer preventing liquid water from entering the gas stream. Additionally, the Nafion saturator only achieved a water saturation of approximately 90%, thus preventing liquid water from condensing in the gas feed. The gas feed from the water saturator was at T = 21.3 °C and ptotal = 3.20 bar. A Texas Instruments LM35CA Precision Centigrade temperature sensor and a Specter Corporation (model 9000, 0–150 psig) pressure transducer were connected to the outlet of the water saturator to monitor the temperature and pressure of the gas. The temperature sensor and pressure transducer were connected via an Arduino Uno project board. The temperature and pressure data were recorded through National Instruments Laboratory Virtual Instrument Engineering Workbench (LabVIEW).

Figure 4

Figure 4. Schematic of the Nafion water saturator.

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An AirTAC 4V110-06 five-port, two-way valve was used to switch between the wet and dry gas feeds to the sample cells (Figure 3). To balance pressures upon switching gas feeds, an Equilibar LF Series Precision backpressure regulator was installed to restrict the bypassing fluid according to the inlet backpressure from the adsorbent cells. After the gas passes through the switching two-way valve, it was split into eight sample cells. Each cell was connected to a needle valve to balance the gas flows coming out of each cell to 300 Scm3 min–1. The flow rates for each cell were measured using an Agilent Technologies ADM 2000 universal flow meter.
All eight sample cells were inserted into an aluminum alloy block (aluminum alloy 7075). The aluminum alloy block also had two Watlow FIRERODs (J6A53-L2) and a water coolant channel embedded inside of it. The water used for the cooling of the apparatus was from a domestic water supply with an inlet temperature of T = 5 ± 2 °C. The fire rods and the water cooling were both controlled through LabVIEW. Four Honeywell HEL-700 100 Ω platinum resistance thermometers were inserted into the block after cells 1, 3, 5, and 7. These were then interfaced using a Pico Technology PT-104 USB data logger and the data was recorded via LabVIEW. Each sample cell was made from an aluminum fitting (Swagelok, aluminum alloy 6061-T6) that was drilled to fit a 0.5 μm pore diameter frit at the bottom (Figure 5). In the end of the tubing entering the cell, a 10 μm pore diameter frit was inserted. The outlet of each sample cell was connected to a Honeywell HIH-4010 relative humidity sensor. The data from these humidity sensors were converted to a digital signal using an Arduino Uno project board and recorded through LabVIEW.

Figure 5

Figure 5. Schematic of the adsorption cells detailing the insertion of the cells into the aluminum block.

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2.3. Decoupled Safety Circuit

To ensure the safe continuous operation of the apparatus presented in this work, a decoupled safety circuit was designed to trip using three unique scenarios. The safety circuit controlled a relay for the power supply of the breakthrough apparatus, whereas all safety measurement and safety circuit power were isolated from the instrument control. This allowed the system to operate without experimenter supervision for 24 h per day. The first trip scenario is the uncontrolled startup of the apparatus after a power outage. When a power outage occurs, the safety circuit disconnects the power to the apparatus, thus preventing an uncontrolled startup of the apparatus. The second trip scenario is the overheating of the aluminum blocks. One of the four thermometers that were embedded in the aluminum block is connected to the safety circuit. The circuit is then set up so that when a voltage threshold corresponding to approximately T = 400 °C is achieved on the aluminum block, the safety circuit will remove the power to the apparatus. The third trip scenario is the flooding of the area around the apparatus due to a leak in the water cooling of the aluminum block. Multiple Ideal Security SK616 water flood sensors are placed around the apparatus and interfaced to an Ideal Security SK662 command center. The safety circuit is connected to the command center so that when the water alarm of the flood sensors is triggered, the safety circuit will turn off the apparatus and close the valve for the water supply. Whenever any of the three components of the safety circuit is activated, a manual reset of the circuit is required before the operation of the apparatus can continue.

2.4. Rapid TSA Cycling Apparatus Procedure

Over a full adsorption cycle (adsorption, regeneration, and cooling) both the composition of the gas and the temperature of the cells were controlled. To effectively cycle the adsorbents, a LabVIEW program was implemented where three relays were used (cooling water, fire rod heating, and wet/dry gas) to control five different steps of the cycle. Each step for the cycle is marked in Figure 6. A full cycle on this instrument began by flowing a wet gas (N2/CO2/H2O) through the sample cells for a set amount of time (∼330 s). Once the set time was complete, the wet gas flow was switched to dry gas (N2/CO2) and the fire rods were turned on to heat the aluminum block at 80 °C per minute, marking the start of the regeneration process. The regeneration temperature was set to T = 280 °C under the dry CO2. At T = 280 °C, the fire rods were cycled on and off to maintain this temperature, i.e., proportional control. The cycling of the fire rods resulted in a fluctuation in the temperature of less than ± 3 °C. When the water content reading approached the baseline value of the dry gas (relative humidity ≈ 4%), the fire rods were switched off and cold water flowed through the coolant channels in the block until the block reached T = 33 °C. At T = 80 °C, the wet gas was switched on and the next adsorption cycle was initialized to save on cycling time. For the experiments reported in this work, each cell was loaded with 20–25 mg of an adsorbent. Each overall adsorption and regeneration cycle took less than 15 min.

Figure 6

Figure 6. Breakthrough (blue) curve for zeolite 4A with the corresponding temperature (red) profile for the full cycle conducted during an experiment. Dashed lines indicate what the conditions are during the experiment with regards to temperature control and gas composition.

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2.5. Thermogravimetric Analysis

External water adsorption analyses were conducted using a thermogravimetric analysis (TGA) instrument (TGA 550 Auto apparatus, TA Instruments). This was done before, after, and midway through the total test time. During activation in the TGA, dry He (T = 400 °C, p = 0.8905 bar, at 16 mL min–1) was passed over the adsorbent. The temperature increased at a rate of 25 °C min–1 and the sample was held at T = 400 °C for 120 min. During the adsorption process, 1.4 mol % H2O in He (T = 35 °C, p = 0.8905 bar, at 16 mL min–1) was passed over the adsorbent and these conditions were held for 240 min.
The TGA operated with a He flow through the balance and furnace. For the adsorption experiments, the He gas flowing over the adsorbent was first passed through a water saturator and then diluted by dry He before passing over the adsorbent. The flow rate of He passing through the water saturator was controlled using a Brooks SLA5800 mass flow controller (MFC) and the saturator temperature was controlled using a Polyscience chilling circulating bath.

3. Data Processing

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3.1. Breakthrough Plot Analysis

To analyze the raw data of the cycling apparatus, a program designed through Microsoft Visual Basic for Excel was used following the flow chart shown in Figure 7. Two methods were used for the analysis of the breakthrough plots to determine the uptake of water. The first method was to identify the breakthrough times and then track their changes through the cycles. To find the breakthrough time, the inflection point of the slope of the relative humidity (RH) versus time was used. Tracking of the R2 values of linear regression (least-squares) for a linear fit over 25 s of the RH was chosen as the method to identify the breakthrough time as it was observed that the minimum value of R2 coincided with the breakthrough time as shown in Figure 8a, i.e., the inflection point for the onset of breakthrough is the least linear portion of the data. The second method was to integrate relative humidity during regeneration to assess the water, which was removed from the material surface. This was done through summation between the time when dry gas was initiated and the time when wet gas was reintroduced, i.e., the complete regeneration portion of the cycle.

Figure 7

Figure 7. Logic of the analysis program for analyzing the breakthrough curves.

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Figure 8

Figure 8. (a) R2 for a linear fit (linearity) during the adsorption stage of the cycle (red) with the relative humidity (blue) over the same time period and (b) the relative humidity (blue) of the effluent during the regeneration portion of the experiment.

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To externally determine the change in water adsorption capacity (n, mmol g–1) from the TGA data, the difference in mass between the mass of the dried sample and the final mass of the sample was calculated.

3.2. Water Uptake from Breakthrough Plot Analyses

Relative adsorbent performance change was evaluated by the ratio of the breakthrough time (tb/tb,0) or relative regeneration humidity integration (I/I0) for each measured cycle. The averaged breakthrough time and integration for the first 30 cycles were assumed to be the initial breakthrough time (tb,0) and integration (I0). These relative values were then used to scale the water uptake capacity, as determined using the initial TGA measurement, i.e., the ratios for each cycle were multiplied by the n0 obtained from the TGA.

4. Results and Discussion

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The objective of this work was to cycle adsorbents over 2000 times. At ca. 15 min per cycle, it took 500 h (∼21 days) to collect 2000 cycles for eight samples. To minimize the time of adsorption and desorption, the size of each sample material was restricted to 20–25 mg. Similarly, the time for heating and cooling of the sample cells needed to be minimized while still being capable of cycling to high temperatures (T ≥ 250 °C). Aluminum was found to be a suitable material for the heating block due to its relatively low volumetric heat capacity (Cv = 2.376 × 106 J m–3 °C–1 at T = 20 °C) and high thermal conductivity (λ = 273 W m–1 K–1 at T = 20 °C). (26) For the sample cells, stainless steel and aluminum were investigated. Steel was found to heat slower due to its larger volumetric heat capacity (stainless steel 316, Cv = 3.732 × 106 J m–3 °C–1 at T = 20 °C) (23) compared to aluminum. For higher regeneration temperatures (T ≥ 250 °C), the temperature inside the steel cells was found to be up to 10 °C less than the set temperature as a result of stainless steel’s smaller thermal conductivity (λ = 13.9 W m–1 K–1 at T = 20 °C), (23) which resulted in a greater temperature gradient. Aluminum was found to be the better material for the sample cells due to its low heat capacity and durability over continuous cycling.
The results for the change in the uptake capacity of zeolites 4A and 13X are displayed in Figures 9 and 10, respectively (the average of two sample cells for each material). From these figures, it is shown that the results of the breakthrough curve analyses are in good agreement with the TGA results. The average residual differences for the different breakthrough plot analysis methods are summarized in Table 1. By comparing the residuals with a two-tailed P test (where the null hypothesis was that the difference between the two methods was zero), it was found that for zeolite 4A, there is no significant difference in the two breakthrough plot analysis methods, while for zeolite 13X, the difference was significant. Figure 10 clearly shows that the integration method was more reliable for the zeolite 13X samples. While one might be tempted to conclude that the integration method is more robust, we still feel that both methods should be used because the integration method may have issues with wet gas regeneration.

Figure 9

Figure 9. Breakthrough curves sampled through 2000 cycles of zeolite 4A (a). The uptake capacity of zeolite 4A over 2000 cycles as determined by breakthrough time (red, ○), regeneration region integration (blue, Δ), averaged breakthrough analysis (purple, ■), and TGA (black, ⧫) with a linear fit of the TGA data (black, −) (b). The residual error of the breakthrough time analysis (red, ○), regeneration region integration (blue, Δ), and averaged breakthrough analysis (purple, ■) compared to a linear fit of the TGA data (c). Only every 10th cycle is recorded and reported.

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Figure 10

Figure 10. Breakthrough curves sampled through 2000 cycles of zeolite 13X (a). The uptake capacity of zeolite 13X over 2000 cycles as determined by breakthrough time (red, ○), regeneration region integration (blue, Δ), averaged breakthrough analysis (purple, ■), and TGA (black, ⧫) with a linear fit of the TGA data (black, −) (b). The residual error of breakthrough time analysis (red, ○), regeneration region integration (blue, Δ), and averaged breakthrough analysis (purple, ■) compared to a linear fit of the TGA data (c). Only every 10th cycle is recorded and reported.

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Table 1. Comparison of the Residual Difference between Two Breakthrough Plot Analysis Methods and the Linear Fit of the TGA Water Uptake Determinations
average residual /%breakthrough time analysisintegration analysisP valueaveraged analysis
zeolite 4A3 ± 33 ± 41.0001 ± 1
zeolite 13X5 ± 82 ± 3<.00011 ± 1
The results of this work were compared to the results from Ruthven (17) and Belding et al.’s (20) studies (Figure 11). It is clear that the general trend for zeolite 13X within this work and the work of Belding et al. (20) appears consistent and the comparison of the results for zeolite 4A shows reasonable agreement to some of the work from Ruthven; (17) however, the variance within the Ruthven data is large. We note that a direct comparison is difficult, as the results of Ruthven, (17) Belding et al., (20) and this work were collected at different regeneration temperatures (T = 200, 260, and 280 °C, respectively) with different material sources, which could all be factors resulting in different results. Material purity and possible support material can also be important.

Figure 11

Figure 11. Comparison of the literature results with the work reported herein. Zeolite 4A from this work (black, ○) with a linear fit (black, −) and from the work of Ruthven (17) (red, ×) with a line (red, – −) to draw the eye. Zeolite 13X from this work (black, Δ) with a linear fit (black, −) and from the work of Belding et al. (20) (blue, ◊ and □) with a line (blue, – −) to draw the eye. Data from this study have been averaged over 50 cycles.

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Comparing the results of zeolite 4A with those of zeolite 13X, it is apparent that zeolite 4A is more stable in these experimental conditions, where our internally consistent regeneration conditions showed that zeolites 4A and 13X lost 7 ± 3 and 19 ± 7% of the adsorption capacity, respectively. From the literature, it is known that zeolite 4A is thermally stable up to T = 800 °C, (27−29) while zeolite 13X is less thermally stable showing degradation in the range of T = 200–350 °C. (30,31)
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

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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 adsorption 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 degradation of the materials.

Supporting Information

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The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.iecr.1c00469.

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Author Information

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  • Corresponding Author
  • Authors
    • John H. Jacobs - Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    • Connor E. Deering - Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    • Kevin L. Lesage - Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
    • Mitchell J. Stashick - Chemistry Department, University of Calgary, 2500 University Drive, N.W., Calgary, Alberta T2L 1N4, Canada
  • 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.

Acknowledgments

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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.

References

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    Zarinabad, S.; Samimi, A. Problems of Hydrate Formation in Oil and Gas Pipes Deals. J. Am. Sci. 2012, 88, 1007– 1010
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    Gandhidasan, P.; Al-Farayedhi, A. A.; Al-Mubarak, A. A. Dehydration of Natural Gas Using Solid Desiccants. Energy 2001, 26, 855– 868,  DOI: 10.1016/S0360-5442(01)00034-2
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    Dehydration of natural gas using solid desiccants
    Gandhidasan, P.; Al-Farayedhi, A. A.; Al-Mubarak, A. A.
    Energy (Oxford, United Kingdom) (2001), 26 (9), 855-868CODEN: ENEYDS; ISSN:0360-5442. (Elsevier Science Ltd.)
    Natural gas is an important source of primary energy that, under normal prodn. conditions, is satd. with water vapor. Water vapor increases natural gases' corrosivity, esp. when acid gases are present. Several methods can be used to dry natural gas and, in this paper, a solid desiccant dehydrator using silica gel is considered due to its ability to provide extremely low dew points. The design anal. of a two-tower, silica gel dehydration unit to dry one million std. m3 of natural gas per day is presented in this paper and the effects of various operating parameters on the design of the unit are discussed. The study also covers the anal. of energy requirements for the regeneration of the weak desiccant bed based on some simplified assumptions and it is found that the higher the regeneration temp., the smaller are the required quantities of regeneration gas.
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    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,  DOI: 10.1186/2228-5547-4-35
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    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,  DOI: 10.1039/C7EE02342A
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    Carbon capture and storage (CCS): the way forward
    Bui, Mai; Adjiman, Claire S.; Bardow, Andre; Anthony, Edward J.; Boston, Andy; Brown, Solomon; Fennell, Paul S.; Fuss, Sabine; Galindo, Amparo; Hackett, Leigh A.; Hallett, Jason P.; Herzog, Howard J.; Jackson, George; Kemper, Jasmin; Krevor, Samuel; Maitland, Geoffrey C.; Matuszewski, Michael; Metcalfe, Ian S.; Petit, Camille; Puxty, Graeme; Reimer, Jeffrey; Reiner, David M.; Rubin, Edward S.; Scott, Stuart A.; Shah, Nilay; Smit, Berend; Trusler, J. P. Martin; Webley, Paul; Wilcox, Jennifer; MacDowell, Niall
    Energy & Environmental Science (2018), 11 (5), 1062-1176CODEN: EESNBY; ISSN:1754-5706. (Royal Society of Chemistry)
    Carbon capture and storage (CCS) is broadly recognized as having the potential to play a key role in meeting climate change targets, delivering low carbon heat and power, decarbonising industry and, more recently, its ability to facilitate the net removal of CO2 from the atm. However, despite this broad consensus and its tech. maturity, CCS has not yet been deployed on a scale commensurate with the ambitions articulated a decade ago. Thus, in this paper we review the current state-of-the-art of CO2 capture, transport, utilization and storage from a multi-scale perspective, moving from the global to mol. scales. In light of the COP21 commitments to limit warming to less than 2 °C, we extend the remit of this study to include the key neg. emissions technologies (NETs) of bioenergy with CCS (BECCS), and direct air capture (DAC). Cognisant of the non-tech. barriers to deploying CCS, we reflect on recent experience from the UK's CCS commercialisation program and consider the com. and political barriers to the large-scale deployment of CCS. In all areas, we focus on identifying and clearly articulating the key research challenges that could usefully be addressed in the coming decade.
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    Adeniyi, K. I.; Bernard, F.; Deering, C. E.; Marriott, R. A. Water content of liquid H2S in equilibrium with the hydrate phase. Fluid Phase Equilib. 2021, 529, 112865  DOI: 10.1016/j.fluid.2020.112865
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    Water content of liquid H2S in equilibrium with the hydrate phase
    Adeniyi, Kayode I.; Bernard, Francis; Deering, Connor E.; Marriott, Robert A.
    Fluid Phase Equilibria (2021), 529 (), 112865CODEN: FPEQDT; ISSN:0378-3812. (Elsevier B.V.)
    Acid gas injection contg. H2S is one strategy for managing atm. sulfur emissions where sulfur recovery may not be feasible or economical in some locations. Apart from its toxicity and corrosivity in wet environments, H2S forms a high temp. hydrate in the presence of water, which can cause issues such as plugging of transport pipelines or injection wellheads. Before transportation to injection, liq. water is removed from an injectate within the interstage suction scrubbers before each compression cycle and/or by further dehydration. Water content data are important in order to det. and define the dehydration requirements of acid gas injectates. Prior to this work, there were no water content data for H2S at hydrate forming conditions because of the difficulties in measuring low concn. of water above hydrates and high H2S toxicity. In this study, we report the water content of pure H2S in the hydrate forming regions from p = 4.178 to 20.572 MPa and T = 247.65 to 298.28 K using tunable diode laser spectroscopy. The measured data show a relative water content difference of ca. 2.5% from the model reported in this work using the Sloan et al. (1976), and van der Waal & Platteeuw (1959) equations for the hydrate phase, and the fluid phase model of Bernard et al. (2012).
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    Baker, R. W.; Lokhandwala, K. Natural Gas Processing with Membranes: An Overview. Ind. Eng. Chem. Res. 2008, 47, 2109– 2121,  DOI: 10.1021/ie071083w
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    Natural Gas Processing with Membranes: An Overview
    Baker, Richard W.; Lokhandwala, Kaaeid
    Industrial & Engineering Chemistry Research (2008), 47 (7), 2109-2121CODEN: IECRED; ISSN:0888-5885. (American Chemical Society)
    A review. Every year, the world uses close to 100 trillion scf (std. cubic feet) of natural gas. All of this gas requires treatment before it enters the pipeline, making natural gas processing by far the largest market for industrial gas sepn. processes and equipment. Of this huge market, membranes have less than a 5% share, but this is changing; membrane-based removal of natural gas contaminants is growing faster than any other segment of the membrane gas sepn. business. This paper gives an overview of the membrane technol. in current use for natural gas treatment and outlines the future prospects.
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    Campbell, J. M.; Maddox, R. N. Gas Conditioning and Processing: Gas Treating and Sulfur Recovery, 4th ed.; Campbell Petroleum Series: Norman, Okla, 1998.
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    Wynnyk, K. G.; Hojjati, B.; Pirzadeh, P.; Marriott, R. A. High-Pressure Sour Gas Adsorption on Zeolite 4A. Adsorption 2017, 23, 149– 162,  DOI: 10.1007/s10450-016-9841-6
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    High-pressure sour gas adsorption on zeolite 4A
    Wynnyk, Kyle G.; Hojjati, Behnaz; Pirzadeh, Payman; Marriott, Robert A.
    Adsorption (2017), 23 (1), 149-162CODEN: ADSOFO; ISSN:0929-5607. (Springer)
    In an effort to measure self-consistent adsorption isotherms for sour gas species on zeolite 4A, two high-pressure manometric adsorption instruments have been built for measurement up to p = 225 bar. A comparison of CO2 adsorption up to p = 200 bar on Fitrasorb F400 activated carbon shows the reliability of these instruments. For the purpose of this work, high purity zeolite 4A was synthesized and characterized by SEM/EDX, XRD, FTIR, and DLS. High-pressure adsorption isotherms (abs. and excess) for CO2, COS, CH4 and H2S adsorption on zeolite 4A have been reported for T = 0, 25, and 50 °C along with corresponding parameters for the modified To´th isotherm. The adsorption of COS on zeolite 4A showed some unexpected results, where (i) lower temp. isotherms were dominated by size effects, (ii) the adsorption capacity was half that of CO2 or H2S, and (iii) computational calcns. for HOMO bond orientation indicate that COS should be excluded from zeolite 4A, despite the exptl. results.
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    Wynnyk, K. G.; Hojjati, B.; Marriott, R. A. High-Pressure Sour Gas and Water Adsorption on Zeolite 13X. Ind. Eng. Chem. Res. 2018, 57, 15357– 15365,  DOI: 10.1021/acs.iecr.8b03317
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    High-Pressure Sour Gas and Water Adsorption on Zeolite 13X
    Wynnyk, Kyle G.; Hojjati, Behnaz; Marriott, Robert A.
    Industrial & Engineering Chemistry Research (2018), 57 (45), 15357-15365CODEN: IECRED; ISSN:0888-5885. (American Chemical Society)
    The design and optimization of natural gas conditioning with adsorbents requires self-consistent data up to pressures relevant to gathering and transportation pipelines. Adsorption isotherms for methane, carbon dioxide, carbonyl sulfide, and hydrogen sulfide have been measured by a custom-built high-pressure manometric adsorption instrument. These isotherms are measured up to 100 bar on zeolite 13X (significantly above the inflection of isotherm). Furthermore, water adsorption isotherms were measured by an inhouse modified continuous-flow thermogravimetric adsorption system. For this work, the zeolite 13X was synthesized and characterized by SEM/EDX, XRD, DLS, and FT-RAMAN. Adsorption isotherms (abs. and excess) were detd. for the full range of the adsorptives studied. The manometric system was operated from T = 0 to 50 °C and the gravimetric system from T = 25 to 150 °C. The exptl. data are provided in the Supporting Information; a modified-T´oth equation was reported, and adsorption enthalpies were calcd. As expected, zeolite 13X shows much stronger adsorption for water at all pressures, followed by the acid gases (H2S and CO2), COS, and then CH4. We note that CH4 adsorption continues to increase with increasing pressure and approaches that of CO2 and H2S near p = 100 bar due to the higher compressibility of adsorbed CH4.
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    Wynnyk, K. G.; Hojjati, B.; Marriott, R. A. Sour Gas and Water Adsorption on Common High-Pressure Desiccant Materials: Zeolite 3A, Zeolite 4A, and Silica Gel. J. Chem. Eng. Data 2019, 64, 3156– 3163,  DOI: 10.1021/acs.jced.9b00233
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    Sour Gas and Water Adsorption on Common High-Pressure Desiccant Materials: Zeolite 3A, Zeolite 4A, and Silica Gel
    Wynnyk, Kyle G.; Hojjati, Behnaz; Marriott, Robert A.
    Journal of Chemical & Engineering Data (2019), 64 (7), 3156-3163CODEN: JCEAAX; ISSN:0021-9568. (American Chemical Society)
    When raw sour gas is gathered for transportation over long distances, adsorptive dehydration is often employed to avoid condensable water prior to purifn. at a gas processing plant, i.e., adsorptive dehydration is used to avoid excessive corrosion or hydrate plugging within transportation/gathering lines. To optimize and design adsorptive conditioning facilities, simulation requires self-consistent exptl. adsorption measurements at pressures relevant to gathering and transportation. To this end, manometric adsorption measurements on methane, carbon dioxide, carbonyl sulfide, and hydrogen sulfide on silica gel were measured at high pressures. This data adds to our previous work with sour gas adsorption on zeolites 4A and 13X. Also, in this study, gravimetric measurements for water adsorption are reported for silica gel, zeolite 3A, and zeolite 4A. Abs. and excess adsorption isotherms were detd. for the adsorptives studied with operating temps. ranging from T = 0 to 50 °C and T = 25 to 150 °C for the manometric and gravimetric measurements, resp. Across all of the desiccant materials studied, H2O has the largest adsorption affinity, followed by the acid gases (H2S and CO2), COS, and finally CH4. In terms of H2O adsorption, zeolites 3A and 4A show similar affinity (low-pressure Henry's law slope), whereas zeolite 4A shows a slightly larger capacity. Both zeolites 3A and 4A exceed silica gel in terms of capacity and affinity.
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    Optimal design and operation of molecular sieve gas dehydration units - Part 1
    Herold, R. H. M.; Mokhatab, S.
    Hydrocarbon Processing (2017), 96 (Spec. Suppl.), 25-30CODEN: HPYRAF ISSN:. (Gulf Publishing Co.)
    A review. Discussing the design and operation of mol. sieve units used for natural gas dehydration. The application of expert know-how and practical recommendations that can provide an effective way to maximize mol. sieve life-time and performance is presented. It also focuses on the design principles and practices of mol. sieve units.
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    Herold, R. H.; Mokhatab, S. Optimal design and operation of molecular sieves for gas dehydration-Part 2. Hydrocarbon Process. 2017, 96, 33– 36
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    Li, C.; Jia, W.; Wu, X. Experimental Failure-Mechanism Analysis of 4A Zeolites Used for Natural-Gas Drying. Chem. Technol. Fuels Oils 2015, 51, 245– 251,  DOI: 10.1007/s10553-015-0598-5
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    Experimental Failure-Mechanism Analysis of 4A Zeolites Used for Natural-Gas Drying
    Li, Changjun; Jia, Wenlong; Wu, Xia
    Chemistry and Technology of Fuels and Oils (2015), 51 (3), 245-251CODEN: CTFOAK; ISSN:0009-3092. (Springer)
    Scanning electron microscopic, nitrogen absorption-desorption, and thermogravimetric expts. were conducted on one fresh 4A zeolite and three regenerated 4A zeolite samples taken from the top, middle, and bottom of a natural-gas dehydration bed. The results showed that parts of the regenerated zeolite are blocked due to collapse of the zeolite structure. As a result, the sp. surface area, av. pore vol., and av. pore diam. of regenerated zeolite taken from the middle of the dehydration bed are less by about 59.15, 68.36, and 32.12%, resp., than those of fresh zeolite. Because water mols. cannot enter the internal pores due to blockage caused by collapse of the zeolite structure, the gas-dehydration performance of the regenerated zeolites is reduced. Thermogravimetric anal. of zeolites that adsorbed water showed that the water-adsorption performance of the regenerated zeolites is 35.53% less and the hydrocarbon-adsorption performance of these zeolites is 18.95% greater than those of fresh zeolite.
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    Santiago, R. G.; dos Santos, B. F.; Lima, I. G.; Moura, K. O.; Melo, D. C.; Grava, W. M.; Bastos-Neto, M.; de Lucena, S. M. P.; de Azevedo, D. C. S. Investigation of premature aging of zeolites used in the drying of gas streams. Chem. Eng. Commun. 2019, 206, 1367– 1374,  DOI: 10.1080/00986445.2018.1533468
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    Belding, W. A.; Delmas, M. P. F.; Holeman, W. D. Desiccant Aging and Its Effects on Desiccant Cooling System Performance. Appl. Therm. Eng. 1996, 16, 447– 459,  DOI: 10.1016/1359-4311(95)00022-4
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    Desiccant aging and its effects on desiccant cooling system performance
    Belding, William A.; Delmas, Marc P. F.; Holeman, William D.
    Applied Thermal Engineering (1996), 16 (5), 447-459CODEN: ATENFT; ISSN:1359-4311. (Elsevier)
    Desiccants used for the purpose of space conditioning or enthalpy transfer can be subjected to hundreds of thousands of adsorption/regeneration cycles over their useful life. Studying the loss of a desiccant's equil. water adsorption capacity after exposure to thermal cycling is a common method for quantifying desiccant aging. Since isotherm shape and desiccant capacity can be related to overall cooling-system performance, system cooling capacity and coeffs. of performance over time can be predicted. Adsorption isotherms for several different desiccants have been detd. after subjecting the materials to varying nos. of thermal cycles in a specially designed test unit capable of adsorption desorption cycling every 10 min. Aging curves for a new Type 1M desiccant developed specifically for desiccant cooling applications by LaRoche Industries Inc. are compared to other commonly used desiccants.
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    Masala, A.; Vitillo, J. G.; Mondino, G.; Grande, C. A.; Blom, R.; Manzoli, M.; Marshall, M.; Bordiga, S. CO 2 Capture in Dry and Wet Conditions in UTSA-16 Metal–Organic Framework. ACS Appl. Mater. Interfaces 2017, 9, 455– 463,  DOI: 10.1021/acsami.6b13216
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    CO2 Capture in Dry and Wet Conditions in UTSA-16 Metal-Organic Framework
    Masala, Alessio; Vitillo, Jenny G.; Mondino, Giorgia; Grande, Carlos A.; Blom, Richard; Manzoli, Maela; Marshall, Marc; Bordiga, Silvia
    ACS Applied Materials & Interfaces (2017), 9 (1), 455-463CODEN: AAMICK; ISSN:1944-8244. (American Chemical Society)
    Water is the strongest competitor to CO2 for adsorption on microporous materials, affecting their performances as CO2 scrubbers in processes such as post-combustion C capture. The metal-org. framework, UTSA-16, is a promising material for its capacity to efficiently capture CO2 in large quantities, thanks to the presence of open metal sites (OMS). This work showed UTSA-16 can able fully desorb water at room temp. This property is unique from all other materials with OMS reported to date. UTSA-16 retains 70% of its CO2 sepn. capacity following water admittance in a test flow created to simulate actual post-combustion C capture process conditions. This important aspect not yet obsd. for any other amine-free material is assocd. with high material stability, as tested in 160 cycles., and a small temp. swing necessary for regeneration, places UTSA-16 in the restrict no. of systems with a real technol. future for CO2 sepn. UTSA-16 has a small temp. swing necessary for regeneration, placing it in a restricted no. of systems with a technol. future for CO2 sepn.
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    De Marco, L. M.; Trierweiler, J. O.; Farenzena, M. Determination of Remaining Useful Life in Cyclic Processes. Ind. Eng. Chem. Res. 2019, 58, 22048– 22063,  DOI: 10.1021/acs.iecr.9b03182
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    Determination of Remaining Useful Life in Cyclic Processes
    De Marco, Leonardo M.; Trierweiler, Jorge Otavio; Farenzena, Marcelo
    Industrial & Engineering Chemistry Research (2019), 58 (48), 22048-22063CODEN: IECRED; ISSN:0888-5885. (American Chemical Society)
    The anal. of Remaining Useful Life (RUL) of systems and equipments enables the prevention of failures, so that effective maintenance can be performed in time to correct failures that are close to happening. The degrdn. signal of a variable can be used as a basis for estg. the RUL of a given system since this signal is modeled math. correctly. The RUL of cyclic processes is analyzed with the detn. of the No. of Remaining Cycles (NRC) to maximize prodn., guaranteeing operational safety. Two approaches are considered: Bayesian Methodol. and Time Series. The Bayesian methodol. is based on Bayesian Inference to update the stochastic parameter, providing better representativeness in the estn. of the NRC. The deterministic parameters and the hyperparameters in the prior distribution of the stochastic parameter are estd. through the max. likelihood estn. (MLE) method, while the stochastic parameter in the degrdn. model of a system can be updated every time a new degrdn. data is obtained. However, the Time Series is based on Training sets to be able to fit a model that is similar to the set used for validation. In the estn. of NRC, it is considered stationary model (Simple Exponential Smoothing), nonstationary (Double Exponential Smoothing) and a model that considers the component of seasonality (Triple Exponential Smoothing). A Case Study of a Temp. Swing Adsorption (TSA) unit for natural gas dehydration will be used to evaluate these 2 approaches in predicting NRC in cyclic processes. In this Case Study, the authors propose a novel cycle-packaging methodol. that creates a new dimension, allowing the application of NRC forecasting methodologies, which is the main contribution of this article. Probably the Bayesian Methodol. is the most indicated in the NRC estn., while the Time Series are adequate to identify the cyclic pattern of the process.
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    Gebraeel, N. Z.; Lawley, M. A.; Li, R.; Ryan, J. K. Residual-Life Distributions from Component Degradation Signals: A Bayesian Approach. IIE Transactions 2005, 37, 543– 557,  DOI: 10.1080/07408170590929018
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    Si, X.-S.; Wang, W.; Chen, M.-Y.; Hu, C.-H.; Zhou, D.-H. A Degradation Path-Dependent Approach for Remaining Useful Life Estimation with an Exact and Closed-Form Solution. Eur. J. Oper. Res. 2013, 226, 53– 66,  DOI: 10.1016/j.ejor.2012.10.030
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    Tang, S.; Yu, C.; Wang, X.; Guo, X.; Si, X. Remaining Useful Life Prediction of Lithium-Ion Batteries Based on the Wiener Process with Measurement Error. Energies 2014, 7, 520– 547,  DOI: 10.3390/en7020520
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    Van Der Aa, E. Finite Element Modelling of Temperature Profiles, Distortionsand Residual Stresses Due to TIG Welding. Master Thesis, TU Delft, 2002.
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    Majchrzak-Kucęba, I. A Simple Thermogravimetric Method for the Evaluation of the Degree of Fly Ash Conversion into Zeolite Material. J. Porous Mater. 2013, 20, 407– 415,  DOI: 10.1007/s10934-012-9610-1
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    A simple thermogravimetric method for the evaluation of the degree of fly ash conversion into zeolite material
    Majchrzak-Kuceba, Izabela
    Journal of Porous Materials (2013), 20 (2), 407-415CODEN: JPMAFX; ISSN:1380-2224. (Springer)
    The thermogravimetry was used for the evaluation of degree of conversion of fly ash into zeolite material alongside the CEC and XRD methods being currently proposed for this purpose. This work proposes the calcn. of the thermogravimetric fly ash-to-zeolite conversion factor, CFTGA, based on the comparison of the mass loss of the com. zeolite (std.) occurred during dehydration with that of the fly ash-derived zeolite. This mass loss is characteristic of a specific zeolite type, and the corresponding zeolite water content in the sample of zeolites indicates their degree of crystallinity and zeolite phase content. The use of the TGA method for the indirect detn. of the fly ash-to-zeolite conversion factor would be preferable owing to its speed compared to other methods proposed for this purpose, as well as the capability to use a consistent procedure. Because of its short CFTGA detn. procedure, the thermogravimetric method can be used for the control and detn. of the quality of fly ash-derived zeolite in an industrial plant.
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    Musyoka, N. M.; Petrik, L. F.; Hums, E.; Kuhnt, A.; Schwieger, W. Thermal Stability Studies of Zeolites A and X Synthesized from South African Coal Fly Ash. Res. Chem. Intermed. 2015, 41, 575– 582,  DOI: 10.1007/s11164-013-1211-3
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    Thermal stability studies of zeolites A and X synthesized from South African coal fly ash
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    The thermal stability of zeolites A and X synthesized from coal fly ash was studied by evaluation of TGA-DTA curves obtained on increasing the temp. and by in-situ temp.-programmed XRD anal. It was found that zeolites A and X were both stable up to approx. 800 °C and retained their characteristic diffraction peaks up to 440 °C, meaning the crystal structure was still stable. Of particular interest was that zeolite X, which has a unique hierarchical morphol., was thermally stable and was, hence, suitable for applications requiring elevated temps., for example catalysis and pollution control.
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    Iqbal, A.; Sattar, H.; Haider, R.; Munir, S. Synthesis and Characterization of Pure Phase Zeolite 4A from Coal Fly Ash. J. Cleaner Prod. 2019, 219, 258– 267,  DOI: 10.1016/j.jclepro.2019.02.066
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    Synthesis and characterization of pure phase zeolite 4A from coal fly ash
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    Journal of Cleaner Production (2019), 219 (), 258-267CODEN: JCROE8; ISSN:0959-6526. (Elsevier Ltd.)
    This study was aimed at the synthesis of pure phase zeolite 4A from coal fly ash sourced from Nishat power plant in the Punjab province of Pakistan. Anal. of fly ash (FA) demonstrated that it can be used to produce low silicate type zeolites specifically zeolite 4A due to its Si/Al molar ratio of ∼2. The current investigation emphasized on the addn. of induction time (before and after crystn.) to the fly ash ext. of Si-Al-Na species that was extd. from fly ash. The induction time helped in catalyzing primary and secondary gel formation during the synthesis leading to controlled formation of single phase with high crystallinity and small crystallite size. The physiochem. investigations of synthetic zeolite 4A by using various anal. techniques made the proposed process justified on comparison with com. zeolite 4A. The X-Ray Diffraction (XRD) anal. for synthesize zeolite 4A confirmed only one crystallog. phase and small crystallite size with 82% crystallinity compared to ref. zeolite with 75% crystallinity. Fourier-Transform IR spectroscopy (FTIR) spectra revealed the structural aspects of synthesis and ref. zeolite by indicating the presence of identical structural units with same height and width of peaks. Morphol. anal. by Scanning Electron Microscope (SEM) showed a well-defined cubic shape of synthesis zeolitic crystals. Surface area analyses by Brunauer-Emmett-Teller (BET) showed that synthesized zeolite possessed 122 m2/g surface area that is 3 times higher than ref. zeolite of 36.3 m2/g. The synthesized zeolite was also found to have smaller particle size than ref. zeolite. Thermal stability comparison of both zeolites was studied by non-isothermal Thermo Gravimetric Anal.-DTA (TGA-DTA) thermograms from 25 to 800°C temp. and both the samples were found to be stable at 800°C.
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    Hydrothermal stability of the novel zeolite type LSX in comparison to the traditional 13X modification
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    Ion-exchanged LSX with Si/Al = 1.02 and 13X with Si/Al = 1.18 zeolite series (Li, Na, K, Rb, Ca, Sr, Ba cation exchanged) were hydrothermally treated between 423 and 513 K in liq. water under autogenous water vapor pressure. Beside x-ray powder diffraction, the molybdate method and water sorption uptake have been used to characterize the treated specimens. The zeolites show a similar hydrothermal behavior in spite of their different framework Si/Al ratios and depended only on the type of introduced cation. Significant destabilizing effects were obsd., esp. in the presence of K and Rb cations as well as the bivalent Sr and Ba cations. The LSX zeolites are hydrothermally more stable than the LTA zeolites having the same cations despite their similar chem. framework compn.
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    Fischer, F.; Lutz, W.; Buhl, J.-C.; Laevemann, E. Insights into the Hydrothermal Stability of Zeolite 13X. Microporous Mesoporous Mater. 2018, 262, 258– 268,  DOI: 10.1016/j.micromeso.2017.11.053
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    Insights into the hydrothermal stability of zeolite 13X
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    Zeolite 13X, a hydrophilic adsorbent, can be used for storing thermal energy. However, its crystallinity can degrade under hydrothermal stress in the aq. atm. of an adsorption storage device. This would result in a loss of energy storage capacity. There is still no known method for predicting the long-term hydrothermal stability of zeolites under relevant adsorption storage conditions. A soln. for this could be a kinetic model designed with exptl. data to predict hydrothermal degrdn. The objective of the present study was to examine the hydrothermal stability of zeolite 13X under relevant adsorption storage conditions and to analyze its degrdn. in respect to the influencing factors of H2O vapor pressure, temp. and period of treatment. The studied zeolite 13X powder and zeolite 13X beads have been treated at 200-350° and H2O vapor pressures up to 31 kPa for treatment periods of up to 312 h. The authors analyzed the changes in the zeolite structure, compn. and adsorption properties by x-ray diffraction, SEM, energy-dispersive X-ray spectroscopy, 27Al/29Si MASNMR spectroscopy, molybdate method and H2O sorption. The results show a degrdn. of the cryst. zeolite 13X phase into an amorphous phase under all hydrothermal conditions, although to different degrees. Under specific hydrothermal conditions a portion of the primary cryst. phase withstands further treatment. Based on chem. decompn. mechanisms, this phenomenon are discussed. The complex stability behavior of the zeolite 13X demonstrates that a prediction beyond exptl. data cannot be recommended.
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  5. John H. Jacobs, Connor E. Deering, Ruohong Sui, Amelia P. Cann, Kevin L. Lesage, Robert A. Marriott. The role of carbon dioxide and water in the degradation of zeolite 4A, zeolite 13X and silica gels. New Journal of Chemistry 2023, 47 (11) , 5249-5261. https://doi.org/10.1039/D3NJ00093A
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Cite this: Ind. Eng. Chem. Res. 2021, 60, 19, 7487–7494
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  • Abstract

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    Figure 1

    Figure 1. Image of the breakthrough apparatus for cycling adsorbents.

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    Figure 2

    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).

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    Figure 3

    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).

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    Figure 4

    Figure 4. Schematic of the Nafion water saturator.

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    Figure 5

    Figure 5. Schematic of the adsorption cells detailing the insertion of the cells into the aluminum block.

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    Figure 6

    Figure 6. Breakthrough (blue) curve for zeolite 4A with the corresponding temperature (red) profile for the full cycle conducted during an experiment. Dashed lines indicate what the conditions are during the experiment with regards to temperature control and gas composition.

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    Figure 7

    Figure 7. Logic of the analysis program for analyzing the breakthrough curves.

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    Figure 8

    Figure 8. (a) R2 for a linear fit (linearity) during the adsorption stage of the cycle (red) with the relative humidity (blue) over the same time period and (b) the relative humidity (blue) of the effluent during the regeneration portion of the experiment.

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    Figure 9

    Figure 9. Breakthrough curves sampled through 2000 cycles of zeolite 4A (a). The uptake capacity of zeolite 4A over 2000 cycles as determined by breakthrough time (red, ○), regeneration region integration (blue, Δ), averaged breakthrough analysis (purple, ■), and TGA (black, ⧫) with a linear fit of the TGA data (black, −) (b). The residual error of the breakthrough time analysis (red, ○), regeneration region integration (blue, Δ), and averaged breakthrough analysis (purple, ■) compared to a linear fit of the TGA data (c). Only every 10th cycle is recorded and reported.

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    Figure 10

    Figure 10. Breakthrough curves sampled through 2000 cycles of zeolite 13X (a). The uptake capacity of zeolite 13X over 2000 cycles as determined by breakthrough time (red, ○), regeneration region integration (blue, Δ), averaged breakthrough analysis (purple, ■), and TGA (black, ⧫) with a linear fit of the TGA data (black, −) (b). The residual error of breakthrough time analysis (red, ○), regeneration region integration (blue, Δ), and averaged breakthrough analysis (purple, ■) compared to a linear fit of the TGA data (c). Only every 10th cycle is recorded and reported.

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    Figure 11

    Figure 11. Comparison of the literature results with the work reported herein. Zeolite 4A from this work (black, ○) with a linear fit (black, −) and from the work of Ruthven (17) (red, ×) with a line (red, – −) to draw the eye. Zeolite 13X from this work (black, Δ) with a linear fit (black, −) and from the work of Belding et al. (20) (blue, ◊ and □) with a line (blue, – −) to draw the eye. Data from this study have been averaged over 50 cycles.

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      A review. Every year, the world uses close to 100 trillion scf (std. cubic feet) of natural gas. All of this gas requires treatment before it enters the pipeline, making natural gas processing by far the largest market for industrial gas sepn. processes and equipment. Of this huge market, membranes have less than a 5% share, but this is changing; membrane-based removal of natural gas contaminants is growing faster than any other segment of the membrane gas sepn. business. This paper gives an overview of the membrane technol. in current use for natural gas treatment and outlines the future prospects.
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      Wynnyk, Kyle G.; Hojjati, Behnaz; Marriott, Robert A.
      Industrial & Engineering Chemistry Research (2018), 57 (45), 15357-15365CODEN: IECRED; ISSN:0888-5885. (American Chemical Society)
      The design and optimization of natural gas conditioning with adsorbents requires self-consistent data up to pressures relevant to gathering and transportation pipelines. Adsorption isotherms for methane, carbon dioxide, carbonyl sulfide, and hydrogen sulfide have been measured by a custom-built high-pressure manometric adsorption instrument. These isotherms are measured up to 100 bar on zeolite 13X (significantly above the inflection of isotherm). Furthermore, water adsorption isotherms were measured by an inhouse modified continuous-flow thermogravimetric adsorption system. For this work, the zeolite 13X was synthesized and characterized by SEM/EDX, XRD, DLS, and FT-RAMAN. Adsorption isotherms (abs. and excess) were detd. for the full range of the adsorptives studied. The manometric system was operated from T = 0 to 50 °C and the gravimetric system from T = 25 to 150 °C. The exptl. data are provided in the Supporting Information; a modified-T´oth equation was reported, and adsorption enthalpies were calcd. As expected, zeolite 13X shows much stronger adsorption for water at all pressures, followed by the acid gases (H2S and CO2), COS, and then CH4. We note that CH4 adsorption continues to increase with increasing pressure and approaches that of CO2 and H2S near p = 100 bar due to the higher compressibility of adsorbed CH4.
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    13. 13
      Wynnyk, K. G.; Hojjati, B.; Marriott, R. A. Sour Gas and Water Adsorption on Common High-Pressure Desiccant Materials: Zeolite 3A, Zeolite 4A, and Silica Gel. J. Chem. Eng. Data 2019, 64, 3156– 3163,  DOI: 10.1021/acs.jced.9b00233
      13
      Sour Gas and Water Adsorption on Common High-Pressure Desiccant Materials: Zeolite 3A, Zeolite 4A, and Silica Gel
      Wynnyk, Kyle G.; Hojjati, Behnaz; Marriott, Robert A.
      Journal of Chemical & Engineering Data (2019), 64 (7), 3156-3163CODEN: JCEAAX; ISSN:0021-9568. (American Chemical Society)
      When raw sour gas is gathered for transportation over long distances, adsorptive dehydration is often employed to avoid condensable water prior to purifn. at a gas processing plant, i.e., adsorptive dehydration is used to avoid excessive corrosion or hydrate plugging within transportation/gathering lines. To optimize and design adsorptive conditioning facilities, simulation requires self-consistent exptl. adsorption measurements at pressures relevant to gathering and transportation. To this end, manometric adsorption measurements on methane, carbon dioxide, carbonyl sulfide, and hydrogen sulfide on silica gel were measured at high pressures. This data adds to our previous work with sour gas adsorption on zeolites 4A and 13X. Also, in this study, gravimetric measurements for water adsorption are reported for silica gel, zeolite 3A, and zeolite 4A. Abs. and excess adsorption isotherms were detd. for the adsorptives studied with operating temps. ranging from T = 0 to 50 °C and T = 25 to 150 °C for the manometric and gravimetric measurements, resp. Across all of the desiccant materials studied, H2O has the largest adsorption affinity, followed by the acid gases (H2S and CO2), COS, and finally CH4. In terms of H2O adsorption, zeolites 3A and 4A show similar affinity (low-pressure Henry's law slope), whereas zeolite 4A shows a slightly larger capacity. Both zeolites 3A and 4A exceed silica gel in terms of capacity and affinity.
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    14. 14
      Gas Processors Supplier’s Assoc. (GPSA). Engineering Data Book, Tulsa, OK,1987.
      There is no corresponding record for this reference.
    15. 15
      Herold, R. H.; Mokhatab, S. Optimal design and operation of molecular sieves for gas dehydration-Part 1. Hydrocarbon Process. 2017, 96, 25– 30
      15
      Optimal design and operation of molecular sieve gas dehydration units - Part 1
      Herold, R. H. M.; Mokhatab, S.
      Hydrocarbon Processing (2017), 96 (Spec. Suppl.), 25-30CODEN: HPYRAF ISSN:. (Gulf Publishing Co.)
      A review. Discussing the design and operation of mol. sieve units used for natural gas dehydration. The application of expert know-how and practical recommendations that can provide an effective way to maximize mol. sieve life-time and performance is presented. It also focuses on the design principles and practices of mol. sieve units.
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    16. 16
      Herold, R. H.; Mokhatab, S. Optimal design and operation of molecular sieves for gas dehydration-Part 2. Hydrocarbon Process. 2017, 96, 33– 36
      There is no corresponding record for this reference.
    17. 17
      Ruthven, D. M. Principles of Adsorption and Adsorption Processes; Wiley: New York,1984.
      There is no corresponding record for this reference.
    18. 18
      Li, C.; Jia, W.; Wu, X. Experimental Failure-Mechanism Analysis of 4A Zeolites Used for Natural-Gas Drying. Chem. Technol. Fuels Oils 2015, 51, 245– 251,  DOI: 10.1007/s10553-015-0598-5
      18
      Experimental Failure-Mechanism Analysis of 4A Zeolites Used for Natural-Gas Drying
      Li, Changjun; Jia, Wenlong; Wu, Xia
      Chemistry and Technology of Fuels and Oils (2015), 51 (3), 245-251CODEN: CTFOAK; ISSN:0009-3092. (Springer)
      Scanning electron microscopic, nitrogen absorption-desorption, and thermogravimetric expts. were conducted on one fresh 4A zeolite and three regenerated 4A zeolite samples taken from the top, middle, and bottom of a natural-gas dehydration bed. The results showed that parts of the regenerated zeolite are blocked due to collapse of the zeolite structure. As a result, the sp. surface area, av. pore vol., and av. pore diam. of regenerated zeolite taken from the middle of the dehydration bed are less by about 59.15, 68.36, and 32.12%, resp., than those of fresh zeolite. Because water mols. cannot enter the internal pores due to blockage caused by collapse of the zeolite structure, the gas-dehydration performance of the regenerated zeolites is reduced. Thermogravimetric anal. of zeolites that adsorbed water showed that the water-adsorption performance of the regenerated zeolites is 35.53% less and the hydrocarbon-adsorption performance of these zeolites is 18.95% greater than those of fresh zeolite.
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    19. 19
      Santiago, R. G.; dos Santos, B. F.; Lima, I. G.; Moura, K. O.; Melo, D. C.; Grava, W. M.; Bastos-Neto, M.; de Lucena, S. M. P.; de Azevedo, D. C. S. Investigation of premature aging of zeolites used in the drying of gas streams. Chem. Eng. Commun. 2019, 206, 1367– 1374,  DOI: 10.1080/00986445.2018.1533468
      There is no corresponding record for this reference.
    20. 20
      Belding, W. A.; Delmas, M. P. F.; Holeman, W. D. Desiccant Aging and Its Effects on Desiccant Cooling System Performance. Appl. Therm. Eng. 1996, 16, 447– 459,  DOI: 10.1016/1359-4311(95)00022-4
      20
      Desiccant aging and its effects on desiccant cooling system performance
      Belding, William A.; Delmas, Marc P. F.; Holeman, William D.
      Applied Thermal Engineering (1996), 16 (5), 447-459CODEN: ATENFT; ISSN:1359-4311. (Elsevier)
      Desiccants used for the purpose of space conditioning or enthalpy transfer can be subjected to hundreds of thousands of adsorption/regeneration cycles over their useful life. Studying the loss of a desiccant's equil. water adsorption capacity after exposure to thermal cycling is a common method for quantifying desiccant aging. Since isotherm shape and desiccant capacity can be related to overall cooling-system performance, system cooling capacity and coeffs. of performance over time can be predicted. Adsorption isotherms for several different desiccants have been detd. after subjecting the materials to varying nos. of thermal cycles in a specially designed test unit capable of adsorption desorption cycling every 10 min. Aging curves for a new Type 1M desiccant developed specifically for desiccant cooling applications by LaRoche Industries Inc. are compared to other commonly used desiccants.
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    21. 21
      Masala, A.; Vitillo, J. G.; Mondino, G.; Grande, C. A.; Blom, R.; Manzoli, M.; Marshall, M.; Bordiga, S. CO 2 Capture in Dry and Wet Conditions in UTSA-16 Metal–Organic Framework. ACS Appl. Mater. Interfaces 2017, 9, 455– 463,  DOI: 10.1021/acsami.6b13216
      21
      CO2 Capture in Dry and Wet Conditions in UTSA-16 Metal-Organic Framework
      Masala, Alessio; Vitillo, Jenny G.; Mondino, Giorgia; Grande, Carlos A.; Blom, Richard; Manzoli, Maela; Marshall, Marc; Bordiga, Silvia
      ACS Applied Materials & Interfaces (2017), 9 (1), 455-463CODEN: AAMICK; ISSN:1944-8244. (American Chemical Society)
      Water is the strongest competitor to CO2 for adsorption on microporous materials, affecting their performances as CO2 scrubbers in processes such as post-combustion C capture. The metal-org. framework, UTSA-16, is a promising material for its capacity to efficiently capture CO2 in large quantities, thanks to the presence of open metal sites (OMS). This work showed UTSA-16 can able fully desorb water at room temp. This property is unique from all other materials with OMS reported to date. UTSA-16 retains 70% of its CO2 sepn. capacity following water admittance in a test flow created to simulate actual post-combustion C capture process conditions. This important aspect not yet obsd. for any other amine-free material is assocd. with high material stability, as tested in 160 cycles., and a small temp. swing necessary for regeneration, places UTSA-16 in the restrict no. of systems with a real technol. future for CO2 sepn. UTSA-16 has a small temp. swing necessary for regeneration, placing it in a restricted no. of systems with a technol. future for CO2 sepn.
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    22. 22
      De Marco, L. M.; Trierweiler, J. O.; Farenzena, M. Determination of Remaining Useful Life in Cyclic Processes. Ind. Eng. Chem. Res. 2019, 58, 22048– 22063,  DOI: 10.1021/acs.iecr.9b03182
      22
      Determination of Remaining Useful Life in Cyclic Processes
      De Marco, Leonardo M.; Trierweiler, Jorge Otavio; Farenzena, Marcelo
      Industrial & Engineering Chemistry Research (2019), 58 (48), 22048-22063CODEN: IECRED; ISSN:0888-5885. (American Chemical Society)
      The anal. of Remaining Useful Life (RUL) of systems and equipments enables the prevention of failures, so that effective maintenance can be performed in time to correct failures that are close to happening. The degrdn. signal of a variable can be used as a basis for estg. the RUL of a given system since this signal is modeled math. correctly. The RUL of cyclic processes is analyzed with the detn. of the No. of Remaining Cycles (NRC) to maximize prodn., guaranteeing operational safety. Two approaches are considered: Bayesian Methodol. and Time Series. The Bayesian methodol. is based on Bayesian Inference to update the stochastic parameter, providing better representativeness in the estn. of the NRC. The deterministic parameters and the hyperparameters in the prior distribution of the stochastic parameter are estd. through the max. likelihood estn. (MLE) method, while the stochastic parameter in the degrdn. model of a system can be updated every time a new degrdn. data is obtained. However, the Time Series is based on Training sets to be able to fit a model that is similar to the set used for validation. In the estn. of NRC, it is considered stationary model (Simple Exponential Smoothing), nonstationary (Double Exponential Smoothing) and a model that considers the component of seasonality (Triple Exponential Smoothing). A Case Study of a Temp. Swing Adsorption (TSA) unit for natural gas dehydration will be used to evaluate these 2 approaches in predicting NRC in cyclic processes. In this Case Study, the authors propose a novel cycle-packaging methodol. that creates a new dimension, allowing the application of NRC forecasting methodologies, which is the main contribution of this article. Probably the Bayesian Methodol. is the most indicated in the NRC estn., while the Time Series are adequate to identify the cyclic pattern of the process.
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    23. 23
      Gebraeel, N. Z.; Lawley, M. A.; Li, R.; Ryan, J. K. Residual-Life Distributions from Component Degradation Signals: A Bayesian Approach. IIE Transactions 2005, 37, 543– 557,  DOI: 10.1080/07408170590929018
      There is no corresponding record for this reference.
    24. 24
      Si, X.-S.; Wang, W.; Chen, M.-Y.; Hu, C.-H.; Zhou, D.-H. A Degradation Path-Dependent Approach for Remaining Useful Life Estimation with an Exact and Closed-Form Solution. Eur. J. Oper. Res. 2013, 226, 53– 66,  DOI: 10.1016/j.ejor.2012.10.030
      There is no corresponding record for this reference.
    25. 25
      Tang, S.; Yu, C.; Wang, X.; Guo, X.; Si, X. Remaining Useful Life Prediction of Lithium-Ion Batteries Based on the Wiener Process with Measurement Error. Energies 2014, 7, 520– 547,  DOI: 10.3390/en7020520
      There is no corresponding record for this reference.
    26. 26
      Van Der Aa, E. Finite Element Modelling of Temperature Profiles, Distortionsand Residual Stresses Due to TIG Welding. Master Thesis, TU Delft, 2002.
      There is no corresponding record for this reference.
    27. 27
      Majchrzak-Kucęba, I. A Simple Thermogravimetric Method for the Evaluation of the Degree of Fly Ash Conversion into Zeolite Material. J. Porous Mater. 2013, 20, 407– 415,  DOI: 10.1007/s10934-012-9610-1
      27
      A simple thermogravimetric method for the evaluation of the degree of fly ash conversion into zeolite material
      Majchrzak-Kuceba, Izabela
      Journal of Porous Materials (2013), 20 (2), 407-415CODEN: JPMAFX; ISSN:1380-2224. (Springer)
      The thermogravimetry was used for the evaluation of degree of conversion of fly ash into zeolite material alongside the CEC and XRD methods being currently proposed for this purpose. This work proposes the calcn. of the thermogravimetric fly ash-to-zeolite conversion factor, CFTGA, based on the comparison of the mass loss of the com. zeolite (std.) occurred during dehydration with that of the fly ash-derived zeolite. This mass loss is characteristic of a specific zeolite type, and the corresponding zeolite water content in the sample of zeolites indicates their degree of crystallinity and zeolite phase content. The use of the TGA method for the indirect detn. of the fly ash-to-zeolite conversion factor would be preferable owing to its speed compared to other methods proposed for this purpose, as well as the capability to use a consistent procedure. Because of its short CFTGA detn. procedure, the thermogravimetric method can be used for the control and detn. of the quality of fly ash-derived zeolite in an industrial plant.
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    28. 28
      Musyoka, N. M.; Petrik, L. F.; Hums, E.; Kuhnt, A.; Schwieger, W. Thermal Stability Studies of Zeolites A and X Synthesized from South African Coal Fly Ash. Res. Chem. Intermed. 2015, 41, 575– 582,  DOI: 10.1007/s11164-013-1211-3
      28
      Thermal stability studies of zeolites A and X synthesized from South African coal fly ash
      Musyoka, Nicholas M.; Petrik, Leslie F.; Hums, Eric; Kuhnt, Andreas; Schwieger, Wilhelm
      Research on Chemical Intermediates (2015), 41 (2), 575-582CODEN: RCINEE; ISSN:0922-6168. (Springer)
      The thermal stability of zeolites A and X synthesized from coal fly ash was studied by evaluation of TGA-DTA curves obtained on increasing the temp. and by in-situ temp.-programmed XRD anal. It was found that zeolites A and X were both stable up to approx. 800 °C and retained their characteristic diffraction peaks up to 440 °C, meaning the crystal structure was still stable. Of particular interest was that zeolite X, which has a unique hierarchical morphol., was thermally stable and was, hence, suitable for applications requiring elevated temps., for example catalysis and pollution control.
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    29. 29
      Iqbal, A.; Sattar, H.; Haider, R.; Munir, S. Synthesis and Characterization of Pure Phase Zeolite 4A from Coal Fly Ash. J. Cleaner Prod. 2019, 219, 258– 267,  DOI: 10.1016/j.jclepro.2019.02.066
      29
      Synthesis and characterization of pure phase zeolite 4A from coal fly ash
      Iqbal, Asifa; Sattar, Hamed; Haider, Rizwan; Munir, Shahid
      Journal of Cleaner Production (2019), 219 (), 258-267CODEN: JCROE8; ISSN:0959-6526. (Elsevier Ltd.)
      This study was aimed at the synthesis of pure phase zeolite 4A from coal fly ash sourced from Nishat power plant in the Punjab province of Pakistan. Anal. of fly ash (FA) demonstrated that it can be used to produce low silicate type zeolites specifically zeolite 4A due to its Si/Al molar ratio of ∼2. The current investigation emphasized on the addn. of induction time (before and after crystn.) to the fly ash ext. of Si-Al-Na species that was extd. from fly ash. The induction time helped in catalyzing primary and secondary gel formation during the synthesis leading to controlled formation of single phase with high crystallinity and small crystallite size. The physiochem. investigations of synthetic zeolite 4A by using various anal. techniques made the proposed process justified on comparison with com. zeolite 4A. The X-Ray Diffraction (XRD) anal. for synthesize zeolite 4A confirmed only one crystallog. phase and small crystallite size with 82% crystallinity compared to ref. zeolite with 75% crystallinity. Fourier-Transform IR spectroscopy (FTIR) spectra revealed the structural aspects of synthesis and ref. zeolite by indicating the presence of identical structural units with same height and width of peaks. Morphol. anal. by Scanning Electron Microscope (SEM) showed a well-defined cubic shape of synthesis zeolitic crystals. Surface area analyses by Brunauer-Emmett-Teller (BET) showed that synthesized zeolite possessed 122 m2/g surface area that is 3 times higher than ref. zeolite of 36.3 m2/g. The synthesized zeolite was also found to have smaller particle size than ref. zeolite. Thermal stability comparison of both zeolites was studied by non-isothermal Thermo Gravimetric Anal.-DTA (TGA-DTA) thermograms from 25 to 800°C temp. and both the samples were found to be stable at 800°C.
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    30. 30
      Buhl, J.-Ch.; Gerstmann, M.; Lutz, W.; Ritzmann, A. Hydrothermal Stability of the Novel Zeolite Type LSX in Comparison to the Traditional 13X Modification. Z. Anorg. Allg. Chem. 2004, 630, 604– 608,  DOI: 10.1002/zaac.200300370
      30
      Hydrothermal stability of the novel zeolite type LSX in comparison to the traditional 13X modification
      Buhl, J.-Ch.; Gerstmann, M.; Lutz, W.; Ritzmann, A.
      Zeitschrift fuer Anorganische und Allgemeine Chemie (2004), 630 (4), 604-608CODEN: ZAACAB; ISSN:0044-2313. (Wiley-VCH Verlag GmbH & Co. KGaA)
      Ion-exchanged LSX with Si/Al = 1.02 and 13X with Si/Al = 1.18 zeolite series (Li, Na, K, Rb, Ca, Sr, Ba cation exchanged) were hydrothermally treated between 423 and 513 K in liq. water under autogenous water vapor pressure. Beside x-ray powder diffraction, the molybdate method and water sorption uptake have been used to characterize the treated specimens. The zeolites show a similar hydrothermal behavior in spite of their different framework Si/Al ratios and depended only on the type of introduced cation. Significant destabilizing effects were obsd., esp. in the presence of K and Rb cations as well as the bivalent Sr and Ba cations. The LSX zeolites are hydrothermally more stable than the LTA zeolites having the same cations despite their similar chem. framework compn.
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    31. 31
      Fischer, F.; Lutz, W.; Buhl, J.-C.; Laevemann, E. Insights into the Hydrothermal Stability of Zeolite 13X. Microporous Mesoporous Mater. 2018, 262, 258– 268,  DOI: 10.1016/j.micromeso.2017.11.053
      31
      Insights into the hydrothermal stability of zeolite 13X
      Fischer, Fabian; Lutz, Wolfgang; Buhl, Josef-Christian; Laevemann, Eberhard
      Microporous and Mesoporous Materials (2018), 262 (), 258-268CODEN: MIMMFJ; ISSN:1387-1811. (Elsevier B.V.)
      Zeolite 13X, a hydrophilic adsorbent, can be used for storing thermal energy. However, its crystallinity can degrade under hydrothermal stress in the aq. atm. of an adsorption storage device. This would result in a loss of energy storage capacity. There is still no known method for predicting the long-term hydrothermal stability of zeolites under relevant adsorption storage conditions. A soln. for this could be a kinetic model designed with exptl. data to predict hydrothermal degrdn. The objective of the present study was to examine the hydrothermal stability of zeolite 13X under relevant adsorption storage conditions and to analyze its degrdn. in respect to the influencing factors of H2O vapor pressure, temp. and period of treatment. The studied zeolite 13X powder and zeolite 13X beads have been treated at 200-350° and H2O vapor pressures up to 31 kPa for treatment periods of up to 312 h. The authors analyzed the changes in the zeolite structure, compn. and adsorption properties by x-ray diffraction, SEM, energy-dispersive X-ray spectroscopy, 27Al/29Si MASNMR spectroscopy, molybdate method and H2O sorption. The results show a degrdn. of the cryst. zeolite 13X phase into an amorphous phase under all hydrothermal conditions, although to different degrees. Under specific hydrothermal conditions a portion of the primary cryst. phase withstands further treatment. Based on chem. decompn. mechanisms, this phenomenon are discussed. The complex stability behavior of the zeolite 13X demonstrates that a prediction beyond exptl. data cannot be recommended.
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