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Solvent Effects on the Photothermal Regeneration of CO2 in Monoethanolamine Nanofluids Du T. Nguyen, Josh Stolaroff, and Aaron P. Esser-Kahn ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.5b08151 • Publication Date (Web): 02 Nov 2015 Downloaded from http://pubs.acs.org on November 5, 2015

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ACS Applied Materials & Interfaces

Solvent Effects on the Photothermal Regeneration of CO2 in Monoethanolamine Nanofluids Du Nguyen†§, Joshuah Stolaroff§, and Aaron Esser-Kahn‡* †

Department of Physics and Astronomy, University of California, Irvine, Irvine California, 92697, USA

‡

Department of Chemistry, University of California, Irvine, Irvine California, 92697, USA

§

Lawrence Livermore National Laboratory, Livermore, California 94551, USA

Keywords: carbon black, carbon capture, nanoparticles, photothermal, solar energy Abstract: A potential approach to reduce energy costs associated with carbon capture is to use external and renewable energy sources. The photothermal release of CO2 from monoethanolamine mediated by nanoparticles is a unique solution to this problem. When combined with light absorbing nanoparticles, vapor bubbles form inside the capture solution and release the CO2 without heating up the bulk solvent. The mechanism by which CO2 is released remained unclear and understanding this process can help develop methods for improvement that will increase the efficiency of photothermal CO2 release. Here we report the use of different co-solvents to improve or reduce the photothermal regeneration of CO2 captured by monoethanolamine. We found that properties that reduce the residence time of the gas bubbles (viscosity, boiling point, and convection direction) can enhance the regeneration efficiencies. The reduction of bubble residence times minimizes the reabsorption of CO2 back into the capture solvent where bulk temperatures remain lower than the localized area near the nanoparticles. These properties shed light on the mechanism of release and indicated methods for improving the efficiency of the process. We used this knowledge to develop an improved phothermal CO2 regeneration system in a continuously flowing setup. Using techniques to reduce residence time in the continuously flowing setup, such as alternative co-solvents and smaller fluid volumes, resulted in regeneration efficiency enhancements of over 200%.

Introduction The reduction of global CO2 emissions remains a significant challenge.1 Carbon capture and storage (CCS) from fossil-fueled power plants and industrial processes is considered an important part of climate preservation methods2, however current technologies are expensive and energy-intensive, reducing the output of a coal-fired power plant by a quarter to a third.3 The most established carbon capture technologies are based on aqueous amine solvents, such as monoethanolamine (MEA).4,5 The solvent captures CO2 from flue gas in a packed tower reactor (the “absorber”) and is subsequently heated with steam to release pure CO2 in a separate packed tower (the “stripper”), regenerating the solvent. The majority of energy used by the system is in the form of steam needed to regenerate the CO2-loaded solvent.6 The steam is generally taken from the power plant boiler and thus diverted from electricity production. We recently reported an alternative approach to regenerating carbon capture solvents.7–9 Instead of steam, the solvent is regenerated photothermally with the aid of carbon black nanoparticles. Photothermal heating of nanoparticles is a burgeoning area with applications in several areas, including cancer therapy10,11, chemical reactions12– 15 , distillation and heating16–21, sanitization22, and polymerization23. For mediating chemical reactions, very few studies have examined increasing the efficiency of the reaction. In our proposed chemical reaction of CO2 stripping, the stripper is replaced with a photothermal reactor that exposes the solvent to light. Light provides the vast majority of energy used by the system. Using solar light, this approach could potentially reduce the energy penalty on the power plant. However, the critical element in determining the viability of this process is the efficiency of converting light to chemical reactivity.

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As we showed previously, the nanoscale photothermal phenomenon allows higher CO2 regeneration efficiencies than conventional parabolic troughs as the thermal energy was directly used to break the bond between CO2 from MEA without heating the bulk solution.24,25 In this paper, we further explore the photothermal phenomenon and show that the efficiency of CO2 release can be enhanced by physical effects of the surrounding solvent. Higher efficiencies of CO2 release would lead to proportionally smaller footprints of a photothermal stripper and lower capital costs. The carbon black nanoparticles are a form of amorphous carbon that are less regularly crystalline than graphite and strongly absorb light over a broad wavelength spectrum. In the hypothesized mechanism of CO2 release, CBN absorb incident light energy and convert it locally into thermal energy. The heated area surrounding the particles reaches higher temperatures than the bulk solution, and drives the release of CO2 from MEA. A bubble of CO2 forms around the nanoparticle, causing it to rise to the top of the solution and release CO2.26,27 This enhancement derives from both the solvent boiling point as well as speed with which the nascent gas bubble can reach the surface. In following sections, we investigate the effects of solvent viscosity, boiling point, and flow direction on regeneration efficiency. Using these principles, we construct a system that continuously regenerates a CBN-MEA nanofluid with improved regeneration efficiencies. Experimental Materials: Methanol, ethanol, methoxy-ethanol, ethylene glycol, N,N-dimethylformamide dimethylacetal (DMFDMA), dimethylformamide (DMF), Dimethylacetamide (DMA), N-Methyl-2-pyrrolidone, 2-pyrrolidone, monoethanolamine, and gelatin from porcine skin were obtained from Sigma Aldrich. Carbon black nanoparticles (N115) were generously provided by the Cabot Corporation. Efficiency Measurement: The regeneration efficiencies were measured using the CO2 release rate and actinic light (Supporting Information). A 100 mL custom flask with a vacuum insulated jacket and flat windows was used to contain the NCB/capture fluid mixture, with water used as the solvent for the base case. The nanofluid mixtures consisted of the chosen co-solvent with 30% MEA and 0.2 wt% carbon black. 50 g of the mixture was placed into the flask and loaded gravimetrically with CO2 by bubbling the solution with pure CO2 to 10 wt% (0.5 mol CO2/mol MEA) loading for a total of 5 g of CO2. The photography spotlight was used as the light source and was turned on with a set irradiance of 1560 W/m2, initiating the photothermal release of CO2 into the gas detection system. To remove evaporating liquids from the detectors, the gas stream was filtered through condensing and drying tubes. The gas stream was then fed into a mass flow meter and CO2 meter to simultaneously measure the gas flow rate and CO2 concentration. Measurements were repeated in triplicate by re-saturating the nanofluid mixtures. Viscosity Modification: To examine the effects of viscosity on the photothermal regeneration of CO2, we used gelatin as a non-reactive viscosity modifier to MEA with H2O as the co-solvent. Gelatin was mixed into the MEA solution with concentrations varying between 0 and 2 wt%. Viscosities were measured using an Ostwald viscometer, resulting in measured viscosities between 4.62 to 20.62 cP (Figure 4). Vertical Stirring: A vertical magnetic stirrer was fabricated by modifying a conventional horizontal magnetic stirrer. Two holes were drilled on either side of the stirrer and metal rods were affixed to the holes to create a rotational point. Two acrylic rectangles were cut (12 cm x 0.5 cm) and mounted onto a 3D printed cap fit for the top of the vacuum flask. A single hole was drilled into the bottom of the acrylic sheets and the magnetic stirrer was mounted onto the holes. The device limited the motion of the stirrer so that a stirring plate would only stir it vertically. Continuous Photothermal CO2 Regeneration: A continuous lab-scale solar stripper was also used to evaluate the photothermal regeneration of CO2 with co-solvents alternative to water. We sought to better mimic actual process conditions by using the continuous flow of CO2 saturated NCB nanofluids through the desorption flask, rather than maintaining a static amount within the flask. The nanofluid pumping introduces fresh, saturated NCB nanofluid into the system. The introduction of fresh nanofluid also provides a cooling effect to the bulk liquid. As a result, the measured CO2 release rate reaches a steady state rather than evolve over time. The system operates similarly to the static desorption system with added modifications (Supporting Information). A peristaltic pump was used to flow the nanofluid from an absorption container into the regeneration container containing initially 150g of the nanofluid. The nanofluid was loaded with 0.4 wt% carbon black rather than 0.2 wt% due to the lower liquid thickness in the column. The co-solvent for the nanofluid comprised of either H2O or H2O and MeOH at a ratio of 1:1 wt:wt. The nanofluid was pumped at a flow rate of 1.9 mL/min. The nanofluid flows through the regeneration container where the CO2 is regenerated and measured


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using a gas collection line. At the bottom of the regeneration container, the CO2 lean nanofluid is flowed back into the absorption container with the peristaltic pump. The lean nanofluid reabsorbs CO2 and flows into the regeneration container, completing the cycle. Results and Discussion We hypothesized that basic, physical phenomena including stirring dynamics and viscosity changed the total amount and rate of CO2 release. These physical properties would affect the rate at which the particles move through solution (Figure 1). We determined the CO2 regeneration efficiency by measuring the CO2 release profile of the nanofluids under the presence of light. The nanofluid was placed in a custom flask where light entered with a known irradiance. The resulting photothermal release of CO2 was measured using a mass flow meter and CO2 concentration meter. First, we examined how the viscosity of the capture solvent changed the efficiency using gelatin to modify the viscosity of water. We found that increasing the nanofluid viscosity from 3.7 cP to 20.6 cP decreased the CO2 regeneration efficiencies by 88% (Figure 2) confirming that viscosity reduced the efficiency of the photothermal release process. One explanation for decreased efficiency is the reduction in movement of the CO2 bubbles out of solution resulting in a lower mass transfer of CO2. With an increased viscosity, we hypothesized that the microbubbles that form from the photothermal process reside longer in solution. The increased residence time allows reabsorption of the CO2 back into solution as the bubble moves out of the photothermally induced localized heat. Next, we examined how the boiling point changed the efficiency. We refer to the boiling point throughout, though it is more likely vapor pressure. However, as the gas within the photothermal heating process has an unknown temperature and pressure, we use boiling point for purposes of comparing multiple solvents. Our screen of CO2 regeneration using multiple co-solvents with MEA revealed trends in physical characteristics that appeared to correlate to bulk characteristics of the nanofluids. The co-solvents were chosen from known MEA cosolvents with similar absorption capacities (Table 1).28 With this screen, we did not initially find a correlation. However, separating the protic solvents from the aprotic solvents, a trend between regeneration efficiency and boiling point emerged (Figure 3). The boiling points of the protic solvents ranged from 65 °C to 197 °C, resulting in regeneration efficiencies ranging from 1.37 ± 0.45 mol/MJ to 13.15 ± 0.05 mol/MJ. The higher regeneration efficiencies with lower boiling points may also be because the lower boiling point solvents also had lower viscosities. We found that with lower boiling point solvents, the rate of the bubble expansion was higher than those with the higher boiling point solvents (Supporting Information). The increased volume of the bubble likely leads to enhanced buoyancy and therefore lower residence times. When the aprotic solvents were examined, similar trends were found. The boiling points of the aprotic solvents ranged from 102 °C to 240 °C, resulting in regeneration efficiencies ranging from 3.14 ± 0.63 mol/MJ to 12.69 ± 1.54 mol/MJ. It is possible that differences in heats of absorption influenced by hydrogen bonding can account for shifted regeneration efficiencies of the aprotic solvents. We confirmed that both viscosity and boiling point change the release of gas during a photothermal process, however, we had not directly tested the hypothesis of gas bubbles traveling through solution. We examined the mass transfer and bubble path length directly by using a vertical magnetic stirrer (Figure 4). The vertical stirrer directs the nanofluid convection to either flow with or against the direction of the photothermally generated gas bubbles. When stirring so that the nanofluid convection flowed with the movement of the nanoparticles, we observed regeneration efficiencies of 5.1 ± 0.2 mol/MJ and total CO2 release of 1.21 ± 0.04 g. When the direction of stirring was reversed, the regeneration efficiencies decreased to 3.7 ± 0.4 mol/MJ and the total CO2 release decreased to 0.90 ± 0.03 g, representing a decrease of 28% and 26%, respectively. The direction of the stirring either increases or decreases the bubble residence time and subsequently decreases or increases regeneration efficiencies, respectively. Last, with the understanding that viscosity and boiling points affect CO2 regeneration from MEA nanofluids, we sought to incorporate these concepts into creating more applicable solar CO2 regenerator. In order to implement a more practical photothermal CO2 regeneration scheme, the CO2 capture nanofluid must continuously be regenerated and circulated (Figure 5a). CO2 is bubbled into the nanofluid within an absorption flask. The CO2 loaded nanofluid is then pumped through a column where it is exposed to light. The exposure photothermally releases CO2 where it is measured using a mass flow meter and CO2 concentration meter. The leaner nanofluid is then pumped back into the absorption flask where it is reloaded with CO2. In such a system, the fluid levels of the sections exposed to light may have an impact on the regeneration efficiencies. We found that minimizing the fluid level enhanced the regeneration efficiency over a fully filled apparatus from 3.68 ± 0.42



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mol/MJ to 5.12 ± 0.19 mol/MJ, an increase of 45% (Figure 5b). The decreased fluid volume resulted in forming a film of flowing solvent in the column. The film, as opposed to a bulk volume, created a shorter path-length for the CO2 to escape and resulted in higher efficiencies. Using mixtures of solvents, specifically methanol, also enhanced regeneration efficiencies and indicated that solvent mixtures could be used to obtain optimal process conditions. When we combined methanol with H2O as a co-solvent with a thin film of the nanofluid, we obtained regeneration efficiencies in a continuous, flowing system of 9.82 ± 0.72 mol/MJ. Using this value, an estimated 0.45 km2 of surface area would be required to regenerate CO2 emitted from a 500MW coal-fired power plant with an average solar insolation24 of 561 W/m2. Conclusions In conclusion, we explored a range of solvents and their effects on the photothermal desorption of CO2 from monoethanolamine. By changing the co-solvent for monoethanolamine, it was possible to either inhibit or enhance the photothermal desorption process. We saw initial trends relating co-solvent viscosity and boiling points to the efficiency of the photothermal desorption process. Lower viscosities and lower boiling points both correlated with increased regeneration efficiencies. We hypothesized that the change in regeneration efficiencies was due to these physical properties affecting desorption bubble residence times. We explored the effects of bubble residence times through several experiments. Gelatin was added to the nanofluids to increase viscosity as a non-reactive modifier. We also used a vertical stirrer to either increase or decrease residence times. Each of these experiments indicated that lower residence times led to increased photothermal desorption of CO2 from a nanofluid. Finally, we used the knowledge that minimizing gas bubble transport times enhanced regeneration efficiencies to construct a continuously regenerating system. We found that minimizing the fluid volumes in the regenerating regions of the apparatus and using co-solvent mixtures allowed for more efficient CO2 regeneration. The regeneration efficiency of the more optimized system enables the possible use of MEA nanofluids as a CO2 capture solvent as the required surface area for implementation was reduced from ~2.3 km2, as reported previously7, to ~ 0.45 km2 for a 500 MW coal-fired power plant. Future work can explore the effects of nanoparticle size, optimized solvent ratios for process conditions, and long-term stability and reusability of nanofluid mixtures.

Figure 1. Effects of physical properties on photothermal CO2 regeneration. Viscosity, boiling point, and convective forces can all have an impact on the photothermal regeneration process. In each case, there is the potential to increase the velocity of nanoparticles and gas bubbles out of the solution, liberating the gas. For CO2 regeneration, this can lead to enhanced process efficiencies.


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Figure 2. Effect of viscosity on regeneration efficiency. Using gelatin as a viscosity modifier, the nanofluid viscosities were increased, resulting in a decrease in regeneration efficiency. As the solution became more viscous, the residence time of the carbon black nanoparticles in solution increased, allowing for more reabsorption of CO2 back into the solution.

Figure 3. Co-solvent boiling point. As boiling points increased, regeneration efficiencies decreased. The correlation follows for both protic and aprotic co-solvents, with the aprotic solvents shifted to the right.



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Figure 4. Convection enhanced photothermal CO2 regeneration. Using a vertical stirring device, the direction of the nanofluid convection either flowed with or against the direction of the nanoparticles and gas bubbles. Positive convection resulted in enhanced regeneration efficiencies over negative convection.

Figure 5. Continuous photothermal regeneration. (A) Schematic. CO2 is absorbed into the nanofluid in a round bottom flask. The nanofluid is pumped through a Vigreux column where light initiates the photothermal regeneration of CO2. The fluid at the bottom of the column is pumped back to the absorption flask to continue the cycle. The top of the column is connected to CO2 meter and flow meter for analysis. (B) Comparative regeneration efficiencies. The liquid levels in the column were set as either a thin film or a filled column. The thin film obtained higher regeneration efficiencies due to the lower residence times of the gas bubbles. Using methanol with H2O as the co-solvent also results in higher regeneration efficiencies.

Co-Solvent

Protic/ Aprotic

Boiling Point (°C)

Viscosity (cP)

Total CO2 Release (g)

Regeneration Efficiency (mol/MJ)

Maximum CO2 Release Rate (g/hr)

Water

P

100

1.0

1.10 ± 0.04

4.50 ± 0.40

1.33 ± 0.14


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EtOH

P

78

1.1

1.14 ± 0.07

6.93 ± 0.94

1.73 ± 0.12

EG

P

197

17

0.59 ± 0.13

1.37 ± 0.45

0.55 ± 0.11

Methoxyethanol

P

125

1.7

1.08 ± 0.06

3.98 ± 0.19

1.12 ± 0.17

Methanol

P

64.7

0.5

1.70 ± 0.19

13.15 ± 0.05

2.70 ± 0.14

DMF

A

152

0.9

1.10 ± 0.03

5.57 ± 0.36

1.41 ± 0.07

NMP

A

202

1.7

0.86 ± 0.12

4.84 ± 0.62

1.07 ± 0.05

DMAC

A

165

0.9

1.10 ± 0.03

4.82 ± 0.42

1.34 ± 0.11

2Pyrrolidone

A

240

13.3

0.78 ± 0.08

3.14 ± 0.63

1.01 ± 0.14

DMF DMA

A

100

1.2

4.20 ± 0.69

12.69 ± 1.54

2.90 ± 0.10

Table 1. Co-Solvent properties with photothermal regeneration. ASSOCIATED CONTENT

Experimental details, bubble growth rate. The Supporting Information is available free of charge on the ACS Publications website at http:pubs.acs.org AUTHOR INFORMATION

Corresponding Author * E-mail: [email protected] Author Contributions The manuscript was written through contributions of all authors. All authors have given approval to the final versions of the manuscript Notes The authors declare no competing financial interest ACKNOWLEDGEMENT

Professor Esser-Kahn was supported by the AFOSR Young Investigator Program under FA9550-12-10352, a 3M Non-Tenured Faculty Award, and an ACS-PRF Doctoral New Investigator Award. D.T. Nguyen was supported by the Department of Defense (DoD) through the National Defense Science & Engineering Graduate Fellowship (NDSEG) Program. N115 carbon black was generously supplied by the Cabot Corporation. REFERENCES

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