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DOE OSTI2020

Coal direct chemical looping process: 250 kW pilot-scale testing for power generation and carbon capture

Chemical looping combustion (CLC) is an energy conversion technology that can produce concentrated CO 2 stream without the need for a gas separation step, and thus, has the potential to drastically reduce the energy consumption and cost associated with CO 2 capture in power generation. The coal-direct chemical looping (CDCL) process is a CLC technology that uses a moving bed reducer configuration that can directly consume coal as a feedstock without requiring an upstream gasification step. An integrated 250 kW th CDCL pilot unit using iron-based oxygen carriers was constructed and demonstrated for over 1000 h of testing. The principles for the CDCL pilot unit design and operation are summarized in this article. During the 288-hour continuous operation testing, the CDCL pilot unit achieved >96% coal conversion with a CO 2 purity of >97%. Low carbon carryover into the combustor, i.e. <2%, was also confirmed during the test, which shows the capability of the moving bed reactor to retain and convert coal using the oxygen available on the iron-based oxygen carrier. The results from the pilot unit testing confirms the CDCL concept as a promising coal combustion technology for heat and power generation with CO 2 capture.

10 SYNTHETIC FUELS↗

DOE OSTI2018

A metallic peanut-shaped carbon nanotube and its potential for CO 2 capture

One of the greatest challenges in greenhouse gas reduction is to develop low-cost materials capable of efficient CO 2 capture. Carbon, due to its flexible bonding characteristics, numerous allotropic forms, and lightweight, is an attractive material for such investigation. Inspired by the experimental synthesis of C 50 Cl 10 in milligram quantities and recent works on peanut-shaped carbon nanotubes (PSNT), using state-of-the-art first-principles theory and molecular dynamics simulation, here we have discovered a new form of C 50 fullerene-based PSNT, α-PSNT. which is not only dynamically and thermally stable, but also energetically more stable than previously identified PSNTs composed of C 50 cages, and can withstand temperatures to 1000 K. Due to its unique atomic configuration, α-PSNT exhibits interesting physical properties including a high heat capacity, ultra-soft mechanical property with Young's modulus being a quarter of single-walled carbon nanotube (SWNT), and chirality independent metallicity. A systematical study of the adsorption properties reveals that both pristine and N-doped α-PSNTs have better CO 2 adsorption properties than SWNTs. The underline mechanism is that the intrinsic metallicity improves its ability to capture CO 2 as well as other gases because of the high density of electronic states at the Fermi level.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Solvent-free and one-pot synthesis of ultramicroporous carbons with ultrahigh nitrogen contents for sulfur dioxide capture

SO 2 from industrial tail gas is of great significance to control the environmental issues potentially induced by SO 2 emission. In the present work, porous carbons with rich ultramicropores and ultrahigh N contents (11.5–17.3 wt%) were synthesized by directly pyrolyzing the mixtures of glucose and urea at 700 °C, without the use of any solvents. Additionally, the synthesized porous carbons were characterized for porosity, morphology and elemental compositions, and also systematically investigated for SO 2 capture performance. Furthermore, it is found that the adsorption of SO 2 on synthesized porous carbons shows chemical behavior, owing to the strong acid-based interaction between SO 2 and pyridinic N. As consequence, the SO 2 capacities of synthesized porous carbons are very high, especially at low pressures (4.16 mmol/g at 296.2 K and 10 kPa). The synthesized porous carbons also display impressive adsorption selectivities for SO 2 /CO 2 /N 2 mixed gas, and good reversibility for SO 2 adsorption. Thus, it is believed that the synthesized porous carbons are promising candidates for selective and reversible SO 2 capture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Ultra-selective membrane composed of charge-stabilized fixed carrier and amino acid-based ionic liquid mobile carrier for highly efficient carbon capture

Membrane technology has been extensively studied for CO 2 capture applications, especially for flue gas sources. In the past decades, facilitated transport membranes (FTMs) have made breakthroughs overcoming the permeance-selectivity trade-off upper bound restricting traditional CO 2 separation membranes, but are still facing challenges towards practical applications, including limited performance, such as insufficient CO 2 /N 2 selectivity to achieve 95 % CO 2 dry-base purity by one step separation, and long-term stability. Herein, we designed and fabricated a novel FTM structure containing an ionic liquid (1-ethyl-3-methylimidazolium aminoacetate, [Emim][Gly]) as mobile CO 2 -carrier and a polymeric amine (polyethyleneimine, PEI) as fixed CO 2 -carrier. In this study, the fixed carrier is confined within a carbon nanotube (CNT) framework of 230 nm thickness via electrostatic forces adjusted by a polyelectrolyte (polystyrene sulfonate, PSS), while the mobile carrier diffuses freely within the CNT framework. After optimization of the membrane recipe and spray-coating fabrication procedure, following our previous work, the resulting CNT-PSS-PEI ~ IL membranes demonstrated an ultra-high CO 2 /N 2 selectivity up to 1,000 with CO 2 permeance up to 2,400 GPU (Gas Permeation Unit, 1 GPU = 3.348 × 10 -10 mol·s -1 ·m -2 ·Pa -1 ) under vacuum operation condition. Furthermore, one 100-cm 2 flat sheet membrane sample was prepared and exhibited one-stage CO 2 enrichment from 15 % to 95 % purity (dry-base) for the first time amongst all reported CO 2 separation membranes. The membrane retained a stable performance over 50-h operation period under vacuum condition. The extraordinary CO 2 separation performance illustrates the great potential of the CNT-PSS-PEI ~ IL membranes for flue gas carbon capture application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Efficient carbon capture using sub-textured polymer packing surfaces via 3D printing

Gas absorption is a common unit operation whose performance deeply relies on the gas liquid contact behavior. In this work, we report a solid polymeric surface feature containing microscale striation to improve the solid-liquid and gas-liquid contact and facilitate mass transfer. As a proof of concept, the surface feature is adopted for CO 2 capture absorber packing via 3D printing. Besides traditional embossing texture, an additional laminar striation is applied to the packing surface as a sub-texture. The packing shows notable CO 2 mass transfer increase without interfering with other key operating characteristics including pressure drop and liquid holdup. The improvement is based on the synergy of favorable wettability, thin liquid film and increased liquid mixing from rougher surface. In the demonstration test, the packing height could decrease by 33% using the advanced packing with same CO 2 removal, leading to a significant decrease in equipment size and capital expense for commercial CO 2 capture systems.

3D printing↗

DOE OSTI2014

Pi-CO₂ aqueous post-combustion CO₂ capture: Proof of concept through thermodynamic, hydrodynamic, and gas-lift pump modeling

Partnering in Innovation, Inc. (Pi-Innovation) introduces an aqueous post-combustion carbon dioxide (CO₂) capture system (Pi-CO₂) that offers high market value by directly addressing the primary constraints limiting beneficial re-use markets (lowering parasitic energy costs, reducing delivered cost of capture, eliminating the need for special solvents, etc.). A highly experienced team has completed initial design, modeling, manufacturing verification, and financial analysis for commercial market entry. Coupled thermodynamic and thermal-hydraulic mass transfer modeling results fully support proof of concept. Pi-CO₂ has the potential to lower total cost and risk to levels sufficient to stimulate global demand for CO₂ from local industrial sources.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

Solvent Degradation and Emissions from a 0.7MWe Pilot CO 2 Capture System with Two-stage Stripping

The UKy-CAER team successfully tested an advanced 0.7 MWe post-combustion CO 2 capture system on a coal-fired power plant using a heat integration process combined with two-stage stripping to enhance the CO 2 absorber performance. One of the unique feature of the UKy-CAER integrated process is a two-stage stripping unit for solvent regeneration. The secondary stripper is empowered by the heat rejection from a conventional steam-heated (primary) stripper. The secondary stripper outlet stream at the commercial scale can be used as boiler secondary combustion air, consequently enriching the flue gas with CO 2 , resulting in less energy penalty required by the CO2 capture system. The primary goal of this study was to form an initial assessment of the impact on the amine solvent from coal combustion flue gas contaminants and the potential higher oxygen content in the solvent due to incorporation of the secondary air stripper into the conventional amine scrubber/stripper system. The overall oxidative degradation was comparable to previous reports with 30 wt% MEA solvent at similar flue gas run hours. This suggests that the addition of the secondary air stripper appears to be negligible with regards to solvent oxidation.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2019

SimCCS: An open-source tool for optimizing CO 2 capture, transport, and storage infrastructure

Commercial-scale carbon capture and storage (CCS) technology will involve deploying infrastructure on a massive and costly scale. This effort will require careful and comprehensive planning to ensure that capture locations, storage sites, and the dedicated CO 2 distribution pipelines are selected in a robust and cost-effective manner. Presented in 2009, SimCCS is an optimization model for integrated system design that enables researchers, stakeholders, and policy makers to design CCS infrastructure networks. SimCCS 2.0 is a complete, ground-up redesign that is now a portable software package, useable and shareable by the CCS research, industrial, policy, and public communities. SimCCS 2.0 integrates multiple new capabilities including a refined optimization model, novel candidate network generation techniques, and optional integration with high-performance computing platforms. Accessing user-provided CO 2 source, sink, and transportation data, SimCCS 2.0 creates candidate transportation routes and formalizes an optimization problem that determines the most cost-effective CCS system design. This optimization problem is further solved either through a high-performance computing interface, or through third-party software on a local desktop computing platform. Finally, SimCCS 2.0 employs an open-access geographic information system framework to enable analysis and visualization capabilities. SimCCS 2.0 is written in Java and is publicly available via GitHub to encourage collaboration, modification, and community development.

42 ENGINEERING↗

DOE OSTI2017

Enhancements in mass transfer for carbon capture solvents part I: Homogeneous catalyst

The novel small molecule carbonic anhydrase (CA) mimic [Co III (Salphen-COO - )Cl]HNEt 3 ( 1 ), was synthesized as an additive for increasing CO 2 absorption rates in amine-based post-combustion carbon capture processes (CCS), and its efficacy was verified. 1 was designed for use in a kinetically slow but thermally stable blended solvent, containing the primary amines 1-amino-2-propanol (A2P) and 2-amino-2-methyl-1-propanol (AMP). Together, the A2P/AMP solvent and 1 reduce the overall energy penalty associated with CO 2 capture from coal-derived flue gas, relative to the baseline solvent MEA. 1 is also effective at increasing absorption kinetics of kinetically fast solvents, such as MEA, which can reduce capital costs by requiring a smaller absorber tower. The transition from catalyst testing under idealized laboratory conditions, to process relevant lab- and bench-scale testing adds many additional variables that are not well understood and rarely discussed. As a result, the stepwise testing of both 1 and the novel A2P/AMP solvent blend is described through a transition process that identifies many of these process and evaluation challenges not often addressed when designing a chemical or catalytic additive for industrial CCS systems, where consideration of solvent chemistry is typically the primary goal.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2017

Pilot testing of a heat integrated 0.7 MWe CO 2 capture system with two-stage air-stripping: Amine degradation and metal accumulation

An advanced 0.7 MWe small pilot coal-fired post-combustion CO 2 capture system with heat integration combined with two-stage stripping was tested here on a slipstream of flue gas by the University of Kentucky Center for Applied Energy Research (UKy-CAER). Evaluation of solvent degradation products was performed to determine the impact of oxygen exposure due to incorporation of the secondary air stripper into the conventional amine absorber/stripper system. The overall degradation rates and products observed during the testing campaign were comparable to previously published reports using 30% monoethanolamine (MEA) as the baseline/commissioning solvent. The rates of heat stable salt accumulation and amine degradation were similar to those from conventional CO 2 capture systems using MEA. Metal accumulation as the result of material corrosion inside the system from an improperly constructed material was observed. Finally, the impact of the secondary air stripper appears negligible relative to other published MEA campaigns tested at similar flue gas conditions and system operating hours.

03 NATURAL GAS↗

DOE OSTI2017

Pilot testing of a heat integrated 0.7 MWe CO 2 capture system with two-stage air-stripping: Emission

The University of Kentucky Center for Applied Energy Research (UKy-CAER) designed, constructed and tested an advanced 0.7 MWe post-combustion CO 2 capture system on a coal-fired power plant using a heat integration process combined with two-stage stripping to enhance the CO 2 absorber performance and lower the cost of CO 2 capture. Evaluation of emissions from the solvent and degradation products was performed to determine the impact on the amine solvent of coal combustion flue gas contaminants and oxygen exposure due to incorporation of the secondary air stripper into the conventional amine absorber/stripper system. The overall amine, ammonia and aldehyde emission levels observed during the baseline 30% monoethanolamine (MEA) solvent testing campaign were generally comparable to previously published reports tested at similar flue gas conditions and system operating hours. Ammonia emissions were correlated to high levels of iron and copper in the solvent, likely as a result of material corrosion.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2018

Growth response of environmental bacteria under exposure to nitramines from CO 2 -capture

Nitramines are potentially carcinogenic by-products of amines used in post-combustion CO 2 -capture. The influence of monoethanol (MEA)-, monomethyl (MMA)-, and dimethyl (DMA)-nitramines on the growth of environmental strains of bacteria, Pseudomonas fluorescens (P. fluorescens) and Rhodococcus spp. (R. spp.), was investigated in the laboratory. Additionally, the persistence of the nitramines in the presence of bacteria was determined. Growth of R. spp. was found to be sensitive to MMA-nitramine (EC 50 = 157 mg L -1 ), while P. fluorescens growth was insensitive to all nitramines tested. Moreover, P. fluorescens was capable of degrading 8–10% of the nitramines during the 33 h experiments. Results from this study provide insight into important processes of bacterial response to nitramines that merit further investigation considering the ongoing implementation of CO 2 capture technology.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Creative absorber design and optimization for CO 2 capture with aqueous piperazine

The Texas Carbon Management Program is preparing a Front-End Engineering Design (FEED) of the PZASTM (Piperazine with the Advanced Stripper TM ) for CO 2 capture at a natural gas combined cycle power plant in West Texas. This paper develops the absorber design for the capture system and studies the operational strategies of the absorber in response to ambient temperature swing. The design uses 2 absorber trains, and each train integrates absorption and a water-wash section in one column. Each column has a cross-section area of 174 m 2 and consists of 3 sections of MellapakPlus® 252Y structured packing. Packing heights for each section are 3, 4.9, and 2.7 m from top to bottom. A pump-around intercooler applied at the bottom bed circulates solvent and eliminates the direct contact cooler. The baseline CO 2 removal rate is 90% and will vary between 78% and 90% with ambient temperature. The system uses air cooling to eliminate cooling water usage. The water balance in the system will be managed by operating the water wash at a high circulation rate (1300 kg/h) to condense water during the night and make up for water loss during the day. Finally, the proposed design reduces the capital cost of the absorber column by minimizing the packing height and eliminating the direct contact cooler (DCC), and improves the energy cost by lowering the pump-around intercooling temperature and increasing the pump-around rate.

03 NATURAL GAS↗

DOE OSTI2023

Performance of hydrophobic physical solvents for pre-combustion CO 2 capture at a pilot scale coal gasification facility

Here, in this paper, we present the first pilot plant data for hydrophobic physical solvents for CO 2 and H 2 S removal from coal-derived H 2 -rich syngas. Four physical solvents were tested under pre-combustion CO 2 capture conditions at bench scale and pilot plant scale: one baseline hydrophilic solvent and three hydrophobic solvents. The solvents were: (1) polyethylene-glycol-dimethyl ether (PEGDME), a hydrophilic solvent analog for the commercial process Selexol, (2) tributyl- phosphate (TBP), a commercially available hydrophobic solvent, (3) polyethylene glycol-poly(dimethylsiloxane) (PEG-PDMS-3), and (4) diethyl sebacate (CASSH-1), a novel, computationally screened hydrophobic solvent developed by the National Energy Technology Laboratory (NETL). All solvents were studied under pure gas (CO 2 /N 2 /H 2 /CH 4 ) equilibrium conditions at NETL followed by pilot plant testing with syngas at the University of North Dakota Energy & Environmental Research Center (UND EERC). Long term performance of CASSH-1 and PEDGME was then assessed with results compared to process simulation predictions. Within experimental uncertainties, all solvents showed comparable CO 2 absorption performance at above room temperature operation while the hydrophobic solvents had limited water uptake and low vapor pressure, which alleviates concerns related to corrosion, water absorption, and solvent loss to evaporation. These results indicate low viscosity, low vapor pressure hydrophobic solvents are a promising option for lower cost CO 2 capture from high pressure syngas applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Fabrication of yeast engineered porous 13X adsorbent layers for CO 2 capture

This study investigates a novel environmentally friendly coating technique using yeast fermentation to obtain super porous Zeolite 13X adsorbent layers through freeze-drying technique for CO 2 capture applications. Several mass ratios of sugar to yeast were used to control the porosity and pore sizes in the adsorbent layer. A unique peeling process was integrated to obtain foamy, hollow structures to have deeper layer accessibility of adsorbent for adsorption applications. These coated adsorbent layers were experimentally characterized as a function of the mass ratio of sugar to yeast and adsorbent solid fraction. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and Fourier-transform infrared spectroscopy (FT-IR) are used to analyze the coated layers. Here, the void fraction for coated samples is found to vary between 0.48 and 0.56, making the samples applicable for adsorption applications. Adsorption performance experiments are performed to test the coated samples' performance compared to 13X powder. Due to their simplistic fabrication, cost-effectiveness, rapid pore formation, and high adsorption capacity, these porous 13X layers hold potential for large-scale fabrication and CO 2 capture applications.

Adsorbent coating↗

DOE OSTI2021

Polymeric membranes for CO 2 separation and capture

Over the past decade, CO 2 separation and capture have become the new bandwagon for polymer science and membrane research. This review presents the fundamentals of CO 2 /gas separation in polymeric membranes and discusses how these principles underpin opportunities and challenges for post-combustion carbon capture (CO 2 /N 2 ), hydrogen purification (CO 2 /H 2 ), and natural gas and biogas sweetening (CO 2 /CH 4 ). Emerging polymeric membrane materials are discussed, including a few polymers containing a high content of polar functional groups (i.e., ether oxygen-rich polymers and polymeric ionic liquids), shape-persisting glassy polymers (i.e., perfluoropolymers, thermally rearranged polymers, iptycene-containing polymers), and reactive polymers featuring facilitated transport. Moreover, the promising candidates for each CO 2 separation application are highlighted. Lastly, the permeability-selectivity data reviewed were plotted against their 2008 and 2019 upper bounds.

08 HYDROGEN↗

DOE OSTI2021

New sterically hindered polyvinylamine-containing membranes for CO 2 capture from flue gas

Amine-containing facilitated transport membranes can have both high permeability and selectivity due to the reversible reaction between CO 2 and amino groups for effective carbon capture from flue gas. In this study, we have developed an improved method for the synthesis of high-molecular-weight sterically hindered polyvinylamine (PVAm) as the new fixed-site carrier in thin-film composite membranes for CO 2 capture. Commercially available PVAm was N-monomethylated into poly-N-methyl-N-vinylamine (PVAm-CH 3 ) using the stepwise reductive amination with a highly polar fluorinated alcohol as the solvent to enhance the equilibrium shift to the formation of the imine intermediate. The method prevented over-alkylation, resulting in the increased yield of the target product. PVAm-CH 3 exhibited excellent CO 2 facilitation with a CO 2 permeability of 445.7 Barrer (1 Barrer = 3.349 x 10 –16 mol m m –2 s –1 Pa –1 ) and a CO 2 /N 2 selectivity of 70.3, which are above the Robeson 2008 upper bound. The PVAm-CH 3 solution retained a sufficiently high viscosity after incorporating the aminoacid salt, 2-(1-piperazinyl)ethylamine sarcosinate (PZEA-Sar), as the mobile carrier for the membrane coating on nanoporous polyethersulfone (PES) substrates without any penetration issues. The resultant thin-film composite PVAm-CH3/PZEA-Sar membrane with a thickness of approximately 170 nm exhibited a superior CO 2 performance of 1071 GPU (1 GPU = 3.349 x 10 –10 mol m –2 s –1 Pa –1 ) and a CO 2 /N 2 selectivity of 183 at 57°C and a feed gas pressure of 111.64 kPa (1.5 psig). This PVAm-CH 3 /PZEA-Sar membrane surpassed the latest redefined 2019 CO 2 /N 2 upper bound and outperformed other polymer-based membranes. Density functional theory calculations also demonstrated that PVAm-CH 3 showed a stronger preference, relative to PVAm, toward the more efficient bicarbonate pathway. Thus, the steric hindrance effect of PVAm-CH 3 enhanced the solubility of CO 2 in the polymer matrix and resulted in the higher CO 2 permeance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

13 C NMR study of amino acid salts in facilitated transport membranes for post-combustion carbon capture

Some of amino acid salts (AASs) have been demonstrated to be effective mobile carriers in facilitated transport membranes (FTMs) to achieve superior CO 2 permeance and CO 2 /N 2 selectivity for CO 2 capture from flue gas. Understandings of how the structures of different AASs affect the chemistry of the amine–CO 2 reaction are essential for the future development of more efficient AAS mobile carriers. In this study, the reaction chemistry of selected AASs with CO 2 was investigated by 13 C nuclear magnetic resonance (NMR) spectroscopy. The CO 2 loading and the distribution of major reaction products, including carbamate and bicarbonate products of each studied AAS were quantitatively analyzed. The positive correlation between the CO 2 loading of AAS (mol CO 2 /g AAS) and the CO 2 permeance of FTMs suggested that AAS with a higher CO 2 loading may improve the performance of FTMs. Our results also showed that increasing the steric hindrance of AAS could be a practical way to promote the bicarbonate reaction pathway and thus potentially increase the CO 2 loading (mol CO 2 /mol AAS). Moreover, 2-(1-piperazinyl)ethylamine (PZEA) was found to be a more effective multi-amine than piperazine (PZ) for synthesizing AASs due to the presence of more effective nitrogen sites per molecule. The superior CO 2 permeance of the PZEA-Sar membrane is also attributed to its more uniform membrane formation. As a result, the knowledge gained from this study will inform the rational design of more effective AAS carriers for CO 2 capture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗