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DOE OSTI2019

Low Cost Rare Earth Element (REE) Recovery from Acid Mine Drainage Sludge

In this research effort, three core technologies were evaluated for REE concentration and recovery: (1) Nanofiltration (NF), (2) Electrically conductive membranes for induced rare earth oxide (REO) precipitation, (3) dendrimer-based sorbents for REE capture. The NF showed excellent selectivity between REE components and monovalent ionic salts such as K and Na. For all AMD samples, iron selectivity is a critical challenge since it is the highest concentration bulk constituent. Membrane electrodeposition approach shows promise for scandium and cerium recovery, but iron selectivity not observed. This technology may therefore be more appropriate REE recovery technology for non-iron rich streams such as coal ash. P-dendrimer derived sorbent shows promise for aqueous application, with high sorption capacity for iron demonstrated, and pH tunable selectivity against REE sorption. Although in some cases excellent selectivity for REE was observed, the REE concentrations from all four AMD sites was low enough that the 2wt% final goal was not attained.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Low-Temperature Plasma Treatment for Enhanced Recovery of Highly Valued Critical REEs from Coal (Final Report)

The principle objective of this project was to develop a novel process flowsheet using low-temperature plasma treatment (LTP) integrated with conventional hydrometallurgical processes to recover rare earth elements (REEs), especially highly valued REEs (i.e. scandium and critical REEs), from coal and coal byproducts. LTP treatment was used to pretreat the solid feed material prior to leaching in an effort to improve the leaching characteristics of the REEs and potentially reduce acid consumption. Initially, a detailed experimental program was performed on a laboratory LTP furnace to identify a set of process parameter values to be used for assessing the enhanced leaching performance achieved on four specific gravity fractions of West Kentucky No. 13 and Fire Clay coarse coal refuse materials. High-temperature oxidation (HTO)) was also evaluated as a means for improving REE leachability on the same fractions of both coal sources. The lixiviants used to assess leachability improvements included: i) untreated water, ii) 0.1 M ammonium sulfate solution and iii) 1.2 M sulfuric acid solution at a temperature of 75°C. The laboratory data was used to develop multiple process flow sheets using HTO only to produce a rare earth oxide mix concentrate or utilizing both LTP and HTO treatment processes to generate a high purity heavy REO mix concentrate and a light REO mix concentrate. A techno-economic analysis was performed on each circuit. Low-temperature plasma oxidation was found to enhance REE leaching characteristics for all specific gravity (SG) fractions of the West Kentucky No. 13 coarse refuse material. The leaching recovery improvement was preferentially achieved for the heavy REEs with higher values obtained when treating the lower density fraction material. For example, the leaching recovery for the heavy REEs in the untreated 1.6 SG Float fraction material was 8% in a 0.1 M ammonium sulfate solution. After LTP treatment for 32 hours, heavy REE recovery increased to 33%. The corresponding recovery value for the light REEs was 10%. These findings indicate a strong affinity of the heavy REEs with the organic material, which is the component being reduced in content during the LTP treatment. Scanning electron micrographs showed the development of a honeycomb structure with increased LTP treatment with higher surface area as confirmed from BET measurements. Higher surface area promotes improved leaching efficiency due to enhance chemical interactions. When using 1.2 M sulfuric acid, the LTP treatment was found to provide a heavy REE recovery increase from 23% to 53% for the 1.6 SG Float fraction which corresponded to an ash content increase from around 20% to 35%. However, LTP treatment provided no improvement in leaching characteristic for the 2.2 SG sink material in the acid solution, which was likely due to the low organic content. The LTP treatment of the Fire Clay SG fractions provided no improvement in REE leaching characteristic, which may be due to the association with REE minerals such as monazite and REE-associated mineral matter such as clays. High temperature oxidation using temperatures in the range of 600-750OC was found to significantly enhance the leaching characteristics of both the light and heavy REEs for all density fractions in both coarse coal refuse materials. Generally, the increase in light REE recovery for the West Kentucky material was from 15% for the untreated material to 90% for the HTO treated material at 600°C. Recovery values dropped significantly when using temperatures below 600°C and above 750°C. The impact of the excessive temperatures was most likely a result of sintering. For the heavy REEs, HTO significantly improved recovery in the lighter SG fractions, which may be due to an affinity with the organic content. Only limited heavy REE recovery improvement was obtained for the denser SG fractions. Another benefit of HTO is the conversion of calcium-based minerals to a very soluble calcium oxide, which is removable using a mild acid solution, and the conversion of Fe minerals to relatively insoluble minerals such as hematite and magnetite. The pregnant leaching solution produced from the leaching of all SG fractions obtained from both coal sources was treated using two stages of solvent extraction procedurally modeling a rougher-cleaner circuit followed by oxalic acid precipitation. Rare earth oxide products having a purity greater than 97% was produced from nearly all of the SG fractions. A novel process flowsheet was developed based on the selective leaching of heavy REEs that was made possible through LTP treatment of West Kentucky No. 13 coarse refuse followed by salt leaching. In the flowsheet, coal refuse material is ground to a top size of 1mm and then treated by LTP. The treated material is mixed into a 0.1 M ammonium sulfate solution and then filtered to produce a heavy REE enriched pregnant leach solution. The heavy REEs are concentrated by two stages of selective precipitation to produce a heavy REE mix oxalate and then roasted to obtain a heavy REO mix concentrate. The solid residues remaining after salt leaching is dried and then subjected to HTO treatment followed by concentration using selective precipitation and roasting to produce a light REO mix concentrate. An alternative circuit was developed using HTO treatment only to treat 100% of the coarse refuse material followed by selective precipitation and roasting to generate a high purity REO mix product. A techno-economic analysis performed for the treatment of West Kentucky No. 13 and Fire Clay coarse refuse based on a hypothetical 500-tph plant revealed that the net present value for all scenarios was significantly negative. Primary reasons include: i) a substantial decrease in the basket value of the final product relative to the feed and ii) high chemical costs relative to the amount of product generated. The basket value reduction was primarily due to little to no scandium recovery due to poor leaching characteristics when using low acid concentrations as necessitated by the low feed grades. Operating costs were primarily influenced by the chemical costs relative to the kilograms of concentrate produced and feed grade. For the Fire Clay coarse refuse material, the total operating cost was estimated to be $354 per kg of REO produced which was higher than the basket value of the REO product ($276/kg). Approximately 37% of the total cost was the sulfuric acid used during the leaching process. A comparative analysis performed to assess the economic viability of using low-temperature plasma furnaces found that market value enhancement for the generation of both heavy REO and light REO concentrates will be needed in addition to significant technology advancements to reduce the cost of plasma furnaces.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

At-source Recovery of Rare Earth Elements from Coal Mine Drainage

Conventional acid mine drainage (AMD) treatment consists of pH adjustment, oxidation, and separation of solid precipitates from discharge quality water. Alkaline addition increases the pH to the range 7 to 9 to precipitate the regulated metals Al and Mn ions as hydroxides. Mechanical or chemical oxidation then converts the reduced iron species Fe 2+ to Fe 3+ which precipitates at a low pH value as ferric hydroxide (Fe(OH) 3 ). Co-precipitation of Rare Earth Elements (REEs) with hydroxides creates a gangue-rich matrix from which REEs must be separated. Fe(OH)3 is generally the most abundant gangue-forming metal. Current research by the project team has shown raw, untreated AMD has an average total rare earth element content (TREE) of about 287 μg/L (0.287 ppm). Operators of AMD-producing facilities are obliged to treat it to neutralize acidity and remove regulated metals (e.g., iron (Fe), aluminum (Al), and manganese (Mn)) prior to discharge. Ongoing research indicates conventional AMD treatment concentrates TREE in resulting precipitates (AMD sludge) by an average factor of 2,635x to an average dry weight, elemental concentration of 708 g/t (ppm). While the economics of recovering REEs from AMD sludge are appealing, much of the cost of REE recovery would be incurred during separation of REEs from the gangue metals: Fe, Al, and Mn. Significant gains can be made by precipitating REEs when most of these gangue metals are still in solution. Significant improvements in REE extraction efficiency can be obtained through separation of REEs from the aqueous phase AMD, upstream of conventional AMD treatment by: 1) creating an enriched REE feedstock, 2) producing a more consistent feedstock, 3) reducing transportation costs to an REE refinery, 4) reducing acid consumption in the acid leaching step, and 5) reducing the volume of waste produced at the ALSX plant. This project is exploring two novel approaches for extracting REEs upstream of the conventional AMD treatment plants to create a purified REE feedstock while leaving the bulk of the Fe, Al, and Mn in solution for subsequent treatment. While the average TREE concentration of raw AMD is low and individual sites range between 10 and 2,200 μg/L, successful at-source REE separation will generate a superior feedstock to a conventional ALSX process and significantly improve the economics and environmental performance of REE extraction from AMD. AMD can be classified into two types: type A is net acid and iron is partly oxidized while type B is net alkaline, and iron occurs in the reduced, ferrous state. In Case A, the pH is raised slightly, which will precipitate Fe 3+ and Al 3+ but not REEs. The other important type of AMD is net alkaline water found in flooded, anoxic deep mines. These generally have a pH > 6.0 and are net alkaline. REE concentrations are also much lower than those found in acidic AMD while the volumes and flux are much higher. Most of these are pumped discharges with almost no Al. Case B AMD is strongly reduced and, like Case A water, Fe and Mn ions are similarly reduced and therefore soluble at pH <9.0. REEs and an array of transition ions will be the only trivalent cations in this type of AMD. In Case B, both upward pH adjustment under reducing conditions and application of an electrochemically stimulated supported liquid membrane strategy to separate REEs from ferrous ion will be explored.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Continuous Water Quality Sensing for FGD Wastewater

The coal fired plant power industry requires new solutions for on-line monitoring of flue gas desulfurization (FGD) wastewaters for regulated trace metals to reduce recurring operating and off-site laboratory analysis costs and provide a high level of confidence of compliance with state and federal discharge guidelines. The University of Alabama at Birmingham (UAB) developed an integrated water sensor package for continuous water quality monitoring of flue gas desulfurization (FGD) wastewaters for concentration measurements of Selenium (Se). UAB utilized a diverse team of University Professors/Staff Members/Student(s) (Engineering and Innovative Technology Development Group), a University Affiliated Research Institution from the local area (Southern Research), and a cost sharing Industry Partner (Metrohm). The team developed and validated a proprietary wet chemistry batch process for water sample preparation; and implemented this process as a fully automated on-line monitor prototype system. This prototype system’s performance was evaluated in both the laboratory and during in-field deployment to a coal fired power plant. In both environments it was found that the prototype system was unable to recreate the batch process’s success at preparing FGD water samples for total Se measurements with a commercial-off-the-shelf (COTS) cyclic anodic stripping voltammetry (CSV) system. Through this experience, UAB has provided insight into a number of specific areas where improvements can be made with respect to the COTS systems used in this project to yield a more complete and competitive industry solution for on-line monitoring of total Se in industrial wastewater.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Economic Extraction and Recovery of REEs and Production of Clean Value-Added Products from Low-Rank Coal Fly Ash

The University of North Dakota (UND) Energy & Environmental Research Center (EERC) teamed with Pacific Northwest National Laboratory (PNNL) , the North Dakota Industrial Commission Lignite Research Program, and commercial partners Basin Electric Power Cooperative, Great River Energy, and Southern Company to execute a Cooperative Agreement funded by the U.S. Department of Energy’s (DOE’s) National Energy Technology Laboratory (NETL) focused on identifying unique pathways and pretreatments to extract rare-earth elements (REEs) from low-rank coal (LRC) ash in a more economical and environmentally benign manner than current methods. The EERC drew upon the unique and deep knowledge of the team regarding LRC geochemistry, ash transformation mechanisms during combustion, and fly ash chemistry in the approach to understand the portioning of REEs in LRC ash. A comprehensive characterization effort was undertaken to fully establish the form, associations, and partitioning of the REEs and other elements/minerals of interest in fly ash, as well as the ash chemistry, mineralogy, and morphology. Using this information, the team tested methods of REE extraction to take advantage of the unique and advantageous properties of LRC ash. Multiple complementary approaches were evaluated that combined both novel and proven methods to develop an extractive process for REEs and other high-value metals from LRC ash that provide technological and economic progress on the current state of the art. Methodologies were also evaluated for the potential to synergistically remove toxic metals while extracting other high-value metals from the ash, generating a clean, safe ash material as a value-added product. This would eliminate waste and offer significant additional revenue potential. Based on laboratory-scale testing, an initial high-level technical and economic analysis to estimate operating expenses and product revenues to guide future phases of technology development was implemented. By focusing on minimizing process steps and consumptive use of extraction solutions, a tunable, economically viable process for REE extraction from LRC ash was developed. The tunable process has the ability to be adjusted to adapt to the differing ash chemical and physical properties that are characteristic of LRC ash. This is key to deployment as a commercial process. In demonstrating the process, the EERC was able to illustrate mixed REE concentration greater than the goal of 2 wt%. High-level economic analysis of the process with LRC ash of moderate REE levels demonstrated the potential of the process, but recovery of just the REEs was insufficient to cover operational costs. With the additional extraction of other high-value metals found in LRC ash, the process economics approach would break even, and it is anticipated that with process optimization, the developed process could potentially be economically sound. The same economic analysis performed utilizing LRC ash with high levels of REEs showed the recovery of the REEs alone would make the process economically viable even without further optimization.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Selective hydrothermal extraction of lanthanides: Mimicking natural ore-forming processes [Slides]

Rare Earth Elements (REE) consumption in the US was 20,000 metric ton in 2018. China controls 97% of the global REE market. The aims for new technology are to 1. Avoid investing in extraction of cheap LREE, extract M/HREE only → increase the value of the intermediate/final product, 2. Exclude extraction and concentration of U and Th → avoid investment in rad remediation, and 3. Maximize environmental friendliness of the technology. Hints from nature can aid in achieving these amis.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Advanced sorbents for modular oxygen production for REMS gasifiers

Under a DOE funded effort, Thermosolv LLC has been developing a sorbent-based oxygen production technology for gasification and oxy-combustion applications. The sorbents utilize oxygen-storage properties of certain perovskites to (1) selectively adsorb oxygen at moderate temperature from compressed air and (2) release the adsorbed oxygen into a vacuum or a sweep gas such as CO2 and/or steam. Through cyclic operations of multiple sorbent beds such a process can be made continuous. Pressure drop across the sorbent bed and other similar design considerations dictate that the sorbent be in the form of a high surface-area-to-volume pellet and yet still possess sufficient crush strength and integrity. Process efficiency is determined by the sorption and desorption kinetics and sorbent capacity. Typical process involves cycle times in the order of 100 seconds, a time too short to fully utilize the full volume of the sorbent and the sorption capacity of the sorbent pellets. As a part of this project, Thermosolv LLC undertook the development of oxygen sorbents as a high-surface area supported sorbent on a light-weight inert support to (1) reduce the cost, (2) increase the productivity, and (3) reduce the overall weight of the reactor. Using a previously developed perovskite (LSCF 1991) with its well-characterized performance, composite sorbent pellets each consisting of an inert core coated by a thin layer of the functional perovskite material were produced. Several low-density, inexpensive inert solids supports in the 1/8”-1/4” size were selected to keep the pressure drop across the sorbent bed in the acceptable range. A number of commercial technologies including spray coating, dip coating, incipient impregnation of porous substrate followed by thermal annealing at various temperatures and duration were employed and tested to produce robust composite supported sorbent pellets. A sense of optimum coating thickness was developed by testing sorbent pellets of various increasing diameter pellets. LSCF-1991extrudates ranging in size from 1/32” to 3/16” were tested in a TGA and in a fixed-bed pressure swing test set-up for sorption/desorption cycles of interest. The data show that for the operational conditions of interest the coating thickness for a supported sorbent pellet needs to be approximately 1/32” (about 0.8 mm). Subsequent work thereby concentrated on developing composite pellets of various substrates, shapes and sizes with coating layer of about this size range. Candidate support materials were chosen based on cost, inertness, mechanical strength, thermal expansion and chemical stability with sorbent material, and in a size range to give an acceptable pressure drop in fixed-bad reactor configurations. Coating application methods used for application of the sorbent onto the support included precipitation, spray coating and dip coating from sorbent slurries and sol gels. For all coated supports where we could successfully apply a uniform coating of desired thickness with an acceptable handling performance in terms of exfoliation, TGA-based cyclic sorption/desorption testing was performed to determine cycling capacity of oxygen. Among nearly twenty different support materials tested, best adhesion performance was obtained from stainless saddle supports. In the bench-scale fixed-bad tests stainless steel saddle support composite pellets with a coating thickness in the 0.6 mm or so range, the composite sorbent pellet performance approached up to 95% of that of the 2 mm parent material pellets. In a parallel approach to reducing the cost of the sorbent, alternate sorbent formulations replacing/reducing the amount of cobalt in the LSCF family were also investigated. Successful formulations that could match the performance of LSCF 1991 were identified based on TGA cyclic tests as LSCF 1919 and LSF 1910. In the range of operational envelop of cycle times and other relevant process operating conditions, the reduced Co formulations showed comparable performance in the bench-scale fixed-bad cyclic operations. As a part of this project, we also attempted substitution of La and Sr with Ca and Ba, and Co with Mn, Ni and Cu with little success, but the overall project goal of reducing sorbent cost in terms of raw material and manufacturing expenses was successful.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Sorption Enhanced Mixed Matrix Membranes for Hydrogen (H 2 ) Purification and Carbon Dioxide (CO 2 ) Capture

The technical objective of this project was to develop sorption enhanced mixed matrix membranes with H 2 permeance of 500 gas permeance units (GPU) and H 2 /CO 2 selectivity of 30 at 150-200 °C. These membranes will be the central component in the design of membrane based systems for 90% capture of CO 2 from coal-derived syngas, with 95% CO 2 purity at a cost of electricity 30% less than baseline capture approaches. The unique approach in this proposal is to design crosslinked polymers containing Pd-based nanoparticles achieving strong H 2 sorption and size sieving ability and thus H 2 /CO 2 selectivity. The specific objectives for each budget period (BP) are described below. BP 1: Identify polymer matrix with strong size sieving ability and palladium (Pd)-containing nanomaterials to prepare freestanding mixed matrix films with H 2 permeability of 50 Barrer and H 2 /CO 2 selectivity of 30 at 150-200°C with simulated syngas. BP 2: Prepare and optimize thin film mixed matrix composite membranes materials with H 2 permeance of 500 GPU and H 2 /CO 2 selectivity of 30 at 150-200 °C, and complete the modification of the membrane test unit for the field test in the BP 3. BP 3: Conduct a 20-day field test of the membranes with real syngas at Center for Advanced Energy Research (CAER) of the University of Kentucky (UKy). During the BP2, we have successfully prepared thin-film composite (TFC) membranes based on mixed matrix materials (MMMs) containing Pd nanoparticles in polymers, and demonstrated their superior and robust performance for H 2 /CO 2 separation at 150 – 225 °C. (1) Production of the Pd based nanoparticles with a diameter of 4 nm has been scaled up to 200 mg/day. (2) We have prepared TFC membranes with H 2 permeance above 500 GPU and H 2 /CO 2 selectivity above 30 at temperatures up to 225 °C, which meet the targets for the BP2. (3) We have conducted parametric studies of TFC membranes with a mixed gas containing H 2 S and H 2 O and demonstrated the stability of the membranes. (4) We have established a new testing plan at the Center for Advanced Energy Studies (CAER) at the University of Kentucky because NCCC decided to shut down their gasifier. During this project, four Ph.D. students received the inter-disciplinary training and graduated, including Shailesh Konda, Maryam Omidvar, Deqiang Yin, and Lingxiang Zhu. One postdoctoral researcher (Dr. Liang Huang) and two Ph.D. students (Abhishek Kumar and Hien Nguyen) are involved in this project. The project leads to one provisional patent application, eight peer-reviewed articles, and one manuscript in preparation. The details are shown below.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Materials and Approaches for Mitigation of SOFC Cathode Degradation in SOFC Power Systems

Perovskites such as doped lanthanum manganite and cobaltite have been used successfully as a cathode material in SOFC power systems operating between 700-1000°C. The electrodes, however, remain prone to degradation in presence of Cr containing gas atmosphere under systems operating conditions. Cathode in SOFCs is considered as one of the largest contributors of electrochemical performance degradations, leading to significant increase in ohmic and non-ohmic losses as well as interfacial compound formation. These degradations are mostly irreversible due to permanent changes to chemical and morphological alterations in the electrodes, resulting in the blockage of triple phase boundary (TPB) sites and decrease in oxygen reduction reactions (ORR). Fundamental mechanistic understanding has been developed to elucidate the reaction pathways of electrode poisoning in electronically conducting electrodes (LSM) as well as mixed ionic and electronically conducting electrodes (LSCF). The overall goal of this program has been identification and development of cost effective solutions to mitigate electrode degradations under “real world” systems operating conditions. The overall technological innovations and impact from this work are: The research provides an understanding of the degradation mechanism and cost-effective approaches for implementation in SOFC systems; Develop mitigation processes utilizing low cost getters using conventional synthesis and fabrication route; Develop tailored high surface area powders and coatings for high Cr capture capacity under systems operating conditions; >Developed computational models to understand mechanistic behavior; Experimentally measure rate of Cr evaporation from chromia and alumina forming alloys under SOFC operating conditions; Developed conditions to minimize Cr evaporation from balance-of-plant alloys; This innovation will support the development of getter platform to capture both intrinsic and extrinsic impurities present in air; and, Applications under wide operating temperature range (500-900°C) as well for wide high-temperature electrochemical systems (SOFC, SOEC, and OTM). The work has been successfully developed, validated experimentally and implemented. Successful technology transfer of this knowledge with industrial partners has been accomplished and the getters have been independently tested and validated under their systems operating conditions. The innovation will also find application in related high temperature electrochemical systems such as OTM and SOEC for the prevention of Cr assisted performance degradation. The proposed approach for Cr capture can also be applied to oxy-combustion and other advanced combustion techniques for the reduction of Cr vapor in the exhaust gas stream. This fundamental knowledge gained also has led to the path forward for developing advanced getters for capturing more than one contaminant in air.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Recovery of Rare Earth Elements (REEs) from Coal Mine Drainage, Phase 2

Phase 1 research identified a two-step refining train, acid leaching of AMD precipitate feed followed by solvent extraction (SX), to produce a 2% TREE product. For the Phase 2 bench scale system, the objective was to get the acid leaching step to operate in batch-mode with sufficient storage capacity to feed an aqueous, enriched REE liquor to a pilot SX plant operating in continuous-mode at a feed rate capable of producing 3 g/hr 2% TREE. Important process variables included feed rate, extractant makeup, flowsheet configuration, and stripping conditions. Operating parameters were optimized through a feedback-capable SCADA system configured for the SX bench scale plant. These conditions were met and exceeded. TREE grades approaching 90% were produced while our Techno-Economic Assessment indicated highly favorable economic returns. The project led to the design of a pilot facility for producing roughly 500 kg/TREE/year. That plant is now in the procurement stage with constructed expected to begin in late 2020.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

W.A. Parish Post-Combustion CO 2 Capture and Sequestration Demonstration Project (Final Technical Report)

The Petra Nova Project (Project) is a commercial scale post-combustion carbon capture project developed by a joint venture between NRG Energy, Inc. (NRG) and JX Nippon Oil Exploration (EOR) Limited (JX). The Project is designed to separate and capture carbon dioxide (CO2) from an existing coal-fired unit’s flue gas slipstream at NRG’s W.A. Parish Electric Generating Station (WAP) located southwest of Houston, Texas. The captured CO2 is dried, compressed, and transported via an 81-mile pipeline to the West Ranch oilfield (West Ranch) in Jackson County, Texas, where it is injected to boost oil production. The Project, which is partially funded by a grant (Grant) from the United States (U.S.) Department of Energy (DOE) under the Clean Coal Power Initiative (CCPI) Round 3, uses the Kansai Mitsubishi Carbon Dioxide Recovery advanced amine-based CO 2 absorption technology (KM-CDR Process®), which was jointly developed by Mitsubishi Heavy Industries, Ltd. (MHI) and the Kansai Electric Power Co. Inc., to treat and capture at least ninety percent (90%) of the CO 2 from a 240-megawatt equivalent (MWe) flue gas slipstream off of Unit 8 at WAP. When operating at full capacity, the Project captures approximately 5,200 short tons of CO 2 per day, which would otherwise be emitted into the atmosphere, representing the largest commercial scale deployment of post-combustion CO2 capture technology at a coal power plant to date. Under the Grant, the Project was managed in 3 phases: (1) Phase 1: Project Definition / Front End Engineering Design (FEED) (2) Phase 2: Detailed Engineering, Procurement & Construction (3) Phase 3: Demonstration and Monitoring. On December 29, 2016, commercial operation of the Project was achieved, ending Phase 2 and starting Phase 3, a 3-year demonstration period running from January 1, 2017 through December 31, 2019. The key objectives of Phase 3 were to (a) demonstrate the specific advanced technologies constructed during Phase 2 and (b) monitor the injected CO 2 at West Ranch to demonstrate technologies and protocols for monitoring, verification, and accounting (MVA). As of the end of Phase 3, Petra Nova captured 3,904,978 short tons of CO 2 (3,542,537 metric tons) that was transported to West Ranch. To support the DOE obligation to monitor, verify, and account for the sequestered CO 2 at West Ranch, Petra Nova contracted with the Bureau of Economic Geology (in the Jackson School of Geosciences at The University of Texas at Austin) to (a) design a monitoring program, (b) draft an MVA Plan for DOE review and approval, and (c) working with Petra Nova and the operator of West Ranch to manage and report on the MVA activity. This report discussed the technical aspects of the project during each of the 3 phases of the project as identified above.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Heat Integration Optimization and Dynamic Modeling Investigation for Advancing the Coal-Direct Chemical Looping Process

The purpose of the project is to address the optimization and startup operation of a modular coal direct chemical looping (CDCL) combustion system integrated with a steam cycle for power generation to reduce the risks involved in further scale-up of the technology. The modular reactor design of the CDCL process provides flexibility in the fabrication of the reactor and in its operating capacity (i.e. turndown ratio) at the cost of a more complex heat exchange network (HEN) design and integration. To address the technology gaps and advance the efficiency and economic feasibility of the CDCL technology, the project will perform a detailed and comprehensive analysis of the integration of a modular CDCL reactor system and a steam cycle system under both static and transient conditions via HEN process performance simulations and system dynamic modeling, respectively. The scope of work consists of 1) Experimental and computational studies of the CDCL combustor reactor 2) Comprehensive static (i.e. steady-state) system HEN design analysis in CDCL 550 MWe commercial unit for power generation and 3) Dynamic modeling of site specific design of 10MWe CDCL large pilot plant. The project team has successfully developed and validated a kinetic model for the oxidation of oxygen carriers in the combustor using the unreacted shrinking core model (UCSM). The model is capable of capturing the oxidation kinetics of fully or partially reduced oxygen carrier particles. A computational fluid dynamics (CFD) model is developed to simulate the hydrodynamics, heat transfer, and chemical reaction occurring in the CDCL combustor. The model is developed in MFIX and ANSYS Fluent. Key aspects of CDCL combustor operation, including heat transfer, oxygen carrier oxidation, and the transport of oxygen carrier particles, are simulated using this CFD model. The HEN for a commercial scale 550 MWe CDCL power plant is simulated and optimized using ASPEN Plus. Practical design considerations are incorporated based on industrial experiences. The performance and cost for the commercial CDCL plant is updated based on these analyses. A dynamic model for the 10 MWe CDCL pilot plant is developed in ProTRAX simulation software. The model is based on the pilot plant design developed in project DE-FE0027654 “10 MWe CDCL Large Pilot Plang – Pre-FEED Study” and the steam cycle data obtained from Dover Light & Power plant. The transient behaviors during pilot plant load variation are simulated using the dynamic model.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Intensified Flue Gas Desulfurization Water Treatment for Reuse, Solidification, and Discharge

The goal of this final project report is to summarize the work conducted on project DE-FE0031555. In accordance with the Statement of Project Objectives (SOPO), the University of Kentucky Center for Applied Energy Research (UK CAER) (Recipient) developed a hybrid electrochemical-membrane technology for treating wet flue gas desulfurization (WFGD) blowdown from coal-fired power generation plants that (1) removes government-regulated species and total suspended solids (TSS) via electrocoagulation with solid/liquid separation to avoid further treatments by a biological method specifically for selenium, and (2) reduces total dissolved solids (TDS) in a nanofiltration unit to promote water recycle and reduce freshwater intake. Additional technological configurations were pursued, including (1) nanofiltration combined with zeolite dewatering for a near-zero liquid discharge (ZLD) scenario, and (2) polishing discharge from zeolite dewatering using capacitive deionization (CDI) with 90+% salt rejection to produce water with less than 100ppm TDS for more beneficial use. Project results verified that UK CAER’s hybrid approach addressed the complexities of WFGD blowdown with simplified unit operation at relatively low capital investment by demonstrating: (1) an effective in-situ generated solid sorbent material, green-rust (GR), that specifically removes regulated dissolved species in WFGD blowdown, including selenium, arsenic, and nitrates; (2) a low-cost, high flux nanofiltration treatment that removes both monovalent and divalent species at >80% rejection to adequately provide water recycle and extend the life of FGD equipment by mitigating chloride aided pitting corrosion mechanisms; and (3) a solidification and stabilization process using pozzolanic agents that retain regulated species and satisfy the Resource Conservation and Recovery Act (RCRA) leachate requirements. UK CAER proved electrocoagulation with GR to be an intensified solution for effluent limit guidelines (ELG), and based on preliminary techno-economic analysis (TEA), in comparison to DOE’s Case 1 for Biological Wastewater Treatment that had a purchased equipment cost (PEC) of $\$$5.26 million and a Total plant cost (TPC) of $\$$30.0 million, the EC process had a PEC of $\$$2.67 million and the TPC of $\$$17.0 million. While the electricity consumption for Case 1 was 53 kW, it was 110 kW for the EC process due to dissolving iron for a three-stage reaction design. However, electricity consumption for the EC process could be significantly reduced by adopting a counter-current reactor design for at least a 6-stage chemical reaction operation.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Recovery of Rare Earth Elements (REEs) from Coal Mine Drainage, Phase 2

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

A Modular Heat Engine for the Direct Conversion of Natural Gas to Hydrogen and Power using Hydrogen Turbines (Phase I Final Report)

This report describes a novel, modular heat engine comprising of a one-step hydrogen production from natural gas with in-situ CO 2 separation which is amenable for re-use or sequestration. Combining with a hydrogen turbine subsystem, a distributed or central power generation system is conceived. An added hydrogen storage subsystem enables load-following capability. The techno-economics of the overall system compared favorably against current state-of-the-art natural gas combined cycle plants with post-combustion CO 2 capture.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2022

Improving Ni-Based SOFC Anode Resilience and Durability through Secondary Phase Formation

The project used a multi-disciplinary approach to test test if 2° materials, added to traditional cermet components, enhanced SOFC mechanical strength, anode resilience and durability when subjected to electrochemical and environmental redox cycling. Findings from fracture testing, electrochemical studies and operando Raman spectroscopy measurements demonstrated that aluminum titanate (Al 2 TiO 5 or ALT) mechanically mixed with NiO-YSZ cermets confers superior mechanical strength and slower degradation rates under polarization. No deleterious effects from ALT in conversion efficiency were observed. Specific accomplishments included the following: (1) Refined methods used to fabricate ALT enhanced anodes into bi-layer anode supports to achieve high power densities; (2) Compared the effects of adding ALT mechanically to Ni-YSZ powders prior to anode fabrication with adding ALT through infiltration and co-infiltration of YSZ scaffolds; (3) Tested the resilience of these novel materials to electrochemical and environmental redox cycling and thermal stresses commonly encountered in functioning SOFCs; and (4) Characterized the ability of ALT to improve the carbon tolerance of Ni-YSZ anodes operating with dry methane.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Zeolite Membrane Reactor for Pre-Combustion Carbon Dioxide Capture (Final Scientific/Technical Report)

Water-gas shift (WGS) reaction followed by carbon dioxide (CO 2 ) separation is a critical step in the integrated gasification combined cycle (IGCC) process for fossil-fuel-fired electrical power generation with CO 2 capture. To intensify the IGCC process hydrogen-permselective zeolite membrane reactor offers promise to replace the conventional energy-intensive fixed-bed reactors and solvent-based CO 2 capture units. The objectives of this project were to develop a bench-scale zeolite membrane reactor (total membrane area: 932 cm 2 for a 21-tube membrane bundle) for the water-gas-shift reaction of raw syngas from an oxygen-blown coal-gasifier for H 2 production with simultaneous CO 2 separation at the capability of about 2 kilograms H 2 per day (equivalent to 2 kW IGCC power plant) and to demonstrate significant progress toward achieving overall performance goal of 90% CO 2 capture rate with 95% CO 2 purity at the cost of electricity 30% less than the baseline carbon capture approaches. This report summarizes results obtained in this project on scaling up the zeolite membrane reactor by a factor of 200 in membrane area, tests of the bench-scale zeolite membrane reactor for the water-gas-shift reaction at high temperature and high-pressure, and techno-economic analysis of the integration of the zeolite membrane reactor in IGCC power plant for the electrical generation with CO 2 capture. With effective pore modification by catalytic cracking deposition of MDES (methyldiethoxysilane), fabrication of MFI-type zeolite membranes was successfully scaled-up from a lab-scale disk type to bench-scale multiple-tube bundles on low-cost alumina supports. A Co-Mo based sour shift catalyst was evaluated and used in the zeolite membrane reactors for water-gas-shift reaction. The reaction kinetic and gas-permeation equations were developed and employed in mathematic models to guide/predict experiments/performance of zeolite membrane reactors for water-gas shift reaction. Multiple-tube zeolite membrane bundles and reactors were designed, fabricated and tested for gas separation and water-gas-shift reactions with real raw syngas from a coal-fired gasifier operated at high temperature and pressure. The zeolite membrane reactors demonstrated good long-term thermal and chemical stability and constant H 2 permeance (>300 GPU) together with a Knudsen selectivity (~4.7) for H 2 over CO 2 in the field test (cumulative time >28 hours) with high-sulfur coal-derived syngas. The zeolite-membrane-reactor integrated IGCC process was designed using the performance experimentally measured by the University of Cincinnati team with a single-tube zeolite membrane reactor that offers a CO conversion >98% with more than 90% of CO 2 and H 2 captured. With the above integrative approaches, a techno-economic analysis for a cost-benefit comparison was performed to uncover features that determine the power output, capital expenditure, operating expenditure, cost of electricity and cost of CO 2 capture in a 550-MW zeolite-membrane-reactor integrated IGCC process. The integration of the zeolite membrane reactor in IGCC could provide a significant reduction of 80% and 27% in the power consumption for Selexol™ Acid Gas Removal and CO 2 compression, respectively, which lowers the total auxiliary power consumption by 12.5%. However, the low pressure required at permeate stream for maintaining the driving force of hydrogen permeation through the zeolite membrane costs a huge power in permeate compressor, compensating the power consumption reduction achieved with the membrane reactor. Thus, for coal-fired IGCC for electricity generation with 90% CO 2 captured, the integration of the membrane reactor could provide a CO conversion ~99% and a significant drop in cost-of-electricity using zeolite membrane with H 2 permeance >600 GPU and the H 2 /CO 2 selectivity over 70.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

The MFiX Particle-in-Cell Method (MFiX-PIC) Theory Guide

MFiX (Multiphase Flow with Interphase eXchanges) is an open-source multiphase flow solver developed at the National Energy Technology Laboratory. Within the code, users have access to a single phase or interpenetrating continua-based multiphase two-fluid model (TFM), a discrete element model (DEM), and a particle-in-cell model (PIC). TFM, DEM, and PIC can all be used to create multiphase simulations that include hydrodynamics, chemical reactions, and heat transfer.

01 COAL, LIGNITE, AND PEAT↗