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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

From ash to oxides: Recovery of rare-earth elements as a step towards valorization of coal fly ash waste

Coal fly ash (CFA) is both a valuable waste material and a potential source of environmental contamination. The inclusion of metals such as rare-earth elements offer a possible incentive towards waste valorization if the metals can be extracted and recovered in an economical manner. Rare-earth elements (REEs) have many technological applications and are critically important in the manufacture of electric vehicles, communication devices, and industrial magnets. However, the global supply of rare-earth elements has faced shortages and price shocks. Current methods for separating and isolating individual rare-earth elements use large amounts of energy and organic solvents, raising concerns over environmental impacts. These factors have led to the investigation of nontraditional sources and separation techniques for these elements. Here, we describe a column-based system that uses a newly developed ligand-associated organosilica sorbent to concentrate and separate rare-earth elements from fly ash leachate. The fly ash used in this study originally contained 0.024 wt% rare-earth elements and the final oxide powder after enrichment contained > 10 wt% rare-earth elements, which is a enrichment of > 400 times. This process requires no additional organic solvents after the sorbent media has been synthesized, offering an alternative to the current standard using solvent extraction for rare-earth element recovery.

42 ENGINEERING↗
DOE OSTI2023

Organic acid solution having at least one ionic salt and at least one organic acid which is used for rare earth extraction

One or more embodiments relates to a process for extracting Rare Earth Elements (REEs) from REE-bearing underclays, claystones, shales, coal-mining waste, and waste coal. In at least one embodiment the process includes contacting the REE-bearing underclays, claystones, shales, coal-mining waste, and waste coal with an Organic Acid Solution (OAS) comprising at least one organic acid and at least one ionic salt at a predetermined ambient temperature and predetermined pH; and separating the REE from the REE-bearing underclays, claystones, shales, coal-mining waste, and waste coal, forming REE+Yttrium (REY) concentrate.

Verba, Circe↗
DOE OSTI2023

Laboratory-Scale Coal-Derived Graphene Process (Final Report)

The Energy & Environmental Research Center (EERC) conducted a laboratory-scale coal-derived graphene (CDG) project focused on developing a technological process for making graphene from four U.S. domestic coal or coal wastes, including lignite from North Dakota, subbituminous coal from Wyoming, bituminous coal from Utah, and anthracite from Pennsylvania. The project was divided into two performance or budget periods (BPs), with BP1 comprising the up-front laboratory experiments to make graphene materials from coal beginning on May 1, 2020, to April 30, 2022. BP2 was conducted from May 1, 2022, to April 30, 2023, and was focused on analyzing the CDG process economic feasibility and the technical gaps for technological scale-up and commercialization. During this project, a few different coal-derived high-value products have been demonstrated, including graphite, graphene oxide (GO), reduced graphene oxide (rGO), and graphene quantum dots (GQDs). A new graphite microstructure was discovered and named “croissant graphite” because of the exterior morphological and textural resemblance to croissant food items sold in commercial groceries stores. The new graphite structure and the associated preparation from coal or coal waste feedstocks has been the subject of a U.S. patent application. The systematic experimental processes involving coal cleaning, upgrading, and conversion to high-value carbon products culminated into a developed upgraded coal-to-products (UCP) technology that is being pursued for potential fast-track commercialization, if funding is available. It is envisioned that commercialization of the UCP technology would increase consumption of U.S. domestic coals or coal wastes to make environmentally sustainable high-value products for the electronics industry, high-energy-storage applications, and clean energy technologies such as electric vehicle (EV) lithium-ion batteries (LIBs), for which graphite has become a critical mineral commodity. Croissant graphite microstructures, when observed by field emission scanning electron microscopy (FESEM), display wavy surface morphology and often grow from a base that is made of graphitized particles with honeycomb-like layers, which are believed to be graphene layers. While more studies are needed to fully ascertain the mechanisms of the croissant graphite microstructure formation, it is postulated that their growth may begin from curling of the graphene sheets into ribbon-like structures, and continuous growth and densification of the ribbon-like structures forms croissant microstructures. Additional studies are ongoing to evaluate the electrochemical performance of croissant graphite for LIB applications and to determine the experimental conditions necessary to tune on/off croissant formation so that it can be either optimized or suppressed depending on performance evaluation results. In addition to the discovery of croissant graphite, the graphitization process from the four coal ranks in general was successful. X-ray diffraction (XRD) analysis showed that the degree of graphitization (DoG) ranged from 12% to 80% in an early sample set, and further optimization on lignite coal produces a DoG of about 92%, which was spectacular to see as lignite is the lowest-rank coal. Thus, it is expected that the graphitization performance for higher-rank coals will be similar or better when optimized as well. The coal-derived graphite was used to make GO and rGO. Analytical characterization, e.g., by methods such as Raman spectroscopy, XRD, Fourier transform infrared (FTIR) spectroscopy and FESEM, showed that the sequence of converting the coal to graphite, exfoliating it to GO, and then chemically reducing the GO to rGO was successful. Although coal naturally contains aromatic compounds and some relatively small-sized condensed aromatic units, it does not contain graphene sheets. In the UCP process, the aromatic domains in the coals, particularly low-rank coals, are concentrated and condensed further into graphene sheets, which are ordered into a 3D stack during graphitization. The synthesized graphite is then unpacked by methods such as exfoliation to various graphene products. GQDs were synthesized from all four coal types, and their optical properties were demonstrated to be tunable by the coal precursor preprocessing treatments. In all four coal types, enhanced optical properties were observed for the produced GDQs with incremental improvements made to the coal precursors. GQDs produced from raw coal samples displayed lower ultraviolet–visible (UV–Vis) spectroscopy absorbance intensity compared to those obtained from cleaned and upgraded coal residues. The photoluminescence (PL) intensities also varied with pretreatment conditions and with the concentration of GQDs in aqueous solutions. GQDs obtained from anthracite show longer emission wavelengths and can be excited by visible light as opposed to GQDs derived from the other coal ranks. UV fluorescence 3D maps and spectra revealed that the emission wavelength at which the GQDs solutions display the highest intensity was slightly redshifted based on the coal precursor pretreatments. In low-rank coal (lignite and subbituminous) samples, two clusters were observed in the maps for GQDs, which may suggest that there are potentially two types of fluorophores in solution or two main size populations. The ability to tune the properties of GQDs based on processing methods can be exploited to make GQDs for various optical display or optoelectronics applications. The results also highlight the importance of removing coal-borne impurities to improve the quality of the coal precursor for preparation of graphene products. Coal and/or coal wastes preprocessing methods were developed and applied to clean and upgrade the coal precursors prior to graphitization and subsequent conversion to graphene products. The preprocessing methods involve high specific-gravity separations, mineral acid cleaning (no hydrofluoric acid), and subsequent upgrading by reducing the coal-borne heteroatom (nitrogen, sulfur, and oxygen) content using proprietary chemical agents. Analytical characterization revealed that the preprocessing steps were successful, with ash reductions that range from 38% to 80% and residual ash content that was below the 5 wt% initial target. Based on proximate and ultimate analysis, the heteroatom reduction reactions produced upgraded coal residues with the oxygen content reduced by 8% to 24%, with additional reductions in the nitrogen and sulfur contents. An initial assessment of the waste streams from the UCP process shows very small to negligible environmental impact due to CO 2 , NO x , and SO x because most process steps are performed under inert atmosphere with argon. Consequently, reactive oxygen environments that tend to create these species are avoided. The inorganic and potentially hazardous species are released into aqueous waste streams that are easy to handle for proper disposal. The liquid waste streams were found to contain low-level concentrations of rare-earth elements (REEs), which could be concentrated and recovered as value-added by-products. Additionally, the volatile and gaseous fractions from carbonization and heat treatment contain useful organic compounds that can also be recovered as potential valuable by-products. Thus, the UCP technology is considered an environmentally sustainable and promising emerging technology for making high-value products from coal and coal wastes, with potential additional value-added by-products. Analysis of potential markets for the coal-derived carbon products shows a strong demand in both niche market sectors and across a wide variety of other industrial sectors. Graphite is currently considered a critical mineral commodity that has a large and growing demand in the LIB industry for EV applications. Based on data from Fortune Business Insights (2022) and Marketwatch (2023) reports, the average global graphite market is projected to reach about 33 billion by 2028, growing at a compound annual growth rate (CAGR) of about 7%, with much of this growth expected to be in the LIB industry. GO and rGO have strong market potentials in various application areas, such as coatings for anticorrosion, anti-icing, and antimicrobial protection, thermal barriers, wear resistance, sensors, additive manufacturing such as 3D inks, and others. GQDs are the emerging key player in the bioimaging, photovoltaics, and light-emitting diodes (LEDs) applications, with the potential to replace traditional semiconductor quantum dots (SQDs), which are based on metallic systems that are more toxic and more expensive. Biomedical applications of GQDs are becoming more attractive because of low to no toxicity and extremely low cost compared to SQDs. The major challenges for scale-up and commercialization of coal-derived carbon products such as graphene vary from the inherent attributes of graphene itself to reluctance to accept graphene in new manufacturing processes because of the uncertainty of the unknown. The 2D nature of graphene materials with a thickness of one atom presents significant challenges to proper handling/processing, and process scale-up becomes difficult because it requires high-end, expensive equipment, even for routine handling and analysis for quality assurance and control. Pristine graphene can also be extremely difficult to work into other matrices, thus hindering downstream processibility, especially at large scale. Currently, the cost of graphene and graphene products is still high and presents an economic risk that tends to slow down investment in scaling up emerging technologies. The lack of a standard for graphene materials for quality assurance and quality control poses a great challenge not only for the markets but also for commercialization efforts. A first-look economic feasibility analysis of the UCP technology provided valuable information that suggests the UCP process would be feasible, especially when it is scaled to a pilot scale and could be more competitive at the full scale. Graphitization was found to be the most energy-consuming and most capital-intensive step in the overall process. In small laboratory- and bench-scale experiments, labor is a significant contributor to the total process costs. Although these energy, capital, and labor constraints contribute to a higher selling price for the product, a preliminary economic model suggests that the process would be feasible at large scale when the process is fully integrated, optimized, and automated.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2020

Methods and systems for biological coal-to-biofuels and bioproducts

Methods and systems for the biological conversion of pretreated or solubilized coal or waste coal into biofuels. Coal (10) may be pretreated perhaps in a pretreatment reactor (13). Pretreated coal or even solubilized coal may be introduced into a processing reactor such as a bioreactor (16) containing a plurality of microorganisms (9) such as oleaginous microorganisms which can convert at least some of the pretreated or solubilized coal into lipids (19) or biomass (18), which then may be used directly or as a precursor for various products such as biofuels, feedstock, or the like.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2020

Patterns of Trace Element Accumulation in Waterfowl Restricted to Impoundments Holding Coal Combustion Waste

Waterfowl are often exposed to and readily accumulate anthropogenic contaminants when foraging in polluted environments. Settling impoundments containing coal combustion waste (CCW) enriched in trace elements such as arsenic (As), selenium (Se), and mercury (Hg) are often used by free-ranging migratory and resident waterfowl and represent potential sources for contaminant uptake. To assess accumulation of CCW contaminants, we experimentally restricted waterfowl to a CCW-contaminated impoundment and quantified trace element burdens in blood, muscle, and liver tissues over known periods of exposure (between 3 and 92 d). From these data we developed models 1) to predict elemental bioaccumulation with increased exposure time, and 2) to predict muscle/liver burdens based on concentrations in blood as a nondestructive sampling method. Although Hg and As did not bioaccumulate in our waterfowl, we observed an increase in Se concentrations in muscle, liver, and blood tissues over the duration of our experiment. Furthermore, we found that blood may be used as an effective nondestructive sampling alternative to predict muscle and liver tissue concentrations in birds contaminated with Se and As through dietary exposure. These data provide unique insights into accumulation rates of contaminants for waterfowl utilizing habitats contaminated with CCW and demonstrate the efficacy of nonlethal sampling of waterfowl to quantify contaminant exposure. Environ Toxicol Chem 2020;39:1052–1059.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Recovery and Enhanced Upgrading of Rare Earth Elements from Coal-Based Resources: Bioleaching and Precipitation

Rare earth elements (REEs) are of great importance to modern society and their reliable supply is a major concern of many industries that utilize them in metal alloys, semiconductors, electrical equipment, and defense equipment. REEs in the coal waste have been revealed to be an alternative resource for REEs production. In this study, the extraction, recovery, and upgrading of the REEs from coal waste has been realized with the bioleaching and precipitation processes. Reliable and sustainable acid and oxidant production from the oxidation of the pyrite with Acidithiobacillus ferrooxidans to generate acid for leaching were realized in this research. The acidified bioleaching solution was used to extract REEs from coal waste, with 13–14% yields for most REE elements (~72 h of leaching). However, recovery for longer duration tests was significant higher (varies from 40–60% for individual REEs). After extraction, precipitation and separation processes were designed with the aid of Visual Minteq calculations and modeling to concentrate the REEs. With the procedures designed in this research, a final REEs precipitate product containing 36.7% REEs was produced.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2024

Performance Testing of a Moving-Bed Gasifier Using Coal, Biomass, and Waste Plastic Blends with Washed and Unwashed Legacy Coals and Other Waste Fuels to Generate White Hydrogen

The objective of this effort, primarily funded by the United States Department of Energy (DOE), and led by the Electric Power Research Institute, Inc. (EPRI), with support by Hamilton Maurer International (HMI) and Sotacarbo S.p.A. (Sotacarbo), has been to qualify coal, biomass, and plastic waste blends based on performance testing of selected fuel pellet compositions in a pilot-scale updraft moving-bed (UDMB) gasifier. The testing provided relevant data to advance the commercial-scale design of the moving-bed gasifier to be able to successfully use these feedstocks to produce hydrogen. In particular, the effects of waste plastics on feedstock development (i.e., blending and pelletizing) and the resulting products (i.e., syngas compositions, organic condensate production, and ash characteristics) are the focus. The gasifier used for testing is HMI’s moving-bed gasifier, which has been proven capable of gasifying nearly all coal ranks. It has also shown the ability in prior testing work to gasify wood chips (biomass). However, mixtures of these fuels with plastic wastes have not been prepared and gasified together. The three feedstocks were densified and pelletized by California Pellet Mill (CPM) to meet the feedstock size required by Sotacarbo’s 30mm ID UDMB gasifier, under contract to HMI. The technical tasks and results from this two-year research project included: (1) Feed Procurement and Preparation: Nine different tri-fuel pellets were prepared from varying compositions of fresh mined PRB coal, corn stover biomass, and car fluff waste plastics. Tri-fuel pellets were produced by CPM and shipped to Sotacarbo’s test facility in Carbonia, Sardinia, Italy. (2) Test Plan Development: A test plan was created to define the test runs to be performed. The test plan detailed the different UDMB gasification tests to be performed in Sotacarbo’s 12-inch ID pilot scale gasifier, the process monitoring instrumentation used, and the extractive samples recovered for analysis of the total gasification process mass and energy balance. (3) Gasifier Testing: Nine different gasification runs were performed in the pilot-scale gasifier at Sotacarbo using nine different fuel feedstock compositions generated from varying mixtures of PRB coal, biomass, and plastic wastes. The testing generated performance data on gasification reaction efficiency and performance, yielding relevant data for models used to scale up the gasifier design. This task also included work to refurbish and reassemble the pilot gasifier at Sotacarbo and perform a baseline 100% PRB coal run. (4) Data Analysis and Reporting: Review of the data, determination of figures of merit, and interpretation of the results are reported in the project’s final report, published in March 2024. The results show that all tri-fuel pellets gasified well and maintained structural integrity throughout the gasification process. The syngas generated can be shifted to hydrogen by using commercial syngas shifting technologies. (5) High Fidelity computational fluid dynamics (CFD) Simulation: The National Energy Technology Laboratory (NETL) team performed CFD simulations of the UDMB gasifier for two of the tri-fuel pellets gasified in Sotacarbo’s pilot scale gasifier. The kinetic mechanisms for the pyrolysis of each constituent, PRB coal, corn stover biomass, and waste plastics are based on thermogravimetric analysis performed by Sotacarbo. The gasification model was validated by comparing the predicted syngas composition at the exit of the gasifier with the measured syngas composition. In addition, the reactor’s measured internal temperature profile agreed well with the predicted internal reactor temperature profile. These results validate that the model can be used to predict the performance of the updraft moving bed gasifier for different feedstocks and operating conditions. This paper summarizes the results of the completed work in which the pelletizing procedure was validated to ensure the viability of the tri-fuel pellets for the gasification runs performed at Sotacarbo’s 30 mm UDMB gasifier. The gasification performance data from this series of nine runs will enable modeling of a full-scale HMI industrial scale gasifier supporting both combined heat and power, and Hydrogen production from coal (both fresh mined and legacy) combined with various biomass and waste plastics. Additionally, plans and progress on a follow-up project, being executed by the same project team, will be presented. In this project, a total of twenty (20) different feedstocks are being prepared from varying compositions of biomass (both woody biomass and corn stover) with a mixture of legacy coal waste, plastic waste, and refuse-derived fuel (RDF). The testing will provide information on gasification reaction efficiency/performance, yielding relevant data for models used to scale up the gasifier design to 50 megawatt electric (MWe) (equivalent hydrogen production). Tests will also be performed on a bench-scale fluidized-bed gasifier for comparison purposes. The results of this testing will be used to specify the range of feedstock blends that can be successfully gasified as well as quantify gasifier outputs based on specific blends.

08 HYDROGEN↗
DOE OSTI2023

Assessing and Improving Biooxidation for Acid Generation and Rare Earth Element Extraction

Microorganisms (Acidithiobacillus ferrooxidanns) are effective in oxidizing ferrous ions that can be used to oxidize pyrite and produce sulfuric acid. Many coal waste resources contain significant concentrations of rare earth elements (REE) and critical materials (CM) that can be extracted using sulfuric acid. These coal waste resources often contain significant concentrations of pyrite, which if not utilized or removed present a future environmental liability for potential acid mine drainage. Thus, the combination of pyrite and REE/CM in coal waste provides a significant resource opportunity for sulfuric acid generation that can be utilized using biooxidation. In addition, the pyrite concentrate used for acid generation also contains REE/CM content that is released during biooxidation of the pyrite concentrate that augments the REE/CM release from the main ore being leached with the acid generated from the pyrite. Thus, this approach provides a very significant environmental advantage as well as augmented REE/CM recovery. Although there are many studies associated with biooxidation in relation to mineral oxidation, there is a lack of information regarding the effects of operating parameters on biooxidation performance and optimization for practical applications. In this study, findings from research in assessing and improving biooxidation for acid generation for REE/CM extraction are presented. Results show that bacteria can very effectively and efficiently oxidize ferrous ions to ferric ions, which oxidize pyrite to produce acid for REE/CM extraction. The factors that showed significant impact on biooxidation performance include air flow rate, stirring speed, residence time, solids concentration, and temperature. The dominance of Leptospirillum ferriphilum species was noted in the bioreactor after a prolonged period of operation, although Acidithiobacillus ferrooxidanns was used in the beginning.

Free, Michael L.↗
DOE OSTI2024

Performance Testing of Moving Bed Gasifier Using Biomass and Waste Fuels to Generate Low-Cost Clean Hydrogen

Our need for hydrogen is growing as the world transitions toward a low-carbon future. Hydrogen provides long-term energy storage for grid stability in a solar- and wind-dominated power market and can be used to decarbonize other sectors. One promising process for generating low-cost hydrogen that produces net-negative carbon is to gasify biomass with a mixture of legacy coal wastes, waste plastics, and other wastes with carbon capture. Use of waste fuels lowers costs and diverts waste from landfills. EPRI is leading a project, funded by the U.S. Department of Energy, to conduct performance testing of modular, moving-bed gasification for the generation of low-cost, clean hydrogen from biomass mixed with legacy coal waste, waste plastic, and/or refuse derived fuels. The work scope includes preparation of multiple pellet feedstocks using biomass (both woody biomass and corn stover) with a mixture of legacy coal waste, plastic waste (wire insulation), and refuse-derived fuel (RDF). These pelletized feedstocks are being qualified based on performance testing of selected fuel blend compositions in updraft moving-bed gasifier located in Sardinia, Italy. Testing is being conducted to obtain relevant data to advance the modular design of the moving-bed gasification process, and successfully use these feedstocks to produce a high hydrogen content raw syngas that can be shifted to produce clean hydrogen. Testing results will be used to determine the effects of the various fuels on feedstock development, the resulting products (i.e., syngas compositions, organic condensate production, and ash characteristics), and impacts on gasifier operations.

08 HYDROGEN↗
DOE OSTI2026

Online LIBS–ML Framework for Dynamic Characterization of Heterogeneous Waste-Derived Gasification Feedstocks

LIBS−ML framework for real time feedstock characterization during continuous conveyor transport Heterogeneous waste derived feedstocks (e.g., waste coal, biomass and blends) introduce rapid variability in heating value and ash chemistry that affect gasifier operation, yet conventional laboratory characterization techniques are too slow to support proactive control. To address this gap, this study reports on an online, in situ, dynamic characterization framework that couple’s laser-induced breakdown spectroscopy (LIBS) with leakage safe machine learning (ML) regression to deliver real time, decision quality predictions of gasifier relevant properties. A controlled sample matrix spanning two different waste coals, two different biomasses, and engineered blends under two particle size conditions were constructed and benchmarked using standardized laboratory analyses for proximate/ultimate properties and ash composition. LIBS spectra were acquired dynamically as material flowed on a conveyor belt, using high energy 1064 nm laser ablation and shot averaging to improve repeatability and precision. Supervised regression models (multi layer perceptron (MLP) /artificial neural network (ANN), random forest (RF), and support vector regression (SVR)) and an optimized weighted ensemble were trained on emission line feature sets using nested cross validation with Bayesian hyperparameter tuning and validated against an independent hold out set. The proposed LIBS−ML workflow achieves near laboratory predictive fidelity across parametric targets (including higher heating value (HHV), ash content, fixed carbon, sulfur, major ash forming oxides, and initial deformation temperature (IDT)), with the weighted ensemble providing a robust default predictor under dynamic measurement conditions. These results demonstrate a practical pathway for real time feedstock characterization that can enable feedforward adjustments and more resilient gasifier operation for variable quality waste derived fuels.

Biomass↗