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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Operation and Process Control Development for a Pilot-Scale Leaching and Solvent Extraction Circuit Recovering Rare Earth Elements From Coal-Based Sources

The US Department of Energy in 2010 has identified several rare earth elements as critical materials to enable clean technologies. As part of ongoing research in REEs (rare earth elements) recovery from coal sources, the University of Kentucky has designed, developed and is demonstrating a ¼ ton/hour pilot-scale processing plant to produce high-grade REEs from coal sources. Due to the need to control critical variables (e.g. pH, tank level, etc.), process control is required. To ensure adequate process control, a study was conducted on leaching and solvent extraction control to evaluate the potential of achieving low-cost REE recovery in addition to developing a process control PLC system. The overall operational design and utilization of Six Sigma methodologies is discussed. Further, the application of the controls design, both procedural and electronic for the control of process variables such as pH is discussed. Variations in output parameters were quantified as a function of time. Data trends show that the mean process variable was maintained within prescribed limits. Future work for the utilization of data analysis and integration for data-based decision-making will be discussed.

coal, rare earth elements, pilot plant, automation↗
DOE OSTI2013

Recovery from diabetes in neonatal mice after a low-dose streptozotocin treatment

Highlights: ► We monitored long-term beta cell regeneration in neonatal mice treated with low dose STZ. ► Low-dose STZ neonatal female mice recovered blood glucose in 150 days. ► Glucose intolerance of the STZ treated mice significantly improved in 150 days. -- Abstract: Administration of streptozotocin (STZ) induces destruction of β-cells and is widely used as an experimental animal model of type I diabetes. In neonatal rat, after low-doses of STZ-mediated destruction of β-cells, β-cells regeneration occurs and reversal of hyperglycemia was observed. However, in neonatal mice, β-cell regeneration seems to occur much slowly compared to that observed in the rat. Here, we described the time dependent quantitative changes in β-cell mass during a spontaneous slow recovery of diabetes induced in a low-dose STZ mice model. We then investigated the underlying mechanisms and analyzed the cell source for the recovery of β-cells. We showed here that postnatal day 7 (P7) female mice treated with 50 mg/kg STZ underwent the destruction of a large proportion of β-cells and developed hyperglycemia. The blood glucose increased gradually and reached a peak level at 500 mg/dl on day 35–50. This was followed by a spontaneous regeneration of β-cells. A reversal of non-fasting blood glucose to the control value was observed within 150 days. However, the mice still showed impaired glucose tolerance on day 150 and day 220, although a significant improvement was observed on day 150. Quantification of the β-cell mass revealed that the β-cell mass increased significantly between day 100 and day 150. On day 150 and day 220, the β-cell mass was approximately 23% and 48.5% of the control, respectively. Of the insulin-positive cells, 10% turned out to be PCNA-positive proliferating cells. Our results demonstrated that, β-cell duplication is one of the cell sources for β-cell regeneration.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2020

PILOT PLANT EVALUATIONS OF RARE EARTH ELEMENT RECOVERY AND CONCENTRATION FROM PRE-COMBUSTION BITUMINOUS COAL SOURCES

Rare earths and other critical elements are commonly associated with coal-based sources and sometimes at concentrations that may be attractive for recovery as a byproduct of coal production. The results obtained from laboratory research performed during the past five years have led to the design, construction and testing of a pilot plant that recovered rare earth elements from several bituminous coal-based materials including coarse refuse as well as solutions from a small heap leach and acid mine drainage. From this initial design, rare earth oxide (REO) concentrates having a purity greater than 90% have been produced using solvent extraction as the primary means of concentration. Following cost reduction and process intensification efforts, the circuit was revised to include feed calcination and several selective precipitation stages as a substitute for the original direct leach-solvent extraction circuit. Pilot test results revealed that the modified circuit was ideal for treating the relatively low-grade feedstocks and provided similar final REO purities at a significantly lower cost. This communication will present the flowsheets evaluated in the pilot plant along with technical and economic analyses for each circuit.

Coal↗
DOE OSTI2024

Testing the LSST Difference Image Analysis Pipeline Using Synthetic Source Injection Analysis

Abstract We evaluate the performance of the Legacy Survey of Space and Time Science Pipelines Difference Image Analysis (DIA) on simulated images. By adding synthetic sources to galaxies on images, we trace the recovery of injected synthetic sources to evaluate the pipeline on images from the Dark Energy Science Collaboration Data Challenge 2. The pipeline performs well, with efficiency and flux accuracy consistent with the signal-to-noise ratio of the input images. We explore different spatial degrees of freedom for the Alard–Lupton polynomial-Gaussian image subtraction kernel and analyze for trade-offs in efficiency versus artifact rate. Increasing the kernel spatial degrees of freedom reduces the artifact rate without loss of efficiency. The flux measurements with different kernel spatial degrees of freedom are consistent. We also here provide a set of DIA flags that substantially filter out artifacts from the DIA source table. We explore the morphology and possible origins of the observed remaining subtraction artifacts and suggest that given the complexity of these artifact origins, a convolution kernel with a set of flexible bases with spatial variation may be needed to yield further improvements.

Liu, S. (ORCID:0000000244612143)↗
DOE OSTI2017

Selection biases in empirical p(z) methods for weak lensing

To measure the mass of foreground objects with weak gravitational lensing, one needs to estimate the redshift distribution of lensed background sources. This is commonly done in an empirical fashion, i.e. with a reference sample of galaxies of known spectroscopic redshift, matched to the source population. In this paper, we develop a simple decision tree framework that, under the ideal conditions of a large, purely magnitude-limited reference sample, allows an unbiased recovery of the source redshift probability density function p(z), as a function of magnitude and colour. We use this framework to quantify biases in empirically estimated p(z) caused by selection effects present in realistic reference and weak lensing source catalogues, namely (1) complex selection of reference objects by the targeting strategy and success rate of existing spectroscopic surveys and (2) selection of background sources by the success of object detection and shape measurement at low signal to noise. For intermediate-to-high redshift clusters, and for depths and filter combinations appropriate for ongoing lensing surveys, we find that (1) spectroscopic selection can cause biases above the 10 per cent level, which can be reduced to ≈5 per cent by optimal lensing weighting, while (2) selection effects in the shape catalogue bias mass estimates at or below the 2 per cent level. Finally, this illustrates the importance of completeness of the reference catalogues for empirical redshift estimation.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2022

SCALED-PRODUCTION OF RARE EARTH OXIDES AND CRITICAL MATERIALS FROM COAL-BASED SOURCES

A projected exponential increase in the production of electric vehicles and high-end advanced technologies including those used in the defense industrial is expected to require nearly double the amount of rare earth elements (REEs) and critical elements currently available worldwide. As such, recovery from secondary sources such as coal and coal byproducts may be needed to meet the increased demand. A project has been initiated to evaluate methods and technologies integrated in an existing rare earth pilot plant that have the potential to improve the economics of extracting rare earths and critical materials from coal-based materials. This presentation will provide details about the technologies and results from pilot plant testing.

Honaker, Rick Q↗
DOE OSTI2013

Record high-average current from a high-brightness photoinjector

High-power, high-brightness electron beams are of interest for many applications, especially as drivers for free electron lasers and energy recovery linac light sources. For these particular applications, photoemission injectors are used in most cases, and the initial beam brightness from the injector sets a limit on the quality of the light generated at the end of the accelerator. At Cornell University, we have built such a high-power injector using a DC photoemission gun followed by a superconducting accelerating module. Recent results will be presented demonstrating record setting performance up to 65 mA average current with beam energies of 4-5 MeV.

43 PARTICLE ACCELERATORS↗
DOE OSTI2019

Improving the recovery of Ba from Sr Resin columns using chelating agents

Age dating of Cs-137 sources necessitates the accurate and precise quantification of the isotope Ba-137. In previous efforts to determine the age of Cs-137 source material, variation in Ba recovery was the largest source of uncertainty. This work investigates the use of several common chelating agents (EDTA, CDTA, DTPA, and NTA) to strip barium from Sr Resin columns quantitatively in an effort to improve the reproducibility of the separation. Batch studies showed conditions in which CDTA, EDTA, and NTA may suppress the retention of Ba on the column. Follow-up column studies showed excellent removal of barium from the column with quantitative recovery in the appropriate elution fraction. Our report builds upon previous studies and establishes additional chelating agents that could be used in an age dating separation procedure

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2023

Modular Functionalization of Metal‐Organic Frameworks for Nitrogen Recovery from Fresh Urine**

Abstract Nitrogen recovery from wastewater represents a sustainable route to recycle reactive nitrogen (Nr). It can reduce the demand of producing Nr from the energy‐extensive Haber‐Bosch process and lower the risk of causing eutrophication simultaneously. In this aspect, source‐separated fresh urine is an ideal source for nitrogen recovery given its ubiquity and high nitrogen contents. However, current techniques for nitrogen recovery from fresh urine require high energy input and are of low efficiencies because the recovery target, urea, is a challenge to separate. In this work, we developed a novel fresh urine nitrogen recovery treatment process based on modular functionalized metal–organic frameworks (MOFs). Specifically, we employed three distinct modification methods to MOF‐808 and developed robust functional materials for urea hydrolysis, ammonium adsorption, and ammonia monitoring. By integrating these functional materials into our newly developed nitrogen recovery treatment process, we achieved an average of 75 % total nitrogen reduction and 45 % nitrogen recovery with a 30‐minute treatment of synthetic fresh urine. The nitrogen recovery process developed in this work can serve as a sustainable and efficient nutrient management that is suitable for decentralized wastewater treatment. This work also provides a new perspective of implementing versatile advanced materials for water and wastewater treatment.

Guo, Lei↗
DOE OSTI2023

Modular Functionalization of Metal‐Organic Frameworks for Nitrogen Recovery from Fresh Urine

Nitrogen recovery from wastewater represents a sustainable route to recycle reactive nitrogen (Nr). It can reduce the demand of producing Nr from the energy-extensive Haber-Bosch process and lower the risk of causing eutrophication simultaneously. In this aspect, source-separated fresh urine is an ideal source for nitrogen recovery given its ubiquity and high nitrogen contents. However, current techniques for nitrogen recovery from fresh urine require high energy input and are of low efficiencies because the recovery target, urea, is a challenge to separate. In this work, we developed a novel fresh urine nitrogen recovery treatment process based on modular functionalized metal–organic frameworks (MOFs). Specifically, we employed three distinct modification methods to MOF-808 and developed robust functional materials for urea hydrolysis, ammonium adsorption, and ammonia monitoring. By integrating these functional materials into our newly developed nitrogen recovery treatment process, we achieved an average of 75 % total nitrogen reduction and 45 % nitrogen recovery with a 30-minute treatment of synthetic fresh urine. The nitrogen recovery process developed in this work can serve as a sustainable and efficient nutrient management that is suitable for decentralized wastewater treatment. This work also provides a new perspective of implementing versatile advanced materials for water and wastewater treatment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

New directions and principles for solvent extraction for recovery of lithium from aqueous brines and mineral leachates: A brief review

Increasing demand for lithium for manufacturing of batteries is fueling the unprecedented search for improved recovery and alternative sources. Wider source distribution, lower energy consumption, and greater sustainability make extraction of lithium from brines, both natural and process-derived, an attractive alternative to mineral ores. Solvent extraction, used industrially for production of metals, salts, and pharmaceuticals, has been investigated as a methodology for lithium recovery for several decades. However, industrial application of solvent extraction for lithium recovery has so far been limited. In contrast, direct lithium extraction using adsorbents based on inorganic minerals has rapidly advanced from research to commercialization. A comparison of solvent extraction processes to adsorption highlights these issues and explains the preference for adsorbents. Although the application of solvent extraction has been criticized for use of large amounts of acid, alkali, and organic solvents, steady progress has been made to improve its potential for industrial lithium production, spurred on generally by the advantages of solvent extraction in selectivity and throughput. Previously developed beta-diketone, organophosphate, and crown ether ligands are being adapted and improved. Their novel use with ionic liquids, deep eutectic solvents, and membrane technologies promises to expand capabilities for extraction of lithium from dilute aqueous sources while improving sustainability. Possibilities for further discovery and innovation abound. In this review, we provide a unique perspective from the field of solvent extraction starting with fundamentals such as ion-transfer theory and apply them to understanding lithium selectivity and extraction behavior. In conclusion, the results are cast in the light of the practical realities of developing economical solvent extraction processes.

Brine↗
DOE OSTI2013

Resource recovery from urban stock, the example of cadmium and tellurium from thin film module recycling

Highlights: ► The semiconductor layer on thin-film photovoltaic modules can be removed from the glass-plate by vacuum blast cleaning. ► The separation of blasting agent and semiconductor can be performed using flotation with a valuable yield of 55%. ► PV modules are a promising source for the recovery of tellurium in the future. - Abstract: Raw material supply is essential for all industrial activities. The use of secondary raw material gains more importance since ore grade in primary production is decreasing. Meanwhile urban stock contains considerable amounts of various elements. Photovoltaic (PV) generating systems are part of the urban stock and recycling technologies for PV thin film modules with CdTe as semiconductor are needed because cadmium could cause hazardous environmental impact and tellurium is a scarce element where future supply might be constrained. The paper describes a sequence of mechanical processing techniques for end-of-life PV thin film modules consisting of sandblasting and flotation. Separation of the semiconductor material from the glass surface was possible, however, enrichment and yield of valuables in the flotation step were non-satisfying. Nevertheless, recovery of valuable metals from urban stock is a viable method for the extension of the availability of limited natural resources.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Transmission-mounted combined energy recovery drive

An energy recovery drive system includes a motor-generator that is structured to selectively operate in a motor mode and a generator mode. A first shaft is operatively coupled to a transmission power take-off shaft. A second shaft is operatively coupled to the motor-generator and to an alternative power source. The energy recovery drive system is controllably operated in a plurality of operating modes. In a first operating mode, the motor-generator is in torque providing engagement with each of the first and second shafts. In a second operating mode, the motor-generator is in torque communicating engagement with each of the first and second shafts. In a third operating mode, which the motor-generator is in torque communicating engagement with the second shaft and is disengaged from transferring torque to the first shaft and from receiving torque from the first shaft.

Correa, Dixon Malcolm↗
DOE OSTI2014

Case Study of The ARRA-Funded GSHP Demonstration at the Natural Sources Building, Montana Tech

Under the American Recovery and Reinvestment Act (ARRA), 26 ground source heat pump (GSHP) projects were competitively selected in 2009 to demonstrate the benefits of GSHP systems and innovative technologies for cost reduction and/or performance improvement. One of the selected demonstration projects was proposed by Montana Tech of the University of Montana for a 56,000 sq ft, newly constructed, on-campus research facility – the Natural Resources Building (NRB) located in Butte, Montana. This demonstrated GSHP system consists of a 50 ton water-to-water heat pump and a closed-loop ground heat exchanger with two redundant 7.5 hp constant-speed pumps to use water in the nearby flooded mines as a heat source or heat sink. It works in conjunction with the originally installed steam HX and an air-cooled chiller to provide space heating and cooling. It is coupled with the existing hot water and chilled water piping in the building and operates in the heating or cooling mode based on the outdoor air temperature. The ground loop pumps operate in conjunction with the existing pumps in the building hot and chilled water loops for the operation of the heat pump unit. The goal of this demonstration project is to validate the technical and economic feasibility of the demonstrated commercial-scale GSHP system in the region, and illustrate the feasibility of using mine waters as the heat sink and source for GSHP systems. Should the demonstration prove satisfactory and feasible, it will encourage similar GSHP applications using mine water, thus help save energy and reduce carbon emissions. The actual performance of the system is analyzed with available measured data for January through July 2014. The annual energy performance is predicted and compared with a baseline scenario, with the heating and cooling provided by the originally designed systems. The comparison is made in terms of energy savings, operating cost savings, cost-effectiveness, and environmental benefits. Finally, limitations in conducting the analysis are identified and recommendations for improvement in the control and operation of such systems are made.

15 GEOTHERMAL ENERGY↗
DOE OSTI2026

Sustainable extraction of rare earth elements from coal fly ash leachates using a recyclable ionic liquid

The growing demand for rare earth elements (REEs) has prompted interest in their recovery from alternative sources such as coal fly ash (CFA). This study explores the ionic liquid (IL) betainium bis(trifluoromethylsulfonyl)imide, [Hbet][Tf 2 N], for selective extraction of REEs from leachates of a Class C CFA. While previous studies have demonstrated the effectiveness of using [Hbet][Tf 2 N] to extract REEs from different types of CFA in direct ash-IL systems, this study investigates four CFA leachates prepared using HCl, HNO 3 , H 2 SO 4 , and citrate. Extraction experiments were conducted across varying pH levels and with additives such as ascorbic acid and betaine. Among the systems tested, [Hbet][Tf 2 N] achieved REE recoveries of 51% and 47% from the HCl and citrate leachates, respectively, comparable to 49% REE recovery in ash-IL extraction. Co-extraction of bulk elements was significantly reduced in the leachate-IL systems. Optimal REE extraction occurred near pH 11, and addition of ascorbic acid effectively suppressed iron co-extraction without compromising REE recovery. Recycling experiments demonstrated that [Hbet][Tf₂N] retains its performance over five cycles with manageable losses. These results reveal the promise of [Hbet][Tf 2 N] for effectively recovering REEs from leachates of solid wastes, highlighting its applicability as a sustainable strategy for other aqueous REE feedstocks.

chemistry↗
DOE OSTI2026

Toward Lithium Recovery Using Modular (and Membraneless) Phase Separation and Extraction (MPSE) Technology with Ionic Liquid (IL) Solvents: Effect of Coatings

In this work, a single-channel slope-plate Modular and Membrane-less Phase Separation and Extraction (MPSE) device was fabricated using 3D printing. The slope-plate was designed with an insertable glass slide to enable surface modification with coatings. Self-assembled monolayers (SAMs) and perfluoropolyether (Zdol) coatings were applied to tailor surface wettability and enhance phase separation. Using a model biphasic system of water and hexadecane, both coatings significantly improved the separation efficiency compared to the uncoated device by promoting selective wetting. Building on these results, lithium extraction from a simulated saline solution was investigated using 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([EMIM][NTf₂]) as the ionic liquid (IL) extractant. The IL effectively extracted Li⁺ from the aqueous phase in bulk extraction, demonstrating its potential for lithium recovery. However, the low interfacial tension between the IL and aqueous phases posed challenges for phase separation. The application of SAM and Zdol coatings effectively mitigated this issue. Overall, integrating tailored surface chemistry with the slope-plate MPSE design shows great promise as an efficient and scalable platform for studying liquid–liquid separation and optimizing ionic liquid–based extraction processes for lithium recovery from saline sources.

3D printing↗
DOE OSTI2018

Evaluation of trace elements in U.S. coals using the USGS COALQUAL database version 3.0. Part II: Non-REY critical elements

Coal is a potential source of some valuable elements. In this work, concentrations of 25 critical elements in U.S. coals were evaluated using the COALQUAL Database Version 3.0 aiming to identify best coal sources for potential recovery of critical element. A method was proposed to calculate the mean concentrations of critical elements in U.S. coals, including Li (11.5 ppm), Be (1.9 ppm), Ti (721 ppm), V (21.6 ppm), Mn (50.8 ppm), Co (4.5 ppm), Ga (5.1 ppm), Ge (7.2p pm), Se (2.4 ppm), Zr (30.4 ppm), Nb (3.3 ppm), Sn (1.8 ppm), Sb (1.0 ppm), Ba (266 ppm), Hf (0.77 ppm), and Ta (0.19 ppm).Based on the calculated mean concentrations, a rough estimate indicates that U.S. coals contain a large amount of critical elements that are enough to meet U.S. demands for many years to come, if these elements can be commercially extracted. By comparing with the suggested cut-off grades, we found that 5.8% of the coal samples have Ga concentrations higher than the suggested cut-off grade. The percentages of promising coal samples (higher than cut-off grades) of other elements are below 3%. Results further indicate that despite some variations among elements, bituminous coals from the Appalachian region are likely to have high concentrations of Li, Ga, Be, Se, and Sb which make them a potential source of these critical elements. Bituminous coals from the Interior Coal Province, both Eastern and Western, were found to have relatively high probabilities of having high Ge concentrations. Furthermore very limited coal samples were found from mixed regions to have V and Zr concentrations higher than the corresponding suggested cut-off grades.

01 COAL, LIGNITE, AND PEAT↗