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At least 55 records · Page 3

A Novel Continuous Ultrasound-Assisted Leaching Process for Rare Earth Element Extraction: Environmental and Economic Assessment

Rare earth elements (REEs) make up integral components in personal electronics, healthcare instrumentation, and modern energy technologies. REE leaching with organic acids is an environmentally friendly alternative to traditional extraction methods. Our previous study demonstrated that batch ultrasound-assisted organic acid leaching of REEs can significantly decrease environmental impacts compared to traditional bioleaching. The batch method is limited to small volumes and is unsuitable for industrial implementation. This study proposes a novel approach to increase reaction volume using a continuous ultrasound-assisted organic acid leaching method. Laboratory experiments showed that continuous ultrasound-assisted leaching increased the leaching rate (µg/h) 11.3–24.5 times compared to our previously reported batch method. Techno-economic analysis estimates the cost of the continuous approach using commercially purchased organic acids is $\$$9465/kg of extracted REEs and $\$$4325/kg of extracted REEs, using gluconic acid and citric acid, respectively. The sensitivity analysis reveals that substituting commercially purchased organic acids with microbially produced biolixiviant can reduce the process cost by approximately 99% while minimally increasing energy consumption. Environmental assessment shows that most of the emissions stemmed from the energy required to power the ultrasound reactor. We concluded that increased leaching capacity using a continuous ultrasound-assisted approach is feasible, but process modifications are needed to reduce the environmental impact.

54 - ENVIRONMENTAL SCIENCES/GLOBAL CLIMATE CHANGE ↗

Leaching of CEM III paste by demineralised or mineralised water at pH 7 in relation with aluminium release in drinking water network

Drinking water pipes can be lined with a cement matrix based on CEM III, which can release aluminium into the water. However, the European Union limits the aluminium concentration in drinking water for public health reasons. In order to study the long-term leaching mechanism of aluminium, semi-dynamic leaching tests using an aggressive solution (demineralised water) or drinking water (mineralised water) were conducted on crushed CEM III pastes maintained at pH 7. They resulted in a very high leaching coefficient, approaching 50%. However, in spite of this strong leaching, the amount of Al leached remained very low, at less than 1.5% of the initial amount of Al in the material. Under these conditions, the leaching of Al from a CEM III paste is complex since it involves several steps, where slag (1st and last steps) or cement paste (2nd step) are the main contributors.

36 MATERIALS SCIENCE↗

Impact of carbonation on leaching of constituents from a cementitious waste form for treatment of low activity waste at the DOE Hanford site

Carbonation can be a major aging process during disposal of alkaline cementitious waste forms and can impact constituent leaching by changes in material alkalinity, pore structure, and controlling mineral phases. The effect of carbonation on the leaching of major and trace constituents from Cast Stone, a cementitious waste form developed to treat high salt content low activity waste, was studied through a combination of leaching experiments and reactive transport simulations. Diffusive transport of constituents in the waste form was evaluated using reactive transport modeling of diffusion-controlled leaching test results and a geochemical speciation model derived from pH-dependent leaching. Comparisons between Cast Stone materials aged under nitrogen, air, and 2% carbon dioxide in nitrogen showed that carbonation impacts solubility, physical retention and observed diffusivity of major and trace constituents. Carbonation under 2% CO 2 decreased the diffusion-controlled leaching of chromium by two orders of magnitude. Finally, modeling results suggest that carbonation may also decrease solubility of technetium while changes to microstructure by carbonation increases effective diffusivity of constituents in Cast Stone.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Lattice site–dependent metal leaching in perovskites toward a honeycomb-like water oxidation catalyst

Metal leaching during water oxidation has been typically observed in conjunction with surface reconstruction on perovskite oxide catalysts, but the role of metal leaching at each geometric site has not been distinguished. Here, we manipulate the occurrence and process of surface reconstruction in two model ABO 3 perovskites, i.e., SrSc 0.5 Ir 0.5 O 3 and SrCo 0.5 Ir 0.5 O 3 , which allow us to evaluate the structure and activity evolution step by step. The occurrence and order of leaching of Sr (A-site) and Sc/Co (B-site) were controlled by tailoring the thermodynamic stability of B-site. Sr leaching from A-site mainly generates more electrochemical surface area for the reaction, and additional leaching of Sc/Co from B-site triggers the formation of a honeycomb-like IrO x H y phase with a notable increase in intrinsic activity. A thorough surface reconstruction with dual-site metal leaching induces an activity improvement by approximately two orders of magnitude, which makes the reconstructed SrCo 0.5 Ir 0.5 O 3 among the best for water oxidation in acid.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Strategic Petroleum Reserve Cavern Leaching Monitoring CY22

The U.S. Strategic Petroleum Reserve (SPR) is a crude oil storage system administered by the U.S. Department of Energy. SPR injected a total of over 230 MMB of raw water into 48 caverns as part of oil sales in CY22. Leaching effects were monitored in these caverns to understand how the sales operations may impact the long-term integrity of the caverns. The leaching effects were modeled here using the Sandia Solution Mining Code, SANSMIC. The modeling results indicate that leaching-induced features do not raise concern for the majority of the caverns. In addition to 12 caverns identified in previous leaching reports, seven caverns have been identified for further monitoring based on the results of this report. Twenty-two caverns had pre- and post-leach sonars that were compared with SANSMIC results. Overall, SANSMIC was able to capture the leaching well.

02 PETROLEUM↗

Sister Rod Destructive Examinations (FY23): Appendix J: Leaching of High Burnup Used Nuclear Fuel in Deionized Water

The leaching experiment aims to understand the trends in the radiolysis-enhanced dissolution of HBU SNF when exposed to water (e.g., in-reactor or in-pool cladding failures). Specimens from a baseline M5-clad rod and a heat-treated M5 rod were cut from the fractured CIRFT specimens and placed in 100 mL deionized water for a period of 128 days. Both radial and axial sections were cut to provide different surface areas of fuel in contact with the leachate. During the four-month exposure period, aliquot samples of the leachate were analyzed using gamma spectroscopy and inductively coupled plasma - mass spectrometry (ICP-MS). The analysis quantified the amount of fuel leached into the solutions and provided individual isotopic release fractions (of 30+ isotopes) which were compared as a function of time and surface area of the fuel exposed. Consistent with existing literature, the leaching followed a trend in which isotopes of certain elements such as Cs and Mo were among the first species in the matrix to dissolve, and with the highest release rates. This was followed by a gradual matrix dissolution consisting of uranium and other actinides and a slower-than-matrix release from some isotopes, including Ru and Rh. It was also observed that the circumferential samples having less exposed fuel surface area (to begin with) leached more than the axial samples for a majority of the isotopes during the timespan of the study. Previous experiments were conducted by decladding or exposing the pellet-clad surface completely, but the samples used in this study retained the cladding. One possible explanation for the higher leaching rate of the circumferential samples is that the pellet-clad interface, which has a greater density of grain boundaries and defects, may be the most vulnerable area to leaching of fuel in the presence of water.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Selective leaching and solvent extraction of Lithium from spent batteries

Pre-extracting Li from spent lithium-ion batteries (LIBs) is crucial because the recovery efficiency of Li is low after other critical metals have been extracted. Traditional methods involving black mass roasting followed by water leaching have resulted in the extraction of 76 % Li and 61 % Al. However, pre-leaching Li from pretreated black mass using an oxalic acid solution at both ambient and elevated temperatures significantly improved results, achieving 98.1 % Li, 99.5 % Al, and 100 % Fe extraction while leaving Ni, Co, Mn, and Cu behind under optimal conditions. Oxalic acid crystals were recovered by refrigerating the leach solution at temperatures below 5 °C and were reused with nearly identical leaching efficiency. Selective extraction of Li from the oxalate leach solution was achieved using Cyanex® 936P under optimal conditions. Here, due to its extremely low Li extraction efficiency, Dichloromethane proved unsuitable as a diluent. Comparative extraction tests using Cyanex® 936P, Cyanex® 272, and DEHPA in kerosene demonstrated that Cyanex® 936P is an excellent extractant for Li, effectively separating it from other impurities. Under optimal conditions, 98.8 % of available Li was extracted using 20 % Cyanex® 936P, compared to 51.1 % with Cyanex® 272 and 39.9 % with DEHPA in kerosene. Additionally, stripping Li from Cyanex® 936P using H 2 SO 4 and HCl was explored, with HCl yielding the best performance.

Black mass↗

Electrochemical deposition of amorphous aluminum oxides on lead pipes to prevent lead leaching into the drinking water

Over 5000 public drinking water systems in the US are out of compliance with the Lead and Copper Rule. Lead leaching from lead pipes is limited by the solubility of a naturally occurring scale. Changes in water quality may cause this scale to become more soluble, releasing lead into the drinking water. We propose a novel electrochemical method to prevent lead leaching from lead pipes. In this method, an aluminum wire and an alkaline phosphate electrolyte are inserted into the pipes. The pipes are then anodized for 2 h by using an external power supply, resulting in the electrodeposition of an insoluble aluminum oxide layer on top of the preexisting scale. This technology was tested on lead pipes from the EBMUD water distribution systems located in Berkeley, CA, using recirculating synthetic and actual tap water for 120 days. The untreated pipes leached an average of 23 ppb and 38 ppb of lead respectively, when using free chlorine and monochloramine as disinfection residuals. In contrast, the treated pipes leached 3 ppb and 5 ppb respectively. These results suggest that the proposed treatment has the potential to prevent lead leaching regardless of the disinfection residual and thus should be further explored in a field trial.

36 MATERIALS SCIENCE↗

Phosphorus availability and leaching losses in annual and perennial cropping systems in an upper US Midwest landscape

Abstract Excessive phosphorus (P) applications to croplands can contribute to eutrophication of surface waters through surface runoff and subsurface (leaching) losses. We analyzed leaching losses of total dissolved P (TDP) from no-till corn, hybrid poplar ( Populus nigra X P. maximowiczii ), switchgrass ( Panicum virgatum ), miscanthus ( Miscanthus giganteus ), native grasses, and restored prairie, all planted in 2008 on former cropland in Michigan, USA. All crops except corn (13 kg P ha −1 year −1 ) were grown without P fertilization. Biomass was harvested at the end of each growing season except for poplar. Soil water at 1.2 m depth was sampled weekly to biweekly for TDP determination during March–November 2009–2016 using tension lysimeters. Soil test P (0–25 cm depth) was measured every autumn. Soil water TDP concentrations were usually below levels where eutrophication of surface waters is frequently observed (> 0.02 mg L −1 ) but often higher than in deep groundwater or nearby streams and lakes. Rates of P leaching, estimated from measured concentrations and modeled drainage, did not differ statistically among cropping systems across years; 7-year cropping system means ranged from 0.035 to 0.072 kg P ha −1 year −1 with large interannual variation. Leached P was positively related to STP, which decreased over the 7 years in all systems. These results indicate that both P-fertilized and unfertilized cropping systems may leach legacy P from past cropland management.

54 ENVIRONMENTAL SCIENCES↗

Bipartisan Infrastructure Law (BIL) – Illinois Rare Earth Novel Extraction and Supply (IRENES) - Report on Technology Down Select No. 1 - Acid Baking vs. Heap Leaching

An essential step for recovering rare earth and critical minerals from coal mine waste is one that achieves adequate dissolution of the target elements into a pregnant leachate solution. The simplest technical approach was thought to be heap-leaching that could proceed using mild acid dosing or naturally generated acid from biological activity. For this reason, the University of Kentucky at Lexington (UKY) undertook two efforts to evaluate feasibility, including a laboratory column leaching evaluation and a pilot heap-leaching demonstration. Later, the UK evaluated a pyrometallurgical approach using roasting combined with acid baking and tank leaching at elevated temperatures to improve extraction efficiencies. This report surveys the previously reported leaching yields and calculates the gross value of rare earth oxides as a basket in the pregnant leachate solution.

01 COAL, LIGNITE, AND PEAT↗

Pilot Scale Testing of Lignite Adsorption Capability and the Benefits for the Recovery of Rare Earth Elements from Dilute Leach Solutions

Naturally occurring organic materials containing humic acids show a strong affinity towards rare earth elements (REE) and other critical elements. Leaching experiments on lignite coal waste produced from construction sand production revealed that the contained REEs were associated with the organic matter. Furthermore, adsorption studies revealed that the lignite waste was capable of extracting REEs from a model solution and increased the REE content of the lignite waste by more than 100%. As such, this study aimed to utilize the lignite waste to adsorb REEs from pregnant leach solutions and acid mine drainage sources having low REE concentrations and subsequently leach the lignite material to produce pregnant leach solutions containing relatively high amounts of REEs, which benefits the performance and economic viability of downstream separation and purification processes. An integrated flowsheet was developed based on this concept and tested at a pilot scale. The pregnant leachate solution (PLS) was generated from a heap leach pad containing 2000 tons of Baker seam coarse refuse. The pilot scale circuit was comprised of aluminum precipitation, adsorption using the waste lignite, and rare earth-critical metal (RE-CM) precipitation stages in succession. The results indicated that the aluminum precipitation stage removed over 88% and 99% of the Al and Fe, respectively. The adsorption stage increased the REE content associated with the waste lignite from 457 ppm to 1065 ppm on a whole mass basis. Furthermore, the heavy REE (HREE) content in the feedstock increased by approximately 250%, which raised the percentage of HREE in the REE distribution by 19 absolute percentage points. In addition to the REEs, concentrations of other critical elements such as Mn, Ni, and Zn also improved by 75%, 37%, and 250%, respectively. Bench-scale tests revealed that increasing the solids concentration in the waste lignite and PLS mix from 1% to 20% by weight enhanced the adsorption efficiency from 32.0% to 99.5%, respectively. As such, a new flowsheet was proposed which provides significantly higher REE concentrations in the PLS that can be fed directly to solvent extraction and/or oxalic acid precipitation and, thereby, enhancing process efficiency and economics.

58 GEOSCIENCES↗

Ammonium sulfate leaching of NaOH-treated monazite

Rare earth elements (REEs) can be extracted from monazite under aggressive decomposition and leaching conditions. Much of the waste rocks are removed prior to the extraction process to minimize the costs and waste generation, which is difficult with coal byproducts. The possibility of extracting REEs from low-grade monazite concentrates under relatively mild conditions has been explored to simulate the extraction of REEs from coal byproducts. It has been found that monazite can be decomposed in 10 to 50 % NaOH solutions at 80 °C, with the resulting hydrous oxide being subjected to the ammonium sulfate leaching at pH 4. Further, the ς-potential measurements conducted in the presence of the lixiviant suggest that the NH 4+ ions displace the hydrated Ln 3+ ions from the surface of Ln(OH) 3 (s) by an ion-exchange mechanism, which may be driven by the large differences in the hydration enthalpies between the charged species involved. This approach may be advantageous over acid leaching, including the regeneration of spent lixiviant, lower chemical consumption, and leaching at higher pH.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Gas-solid reaction-based selective lithium leaching strategy for efficient LiFePO 4 recycling

As the electric-vehicle market continues to expand, LiFePO 4 (LFP) batteries, valued for their intrinsic safety and cost-effectiveness, are being increasingly utilized. However, this widespread adoption highlights the urgent need for innovative and environmentally friendly recycling methods for spent LFP batteries due to their relatively low material value and the environmental challenges associated with traditional recycling processes. Here, in this study, we present a novel selective lithium leaching technique that involves a gas–solid reaction with chlorine gas. This method achieves a remarkable leaching efficiency of 99.8 % and a selectivity of 98.8 % at 200 °C within just 10 min, without generating acidic wastewater. The resulting LiCl solution was successfully converted into Li 2 CO 3 with an excellent purity of 99.5 %, while producing NaCl solution as the only byproduct. Notably, the olivine structure of the LFP was preserved as FePO 4 after lithium leaching. The regenerated LFP demonstrated excellent performance, retaining 94.1 % of its capacity after 150 cycles, while the lithium-leached FePO 4 delivered a reversible capacity exceeding 150 mAh/g. This approach not only enhances the efficiency of LFP recycling but also paves the way for more sustainable battery technologies.

36 MATERIALS SCIENCE↗

Electrochemical leaching of spent LIBs: Kinetics, novel reactor, and modeling

The use of electrons as main reagent for the recovery and recycling of critical metals from spent lithium-ion batteries (LIBs) is a process electrification strategy that can be used to close the life-cycle loop of LIBs through more sustainable methods. Electrochemical leaching, a process that uses a reductant that is constantly regenerated electrochemically for the leaching of lithium-ion battery black mass (LIBBM), has shown high extraction efficiencies and sustainable scores. However, slow kinetics, reactor design challenges and lack of deeper understanding of the underlying processes are barriers to the optimization, scale-up, and market adoption of this technology. In this paper, a kinetic study and mathematical model for dissolving LIBBM is presented to better understand the underlying mechanisms aiming to reduce the processing time and make predictions for future design and scale-up. The effect of acid and electrochemically mediated reductant concentrations, LIBBM loading, and cathode/reactor designs were explored. As a result, the leaching time was reduced from 7h to under 1h at a pulp density of 73 g/L, without external heating. A novel reactor with parallel baffle electrodes (PBE) was developed, which significantly reduced the leaching time by improving convection in a stirred slurry electrochemical reactor. Dimensionless numbers were deduced from an unsteady state model, which can be used in dimensional analysis for future process design and scale-up.

25 ENERGY STORAGE↗

Functional Predictor Variables for the Leaching Potential of Arsenic and Selenium from Coal Fly Ash

The release of leachates from intact coal ash impoundments is a concern due to the enrichment and mobilization of toxic elements such as arsenic (As) and selenium (Se). This study aims to explore the intrinsic properties of coal fly ash that correlate with the relative leachability of As and Se. We performed leaching experiments with 52 fly ash samples collected from 15 different U.S. power plants and representing coal feedstocks from the three major domestic regions. We assessed the mobilization potential of As and Se in fly ash based on standardized leaching protocols and performed multivariate and lasso regression analyses to explore correlations of leachable As and Se contents with characteristics such as major element contents, loss on ignition, and pH. The results of regression models indicated that major elements (Fe, Ca, and Al) for a wide range of fly ashes can serve as predictor variables for the leaching potential of As but not for Se. LOI and pH were not important predictive variables in the models. Both regression approaches resulted in relatively strong fits for leachable As (correlation coefficient R 2 = 0.78 for both models) compared to models for leachable Se (R 2 = 0.49). Overall, these results suggest that correlation models combined with on-site elemental analysis with portable analyzers may enable a screening method for leachable As in coal ash.

01 COAL, LIGNITE, AND PEAT↗

Process design for recovering rare-earth elements from mine tailings with low rare-earth concentrations via sequential leaching and solvent extraction

Rare earth elements (REEs) are essential for advanced technologies and yet face significant supply chain risks due to their concentrated global production and limited domestic availability. Addressing this challenge requires efficient processes capable of upgrading low-grade secondary resources such as mine tailings. In this study, we developed a novel separation flowsheet that integrates sequential leaching and 2-stage solvent extraction (SX) processes to recover high-purity heavy REEs (HREEs) and light REEs (LREEs) from a simulated mine-tailing concentrate containing 2.4 wt% total REEs (TREEs; 0.6 wt% LREEs and 1.8 wt% HREEs). Sequential leaching with controlled pH adjustment selectively precipitated REEs while retaining the large amount of impurities in the solution, producing an REE-enriched leachate by following leaching processes with roughly twice the REE concentration and half the impurity concentration compared to that of single-step leaching. The optimized SX flowsheet employed Cyanex 572 to extract HREEs and Fe over LREEs, followed by Fe removal using tributyl phosphate (TBP), while the raffinate stream was processed by SX with di(2-ethylhexyl)phosphoric acid (D2EHPA) to recover LREEs under optimized conditions balancing both extraction efficiency and purity. Although increased extractant availability in the organic phase improved LREE recovery, it also increased co-extraction of Ca, underscoring trade-offs in process optimization. Both HREE- and LREE-rich solutions were subsequently precipitated into solid products via oxalate precipitation, resulting in high-purity REE solids containing ∼92.0 wt% HREEs (∼95.7 wt% TREEs) and ∼92.8 wt% LREEs (∼94.0 wt% TREEs). In conclusion, this proof-of-concept study using simulated mine tailings demonstrates a promising approach for upgrading low-grade REE resources, while highlighting the need for future validation with real materials.

Mine tailings↗

Innovative recycling of high purity silver from silicon solar cells by acid leaching and ultrasonication

Precious and scarce silver (Ag) is used as a front electrical contact in silicon solar panels. With massive amounts of solar panel waste coming to end-of-life, it is imperative to recover all the Ag from these modules. In this paper, we propose a novel method to easily reclaim Ag from end-of-life silicon solar cells using low concentration sulfuric acid (H 2 SO 4 ) leaching followed by ultrasonication. Our process simplifies the Ag recycling procedure by directly recovering the Ag contacts from solar cells, eliminating the need for secondary precipitation/electrodeposition. First, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) was used to study the leaching and ultrasonication process on rejected solar wafers. Next, a solar panel from landfill was heated in a furnace to burn off the polymer encapsulant. The silicon wafers were then collected from the burning process and leached in 2 M H 2 SO 4 at two different shaking speeds for 48 hours at room temperature. Finally, the end-of-life silicon wafer pieces were collected, sonicated in water, and then the sonication water was centrifuged to show a proof-of-concept to recover the Ag contacts. Inductively coupled plasma optical emission spectroscopy (ICPOES) is used to monitor dissolved elements in the leachate as a function of time and shaking speed. XPS is used to evaluate the composition of the silicon cell wafer surface before and after H 2 SO 4 leaching. SEM is used to image the recovered Ag contacts morphology and EDX confirms the recovered particles contain high amounts of Ag. Furthermore, a proposed schematic illustrates the authors’ hypothesis for the peeling mechanism.

14 SOLAR ENERGY↗

Tank 50 Simulant Grout and Toxicity Characteristic Leaching Procedure (TCLP) Results for Methyl Mercury Waste Acceptance Criteria (WAC) Limit

Testing of simulated Tank 50 salt solution grout, spiked with methyl mercury (MeHg) and ionic mercury, used the Toxicity Characteristic Leaching Procedure (TCLP) to evaluate leaching performance with respect to Hg and the Waste Acceptance Criteria (WAC) limits for the Saltstone Production Facility (SPF). This report describes the test parameters for simulant preparation and confirmatory analysis, grout preparation, TCLP leach testing and subsequent leachate analyses. These scoping tests were designed to provide an initial evaluation of the effect of increased MeHg and ionic Hg on the TCLP and were requested by Savannah River Remediation LLC (SRR) through a Technical Assistance Request (TAR). It is expected that this preliminary testing will likely lead to future, more detailed, testing involving the mercury (Hg) WAC and Hg limits with respect to the Tank 50 TCLP for mercury. The TCLP concentrations for total Hg have approached 0.06 mg/L in recent years for Tank 50 radioactive solutions containing up to 105 mg/L of Hg in the form of ionic (Hg(I/II), elemental (Hg(0)) and organo-mercury such as MeHg. In discussions with SRR personnel, it was decided for this non-baseline work to target Hg spike concentrations, using predominately MeHg, in the range of 150 to 350 mg/L total Hg to investigate corresponding Hg TCLP leaching behaviors.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗