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DOE OSTI2023

Development of a Multi Sensor Data Science System for Monitoring a Solvent Extraction Process

Idaho National Laboratory is designing and constructing a solvent extraction test bed, Beartooth, as part of a nuclear fuel cycle stewardship initiative. The test bed will provide facilities and equipment for testing novel extraction processes and give early career scientists opportunities to gain skills in performing separations chemistry. The test bed is being uniquely designed to enable machine learning capabilities for the characterization of chemical process operations. One of the intentions of incorporating machine learning methods is to provide process operators with enhanced situational awareness for the optimization of separations techniques and possible detection of a diversion event. As a result, the objective of this Laboratory Directed Research and Development project is to develop a multi-sensor data collections system and implement machine learning techniques on signals from an existing centrifugal contactor cascade to identify equipment usage and process events. This presentation will provide an overview of sensors used and experiments conducted to date.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1982

Improved Supercritical-Solvent Extraction of Coal

Raw coal upgraded by supercritical-solvent extraction system that uses two materials instead of one. System achieved extraction yields of 20 to 49 weight percent. Single-solvent yields are about 25 weight percent. Experimental results show extraction yields may be timedependent. Observed decreases in weight of coal agreed well with increases in ash content of residue.

Compton, L.↗

DOE OSTI2022

An Overview in the Development of a Multi-Sensor Data Science System for Monitoring a Solvent Extraction Process

To enhance nuclear nonproliferation stewardship, Idaho National Laboratory is building the Beartooth nuclear fuel cycle processing test bed. The Beartooth test bed will allow researchers the opportunity to study nuclear fuel processing operations including the use of centrifugal contactors in solvent extraction processes. The test bed is designed to support data collection and machine learning to monitor process operations. As part of this project, researchers will study data collected from a host of sensors that have not been typically used to monitor solvent extraction processes such as vibration, acoustic, colormetric, and thermal measurement data. The goal of this research is to employ machine learning and data analytics to study the confluence of signals collected from both traditionally and non-traditionally used sensors to provide operator process awareness and discover process anomalies. An overview of planned sensors and experiments that will focus on signal discovery will be presented.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

An Overview in the Development of a Multi-Sensor Data Science System for Monitoring a Solvent Extraction Process

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Membrane-based solvent extraction for the recovery of rare earths from phosphate mining process streams

This study reports on the capture of rare earth elements (REEs) from phosphate industry process streams, including phosphoric acid (PA) sludge and phosphogypsum (PG), using a membrane solvent extraction (MSX) process. While MSX has been proven effective for a relatively concentrated feed, its effectiveness for dilute REEs solutions remains unexplored. Investigated PA-sludge and PG particles contain total REEs concentrations of ∼1100 and ∼320 ppm, respectively. Acid leaching, implemented to dissolve the REEs, significantly dilutes the REEs concentration to ∼210 ppm for PA-sludge leachate and ∼60 ppm for PG leachate. These low concentrations, compounded by the higher levels of non-REE ions and radioactive species, uranium (U) and thorium (Th), poses challenges to the MSX process. Here, we demonstrated that N,N,N′,N′-tetraoctyl-diglycolamide (TODGA) selectively binds REEs from a >3 M nitric-acid leachate while effectively rejecting U and Th. Concentrations of light REEs in strip solution were doubled compared to the feed, while heavy REEs were preferentially extracted. Furthermore, >99% purity gypsum, free of U and Th, was precipitated during the acid leaching process, aiding separation by removing significant amounts of non-REEs species (e.g., calcium) prior to the MSX process. Molecular simulations support the experimental data, suggesting preferential separation of heavy over light REEs. Based on these results, a cost-effective integrated process including pretreatment, acid leaching, MSX, and wastewater treatment is proposed for the co-recovery of REEs, phosphoric acid, gypsum, and U. This study shows MSX as a technically and economically feasible process for the recovery of REEs from low-concentration process streams, offering advantages over conventional solvent extraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Color Sensor Comparison for Solvent Extraction Processes

Idaho National Laboratory is building Beartooth, a test bed to advance research into nuclear fuel cycle reprocessing. This test bed will give researchers the opportunity to study solvent extraction processes. Beartooth extraction operations will include the use of centrifugal contactors designed for the recovery and purification of special nuclear material from spent fuel. This new test bed facility provides researchers with the opportunity to study innovative technologies. As part of that initiative, this project will integrate non-traditional (atypical to a solvent extraction process) measurement sensors into a system of contactors to determine the state-of-health. These non-traditional sensors have the potential to enhance nuclear safeguarding efforts and other process activities. The non-traditional sensors include accelerometers, acoustic microphones, colorimetric, pH, conductivity, viscosity, density, and infrared cameras. This report documents the testing and evaluation of two different colorimetric RGB sensors.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

An Explainable Classification Framework for Determining and Understanding the Suitability of Solvent Extraction for Bioproduct Recovery

Lignocellulosic biomass is an abundant feedstock for producing sustainable fuels and chemicals. However, a key challenge in most biomass utilization strategies is the recovery of products from a dilute, typically aqueous, phase. In this respect, liquid–liquid extraction, which relies on a solvent to transfer a product of interest from one liquid phase to another (solvent-rich) phase, is a technology that can reduce the energy requirements for product recovery. To reduce solvent consumption, liquid–liquid extraction needs to be combined with another separation method (e.g., distillation) to recycle the solvent. Despite the research on solvent extraction, there are limited system-wide methods that allow us to determine when extraction is well suited to carry out a specific separation. Accordingly, we present a classification framework to predict whether extraction, coupled with distillation, is feasible and more economical than distillation. Our framework is based on features such as feed composition, liquid–liquid equilibrium constants, relative volatilities, and solvent price, and leads to trained classifiers that show good prediction accuracy. We further study how specific features influence the suitability of extraction. Furthermore, to showcase the applicability of the framework, we use it to analyze the separation of acetic acid from water.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1982

Carbon, hydrogen and nitrogen isotopes in solvent-extractable organic matter from carbonaceous chondrites

CCl4 and CH3OH solvent extractions were performed on the Murray, Murchison, Orgueil and Renazzo carbonaceous chondrites. Delta-D values of +300-+500% are found in the case of the CH3OH-soluble organic matter. The combined C, H and N isotope data makes it unlikely that the CH3OH-soluble components are derivable from, or simply related to, the insoluble organic polymer found in the same meteorites. A relation between the event that formed hydrous minerals in CI1 and CM2 meteorites and the introduction of water- and methanol-soluble organic compounds is suggested. Organic matter soluble in CCl4 has no N, and delta-C-13 values are lower than for CH3OH-soluble phases. It is concluded that there either are large isotopic fractionations for carbon and hydrogen between different soluble organic phases, or the less polar components are partially of terrestrial origin.

Becker, R. H.↗

DOE OSTI2023

Recovery of critical elements from end-of-life lithium ion batteries with supported membrane solvent extraction

Single-stage and multi-stage systems and methods for the recovery of critical elements in substantially pure form from lithium ion batteries are provided. The systems and methods include supported membrane solvent extraction using an immobilized organic phase within the pores of permeable hollow fibers. The permeable hollow fibers are contacted by a feed solution on one side, and a strip solution on another side, to provide the simultaneous extraction and stripping of elements from dissolved lithium ion cathode materials, while rejecting other elements from the feed solution. The single- and multi-stage systems and methods can selectively recover cobalt, manganese, nickel, lithium, aluminum and other elements from spent battery cathodes and are not limited by equilibrium constraints as compared to traditional solvent extraction processes.

Bhave, Ramesh R.↗

DOE OSTI2022

Flowsheet Design for the Purification of Mo-99 and Uranium Target Recovery by Solvent Extraction

New production and purification methods are sought to meet the increasing demand of 99 Mo but without the use of highly enriched uranium (HEU). To this end, larger quantities of low-enriched uranium (LEU) or even natural uranium (NU) are being leveraged to maintain high production capacities of 99 Mo. Solvent extraction is widely used to treat bulk quantities of uranium and to separate out trace quantities of fission products. This report describes the calculation of AMUSE-generated flowsheets to process irradiated uranium targets to recover 99 Mo by solvent extraction. Flowsheets are presented and discussed along with a number of advantages and disadvantages.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Preliminary Results of a Multi-Sensor Data Science System for Monitoring a Solvent Extraction Process

Idaho National Laboratory is building a test bed to allow researchers the opportunity to study nuclear fuel processing operations. This includes studying the solvent extraction process and the use of centrifugal contactors. The goal of this project is to develop a system that utilizes non-traditional measurement sources such as vibration, acoustics, current, color, flow, and temperature in conjunction with data-based, machine learning techniques that will allow for signal discovery. This multi-sensor data supports the development of safeguards by design, provides operator process awareness, and aids in the discovery of process anomalies. This paper highlights some of the preliminary results from initial data collection campaigns and shares some of the lessons learned.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2022

Process Scale-Up of an Energy-Efficient Membrane Solvent Extraction Process for Rare Earth Recycling from Electronic Wastes

This study reports the process scale-up and long-term performance of an energy-efficient and cost-effective membrane solvent extraction (MSX) process for separation and recovery of high purity rare earth oxides (REOs) from scrap permanent magnets (SPMs). Here, the rare earth elements (REEs), including dysprosium, neodymium, and praseodymium, are recovered from SPMs using a neutral extractant, tetraoctyl diglycolamide (TODGA) embedded in a microporous polypropylene hollow fiber membrane module. The MSX process performance is demonstrated with bench scale module with membrane surface area of 1.4 m 2 to industrial scale modules with membrane surface area of up to 20 m2 to enable the processing of up to 1 ton month –1 of SPMs. The purity and the yield of the recovered REOs are >99.5 wt% and >95%, respectively. The average extraction rate of REOs is >10 g m –2 hr –1 . A skid of MSX system is assembled with a membrane area of 40 m 2 . The MSX skid successfully recovers REOs with a capacity of 300 kg REOs/month. Finally, it is determined that the organic phase containing the extractant maintains its performance up to 250 h. The results suggest that the MSX process is an economically viable and environmentally friendly process for separation and recovery of REOs from electronic wastes.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Data Challenges in Multi-Sensor Data Science System for Monitoring a Solvent Extraction Process

Idaho National Laboratory (INL) is maintaining and gaining knowledge into the nuclear fuel cycle by building a test bed to allow researchers the opportunity to study nuclear fuel processing operations. This includes studying solvent extraction processes that use centrifugal contactors. As part of INL’s mission, the goal of this project is to develop a system that utilizes non-traditional measurement sources such as vibration, acoustics, current, light, flow, and temperature in conjunction with data-based, machine learning techniques that will allow for signal discovery. This multisensory data can support the development of safeguards by design, provide operator process awareness, and discover process anomalies. This poster will highlight some of the data collection and analytics challenges for the multi-sensor system as well as the mitigation strategies to build a robust system. Additionally, some preliminary data from the first testing campaign will be shown to help illustrate the data needs of the system.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2026

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↗

DOE OSTI2023

Use of Sensors and Machine Learning for Signal Discovery in a Solvent Extraction Process – 23280

Reprocessing is an important step in the nuclear fuel cycle where usable nuclear materials are extracted from spent fuel for recycling. The extraction of materials for reuse simultaneously reduces not only the volume of nuclear waste, but its decay time to radioactivity levels similar to that of the originating uranium ore. As part of an initiative to steward research, development, and innovation into the nuclear fuel cycle, Idaho National Laboratory is designing and constructing a solvent extraction testbed named Beartooth. Beartooth will allow researchers to refine extraction processes, test innovative extraction processes, and give early career scientists opportunities to gain skills in performing separations chemistry that uses centrifugal contactors. In addition, the Beartooth testbed is being uniquely designed to enable novel technologies including machine learning capabilities for the characterization of chemical process operations in near real-time. To aid in the design of Beartooth, a team of researchers are installing a variety of atypical sensors into a system of contactors for signal discovery. The team will implement machine learning methods on sensor data to determine signal features with the goal of providing a process operator with a deeper understanding of the chemical process and equipment usage. This work will summarize sensors utilized and preliminary results from an infrared camera.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Use of Sensors and Machine Learning for Signal Discovery in a Solvent Extraction Process

Reprocessing is an important step in the nuclear fuel cycle where usable nuclear materials are extracted from used fuel for recycling. The separation of materials for reuse simultaneously reduces not only the volume of nuclear waste, but its decay time to radioactivity levels similar to that of the originating uranium ore. As part of an initiative to steward research, development, and innovation into the nuclear fuel cycle, Idaho National Laboratory is designing and constructing a solvent extraction testbed named Beartooth. This testbed will allow researchers to refine separation processes, test innovative extraction processes, and give early career scientists opportunities to gain skills in performing separations chemistry utilizing centrifugal contactors. In addition, the Beartooth testbed is being uniquely designed to enable novel technologies including machine learning capabilities for the characterization of chemical process operations in near real-time. To aid in the design of Beartooth, a team of researchers are installing a variety of atypical sensors into a system of contactors for signal discovery. The team will implement machine learning methods on acquired sensor data to extract signal features. The goal is to provide a process operator with a deeper understanding of the chemical process and equipment usage. This work will summarize sensors utilized and preliminary results from an infrared camera.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Rapid Sensing to Facilitate Purification of Rare Earth Element-Containing Process Streams Produced Through Membrane-Assisted Solvent Extraction

The development of an economically competitive domestic supply of rare earth elements and yttrium (REY) is necessary for our nation’s economic growth and national security. The achievement of a secure domestic supply of REY requires not only the development of effective processes for recovery of REY from naturally occurring materials and/or recycled products, but also the development of downstream processes for the ultimate production of high-REY content solids. An impediment to the development of such processes is the scarcity of analytical methods that provide rapid determination of the process stream compositions. In this work, a membrane-based extraction process was used to selectively recover REYs from a dilute solution in the presence of much higher concentrations of Ca and Al. In tandem, the use of a portable spectrometer equipped with an immobilized zinc adeninate benzene tricarboxylate metal-organic framework sensing material makes possible the rapid detection of the presence of ppm concentrations of Tb and Eu in both weakly acidic and strongly acidic process streams within minutes. A solvent extraction processing time of 15-60 min maximized REY selectivity over gangue ions while achieving up to 80% REY and minimal gangue ion recovery. Taken together, these experiments highlight not only an innovative method for REY purification but also the importance of inexpensive, portable characterization methods for near real-time analysis of REY content.

Membrane-assisted solvent extraction↗

DOE OSTI2024

Large-scale atomistic model construction of subbituminous and bituminous coals for solvent extraction simulations with reactive molecular dynamics

Large-scale atomistic models for complex polycyclic aromatic hydrocarbon systems help understand the chemical properties and behaviors of complex feedstocks such as coal or petroleum. However, the development and utilization of large-scale models remain limited due to the difficulty in achieving the varied structural characteristics necessary to capture stochastic nature of these feedstocks. Here we demonstrate a systematic workflow to construct stochastic molecular systems from a broad analytical suite: high-resolution transmission electron microscopy (HRTEM), carbon-13 nuclear magnetic resonance spectroscopy ( 13 C NMR), laser desorption ionization mass spectroscopy (LDI-MS), and elemental analysis. We present a model construction and analysis utility of a new Python-based module. We selected one subbituminous and three high-volatile bituminous coals to construct large-scale models (~40,000 atoms). The constructed models were utilized to examine the affinity for solvent extraction (naphthalene or tetralin) and the effect of structural properties (e.g., aromatic cluster size, functional groups, and cross-linking) in reactive molecular dynamics simulations. Complex chemical reactions were monitored with bond order transitions, intermediates formation, and mass distributions. Reactive molecular dynamics simulations suggest a plausible chemical extraction process and products for the complex fossil feedstocks. The results indicated that radical formations with bond breaking of bridging oxygens and carbons were required at high temperatures to facilitate hydrogeneration and extraction of gas molecules from radical-free molecules. We observed that aliphatic chains of tetralin were easily decomposed and combined with radicals to form small size of molecules with aryl bonding, mainly increasing molecules in the 500–1000 Da, while naphthalene had little impact on chemical extraction process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗