Track 2: 2024 Lithium-Battery Technology-Rare Earths Agenda

Thursday, 30 May

8:00 am Conference Registration & Arrival Tea

9:00 Conference Chairperson’s Opening Remarks

9:10 Sponsor’s Welcome

9:15 Keynote Presentation: Moving up The Value Chain from Mines to Batteries

Celina Mikolajczak, Chief Battery Technology Officer, Lyten (joining virtually)
Andrew Nissan, Senior Director of Battery Strategic Sourcing, Lyten

The presentation explores the critical role of innovation, sustainability, and strategic partnerships with mining companies into the production battery raw materials. The need for the mining industry to adopt advanced technologies and sustainable practices to meet the growing demand for battery materials driven by the expansion of global demand for electrification. This talk highlights successful case studies and industry best practices that demonstrate the potential for value creation along the entire supply chain. Overall, the presentation underscores the opportunities and challenges faced by the mining sector in moving up the value chain in partnership with the global battery industry.

9:55 Australian Leverage to Global Carbon Neutrality

Adrian Griffin, Principal, Future Technology Trust, Australia

The global ESG compliance push is affecting almost all businesses, and supply-chain emissions are doing the front running. Emission reductions inherent in the renewable energy sector are perceived as a climate-change savior; however, that sector relies on the minerals industry, which not only supplies it with raw-material inputs, but also leads the way in recycling end-of-life materials to maintain sustainability and minimise carbon footprints. Indeed, a vast range of critical minerals is required to maintain the very existence of renewable energy and the battery back-up necessary for storage and grid levelling. The battery industry, an insatiable consumer of minerals, is thus an integral part of the drive towards carbon neutrality and greening of the planet. Australia occupies a unique position in the supply chain being developed for carbon neutrality, since it is a significant source of many of the resources required—among them nickel, cobalt, manganese, lithium, and rare earths. That supply chain starts with exploration and mining to feed the downstream processing and manufacture of the materials being created to electrify the world, including domestic, industrial, and transport applications. But that’s not the end of the materials lifecycle; what happens to spent materials at the end of each product’s life must also be considered. Reducing carbon footprints involves more than examining ways of shipping nickel, cobalt, lithium, iron, and phosphorous to battery producers to fashion into storage devices, as indeed it takes more than the mining of rare earths to produce high-performance magnets, or the production of copper to expand power grids. Lifecycle optimisation must also extend into high-technology manufacturing areas. As the source of a large proportion of the world’s critical minerals, Australia has the greatest potential of any country to reduce carbon footprints by downstreaming its mineral products into things like refined metals, magnets, motors, wind turbines, battery chemicals, precursors, anode and cathode active materials, cells, and batteries. But if such downstream production is necessary, Australia cannot simply rest on its laurels and keep producing the same minerals it did before (including nickel for the production of ternary cells). Should it not instead backward-integrate from a product with superior lifecycle attributes and mine accordingly to produce that product? As Australia strives to adopt the best available technologies to supply precursors, cathode powders and, ultimately, batteries for renewable energy storage, lithium ferro phosphate (or LFP) is a case in point. For OEMs, advanced materials like LFP can provide previously unrecognised advantages in relation to reducing carbon emissions. Advanced metallurgical techniques currently being developed by Australian companies as part of ‘urban mining’—that is, the rebirthing of the critical materials in end-of-life products—provide further environmental benefits. One could say, then, that Australia has the ultimate leverage in terms of global decarbonisation.

10:20 Piloting the Neometals ELI Process

Mike Tamlin, Head of Lithium, Neometals, Australia

Considering the rapidly growing demand for lithium and the activity in the sector, the development of a lower-cost direct route to battery-grade lithium hydroxide monohydrate from a purified lithium chloride solution is long overdue. Over the past 7 years, Neometals has been developing the patented ELi process to achieve exactly this goal. Most recently, Neometals has been working with commercial laboratories and technology vendors to develop and demonstrate a flexible flowsheet for both spodumene and lithium chloride brine feeds that can effectively reduce key impurity levels, enabling direct electrolysis to produce a lithium hydroxide solution (avoiding much of the costs and inefficiencies of conventional routes). In support of an engineering cost study, Neometals has now completed bench and pilot-scale demonstration of the critical unit processes needed for purification of several lithium chloride brines and a lithium chloride solution derived from a Western Australia spodumene sample. The purification flowsheet involves sequential i) bulk impurity removal steps, and ii) impurity rejection/polishing steps to achieve levels of impurities, including the divalent cations (Mg2+, Ca2+, Sr2+), boron, silicon, and sulphate to sub-mg/L levels. Results from the purification and electrolysis steps will be presented in this paper and used to support the claimed relative economic advantages of this flowsheet compared to more conventional processing options.

10:45 Process Modelling and Life Cycle Assessment: Conventional and Novel Processing of Spodumene

Mike Dry, Owner, Arithmetek, Canada

Phoebe Whatoff, Minviro, UK

Lithium is considered a critical metal to enable the transition from a fossil fueled to an electric economy. It is estimated that lithium demand can grow up to 500% by 2050 compared to 2018 production. However, the cost of production will remain important, and it is critical that the increased production required for moving to an electric economy is not offset by an increase in adverse environmental impacts during raw material extraction. In this study, process modelling is combined with prospective LCA modelling, enabling earlier and much better-informed decisions about economic and environmental sustainability. The production of lithium carbonate from spodumene is considered. The conventional route is thermal decrepitation, sulphuric acid bake, water leach, purification, and recovery of lithium. The novel approach is thermal decrepitation, pressure leaching with CO₂, precipitation and purification of lithium carbonate. To ensure holistic decision-making it is important that costs, revenue, carbon footprint, water scarcity footprint and other environmental impact categories are all considered throughout the iterative design phase. Process modelling can be used to evaluate the technical and economic feasibility of a project design, whilst life cycle assessment (LCA) can be used to quantify environmental impacts of a production route or processing technology. LCA is a methodology to quantify environmental impacts associated with all stages of a product, process, or activity. An integrated approach is presented that enables the early consideration of economic and environmental factors when evaluating alternative technologies.

11:10 am Morning Tea in the Exhibit Hall (Sponsorship Opportunity Available)

11:35 The Production of High-Purity Battery-Grade Lithium Carbonate Product from Lithium Brine Sources

Nipen Shah, Head of Sales, JordProxa

The rise in demand for low-cost, high-energy density, safe and reliable batteries for the EV market is driving process and flowsheet development to produce high-quality low-cost precursor materials. Lithium is extracted from various feed sources around the world and is available for refining into a battery grade product as lithium carbonate or lithium hydroxide. Differing geologies and upstream chemistry in particular present a broad range of “impurity fingerprints” in the feed solutions that will determine the number of processing steps we need to incorporate in the flow sheet to achieve the desired product purity. These challenging feeds require careful examination and testing to prepare optimal flowsheets for each application with primary focus on meeting the stringent purity requirements, whilst seeking a balance between capital and operating costs. The lithium brines have a variable lithium content depending on each salt flat, and various impurities that are not desirable in the final product (such as calcium, magnesium, boron, sulphate, among others). The brine goes through several processing steps such as lithium extraction, concentration, refining and conversion to lithium carbonate to produce battery grade lithium carbonate. With the use of sophisticated simulation software, test work and extensive technical know-how, robust flowsheets have been developed to produce battery grade lithium carbonate from a variety of brine feed sources. This paper briefly outlines the typical feed chemistries and corresponding flow sheet options, and the balance between purity, capital, and operating expenditures during flowsheet development.

12:00 pm Membrane-Assisted Direct Lithium Extraction

Amir Razmjou, Associate Professor, Edith Cowan University, Australia

Direct lithium extraction (DLE) has led to the development of numerous technologies with the potential to recover up to 90% of lithium from various brines through laboratory studies. Nevertheless, establishing a sustainable DLE process that supports a lithium-dependent low-carbon economy still faces challenges. In recent times, there has been a continuous quest for DLE technologies that require fewer pre-treatments, use fewer materials, and employ simplified extraction procedures while ensuring high selectivity for lithium. This abstract introduces DLE technologies, exploring the different methods used to extract lithium directly from various sources. It discusses the principles, benefits, and challenges associated with these technologies. Moreover, it emphasises the environmental advantages, sustainability considerations, and potential reduction in carbon footprint achievable through DLE processes, highlighting their capacity to minimise environmental impacts compared to conventional extraction methods. The economic aspects of DLE, including cost-effectiveness, scalability, and market potential, are also explained. Moreover, membrane technology is explored as a disruptive method that could significantly enhance the large-scale implementation of DLE. Dr. Razmjou’s team has used several types of building blocks, such as nano-clay, metal/covalent organic frameworks, graphene/oxide, and MXene, to make significant progress in this field by experimentally fabricating membranes. This overview summarises their findings and outlines the strategies for designing materials to develop lithium-selective membranes incorporating nanochannels and nanopores.

12:25 Kinetics of Spodumene Recrystallisation

Bogdan Długogórski, Distinguished Research Professor, Charles Darwin University

In this presentation, we will review the kinetic models that cast the decrepitation of α-spodumene to β-spodumene [1-4] in terms of simple, and easy to apply, mathematical equations. We will also provide the predictions from the models for typical operating conditions of the kilns in lithium refineries. Such predictions could serve to optimise the kilns, and therefore to assist in the decarbonisation of spodumene processing. Two of the models [2,3] derive from the X-ray diffraction (XRD) measurements, allowing predictions of the formation of both γ- and β-spodumene from two tandem reactions: α-spod → φ β-spod + (1 – φ) γ-spod (k1), γ-spod → β-spod (k2) where, φ is the selectivity parameter that typically falls between 0.3 and 0.5. The kinetic rates (k1 and k2) correspond to the products of the Arrhenius formula and the first order reaction model: k1 = A1exp(-E1/(R T))Cα and k2 = A2exp(-E2/(R T))Cγ. Where E and A have their traditional meaning of the activation energy and the frequency factor, respectively, and Cα, Cγ and R reflect the mass fraction of α-spodumene and γ -spodumene and the ideal gas constant, in that order. Typical values of the Arrhenius constants are 780 kJ mol-1 and 75 for E1,2 and ln(A1,2/min-1), respectively [2]. The more recent work of Fosu et al. quotes E1 and E2 as 655 kJ mol-1 and 730 kJ mol-1, correspondingly, as well as ln(A1/min-1) = 59.3 and ln(A2/min-1) = 63.7. In contrast, the models based on the heat measurements in the DTA (differential thermal analyser) [1] and DSC (differential scanning calorimeter) [4] consider the spodumene recrystallisation process to proceed in an idealised one-step unimolecular reaction, which, for the model of Botto et al. [1], comprises E = 275 kJ mol-1 and ln(A/min-1) = 25.3 α-spod → β-spod, with the k = Aexp(-E/(R T))Cα

12:50 Phosphate Removal from Wastewater Using Calcium Silicate By-Products Derived from the LieNA Process

Shilpi Ray Biswas, Researcher, Murdoch University, Australia

Phosphorus is an important nutrient for living cells. Phosphorus is present in soils, sediment, and water in various chemical forms, most commonly as the phosphate (PO4-3) species. High phosphorus concentrations in aquatic environments may result from agricultural and urban runoff, leaking septic systems, or discharges from sewage treatment plants. Phosphorus abundance can cause eutrophication of water bodies and may lead to algal blooming which can be toxic to humans and animals. On the other hand, phosphorus is a finite resource. Consequently, phosphorus removal is important, and in addition, the recovery and recycling of phosphorus for applications such as fertiliser manufacture would be beneficial. This study evaluates the use of calcium silicate by-product (CSB) residue derived from the LieNA process to remove phosphate from wastewater systems. LieNA is a novel technology, developed by Lithium Australia Limited, to extract lithium directly from α-spodumene without the requirement for high-temperature conversion to β-spodumene. XRF, SEM, and TIMA analysis reveal that the CSB residue mostly comprises calcium, sodium, silicon, and oxygen. Phosphate removal experiments using CSB were conducted under a variety of conditions. The CSB showed good adsorption properties for the removal of phosphate from simulated phosphate-containing wastewater. Phosphate removal efficiency was strongly controlled by the dosage of CSB, the initial pH of the solution, and the adsorption time. Phosphate removal efficiency reached 99% after 24 hours adsorption time, at a temperature of 25°C, adsorbate dose—20g L-1, initial pH of 12, and a 100-rpm stirring speed. The phosphate adsorption had reached equilibrium after 24 hours and the adsorption capacity under these optimum conditions was 4.93 mg PO4-3 per gram of CSB. The data from adsorption kinetic measurements were well fitted by a pseudo-first order model. The phosphate recovery efficiency with CSB was compared to that for other calcium compounds, specifically laboratory-grade calcium hydroxide and calcium meta silicate, both of which have been proven effective for phosphate removal in different research studies. In the present research, CSB exhibited 57% removal efficiency for Hg whereas the removal efficiency of selected toxic metals (Zn, Cu, Cd, Pb and As) was observed to vary between 10-20% after 24 hours adsorption time, at 25°C, with adsorbate dose of 5 g L-1, initial pH of 5, and stirring speed of 100 rpm. This investigation has therefore clearly demonstrated the potential for using CSB to reduce the concentration of phosphate and toxic elements from wastewater.

1:15 Networking Luncheon (Sponsorship Opportunity Available)

2:10 Chairperson’s Afternoon Remarks

2:15 Clariant New-Generation Collectors for Flotation of Lithium Ores

Matthew Pupazzoni, Business Development Metallurgist, Clariant Mining Solutions, Australia

Global demand for lithium has increased significantly over recent years due to a dramatic increase in the use of rechargeable lithium-ion batteries in a multitude of applications, including electric vehicles, electric power storage, and electronic devices. Hard rock mining of pegmatites has emerged as a major source of lithium to meet this growing demand. The key minerals include spodumene, lepidolite, and petalite, and they are often beneficiated via complex flowsheets using multiple techniques including dense media separation, magnetic separation, and froth flotation. In the flow sheets for processing lithium ores, flotation is often used for processing fine particle-size feed, for complex ore deposits, and where high-grade concentrates are required. Clariant Mining Solutions is focused on helping the mining industry deliver the minerals needed to enable the decarbonisation megatrend in a sustainable way, and to this effect, Clariant has been working to develop a range of new collectors for more efficient flotation of spodumene and other challenging lithium ores. This paper presents some of the most recent developments. Fatty acids are often used for lithium flotation; however, the grade and recovery achieved with these collectors is often below the desired level. Also, high dosages of fatty acids are often required, and residual fatty acids in the concentrates can impart a fatty odor to the lithium concentrate which is undesired during further processing into lithium carbonate or hydroxide. Fatty acid collectors can also cause formation of calcium soaps which give rise to filtration problems and the need for acid washing. Clariant is using two strategies to develop improved lithium collectors. The first is to formulate collectors containing fatty acids but minimising the negative effects of fatty acids, and the second is to completely replace the fatty acids with alternative chemicals. Modified fatty acid formulations can improve the metallurgical performance and significantly lower dosages, thereby minimising the issues associated with residual fatty odor and soap formation while achieving lithium recoveries greater than those achieved with conventional fatty acid collectors at an improved grade. Furthermore, Clariant’s novel collectors that are free of fatty acids have been found to produce superior-grade concentrates and improved recovery at less than half the dosage of fatty acid collectors. These collectors completely eliminate the residual fatty odor and have also shown improvements in the filtration efficiency of the final concentrate.

2:40 Rethinking Powder Handling in Critical Minerals Processing: Designing for Robustness and Value Retention

Tristan Bower, Head of Global Sales, Floveyor, Australia

The increasing demand for critical minerals, encompassing lithium, nickel sulphate, rare earths, graphite, and vanadium, underscores the importance of overcoming operational hurdles in mineral refineries. Effective powder handling at the end of the production stream is essential to maintaining the integrity of these valuable products and ensuring consistent plant operation. Conveying systems play a central role in the quality of the final product. Impurities in the input materials and suboptimal conditions during mineral processing can lead to sizeable and expensive complications, including agglomeration, surface deposition, and moisture problems, potentially disrupting operations and impacting the quality of the final product. To mitigate these risks, a shift in design philosophy is required, from anticipating optimal conditions, to preparing for worst-case scenarios. Incorporating strategies in the process, such as redundancy lines, inline material conditioning, non-stick coatings, and strategic maintenance measures, can significantly enhance plant resilience. Furthermore, acknowledging powder handling as an integral part of the process, rather than an ancillary concern, is vital for ensuring robust and efficient operations. The stakes are high, considering the commercial value of these critical minerals. Any compromise in product integrity due to structural damage, contamination, or operational disruptions can lead to major financial losses. Investing in resilient plant design and robust powder handling systems contributes to maximising returns while safeguarding both the integrity of these valuable mineral products and the continuity of refinery operations. This presentation delves into downstream processing, highlighting the critical role of innovative, industrial powder handling systems to ensure value retention and operational reliability in the processing of critical minerals.

3:05 Processing and Disposal of Residues Comprising Naturally-Occurring Radioactive Material (NORM)

Hagen Gunther Jung, Executive Director, GeoEnergy Consult, Germany

Through mining/processing of rare-earths and further commodities like uranium, tantalum, etc. NORM residues accumulate, posing radiological hazards and affecting the operational efficiency. If all possibilities for minimization are exhausted, managing those requires a well-considered sequence of safe processing. NORM residues need to be (radiologically) characterised, optionally decontaminated and treated/conditioned, and finally disposed of in licensed facilities. Regulators require well-planned measures as precondition for permitting. Moreover, good management of NORM residues helps to avoid liability risks. Removal of radionuclides from equipment and facilities (e.g.; pipework for in-situ-leaching, other processing installations, etc.) through decontamination leads to dose reduction for staff and public, and prevents any contamination spreading. In a technical view, the huge advantage of removing radioactive contamination is: 1) Waste volume reduction, essential, e.g;. in the course of decommissioning: by decontamination only a residual fraction, then containing the separated radionuclides, requires further treatment as NORM waste while the largest part becomes eligible for disposal as cheaper conventional waste; 2) Re-usability of spent equipment (which otherwise would have to be disposed of), thus minimising the equipment consumption. Manual preparation and water-jetting are relatively mild and usually allow re-use of decontaminated equipment. By contrast, as chemical decontamination can employ reagents like phosphoric acid, the opportunity for equipment re-use here needs to be verified specifically. Abrasive blasting with sand does usually not allow reuse due to the caused loss in material thickness. In general, all decontamination technologies can be conducted manually or are automated for higher throughput. Important objectives of optional treatment, if indicated, are volume reduction, and foremost, fixation/immobilisation of radionuclides to prevent from spreading. For various residue types, different treatment or sequence of treatment options apply like radionuclide extraction, purification (of wastewater), incineration or high-force compaction, etc. In the case this becomes necessary, NORM residues are ready for final disposal if treatment is accomplished. Often the state is assumed to be responsible for actual disposal, i.e.; operations only deliver (treated) residues to licensed disposal facilities. However, e.g.; in the case of high volume, it can be justified that operations have an onsite disposal facility. Anyway, several disposal options are given, like backfill in mined-out underground voids or open pits, reinjection into original deposit (of flowable residues), surface/near-surface disposal (e.g.; landfill) or underground disposal (e.g.; co-disposal with radioactive waste). Which option will be realised depends both on technical/radiological properties and on country-specific regulatory requirements.

3:30 Process Selection Considerations for Recovery of Rare Earths from Mineral Sands Concentrates

Gavin Beer, Head Metallurgical Projects, Met-Chem Consulting, Australia

Mineral sand deposits contain a concentrated amount of economically important minerals known as “heavy minerals”. The minerals of economic interest typically comprise of zircon (a zirconium source) and rutile, leucoxene and/or ilmenite (titanium sources). These deposits also contain rare earth minerals such as monazite and xenotime. With the increased demand for rare earths, and specifically “magnet rare earths” of praseodymium, neodymium, terbium and dysprosium, there is an increased focus to recover the rare earths from these deposits. As both monazite and xenotime are only sparingly soluble in acid solutions, a pretreatment (“cracking”) stage is required. There are presently two commercial methods used in industry for cracking this type of concentrate. The most widely used method, known as sulfuric acid baking, mixes the concentrate with concentrated sulfuric acid followed by thermally heating to produce solid rare earth sulfates. The other method, known as caustic conversion, involves the mixing of the concentrate with a strong sodium hydroxide solution and heating to near boiling point to produce solid rare earth hydroxides. Both methods then can dissolve the soluble rare earths followed by purification prior to separation either on site or at a remote facility via solvent extraction. This paper discusses the metrics such as cost, recovery, operability, waste management and radionuclide deportment that need to be considered when selecting a process route for these rare earth concentrates.

3:55 Afternoon Tea in the Exhibit Hall (Sponsorship Opportunity Available)

4:20 Lessons Learned from Ionic Clay Testwork

Matthew Nichols, Senior Process Engineer, METS Engineering, Australia

There exists a third class of rare earth (RE) ores, which are called ionic clays. They are typically found in southern China and other subtropical areas. They are formed by the chemical weathering of rare earth elements (REE)-containing parent rocks, resulting in the formation and mobilisation of REE ions, which are then absorbed onto the clay particles and hence, the class name. The Caralue Prospect in South Australia was initially established as a high purity kaolin prospect following identification of thick intervals of bright white kaolin—close to surface—in several historical drill holes. A 2022 drilling program undertaken by iTech identified significant REEs, in the kaolin rich intervals, over a large area. The Caralue Bluff Prospect has an exploration target of 110-220 Mt @ 635-832 ppm TREO and 19-22% Al2O3. (This exploration target is based on 80 drill holes, from a total program of 260 holes, across an area of approximately 12km x 12km, as reported by iTech on 18 August 2022, “Exploration Target Defined at Caralue Bluff.”) Significantly, it remains open in multiple directions, allowing for possible expansion. The REE mineralisation is rich in key magnet REEs, namely neodymium, praseodymium, dysprosium, and thulium (NdPr-Dy-Tb), averaging 25% of the REE basket. Initial testwork organised by iTech Minerals at a commercial laboratory achieved zero recovery. Itech contacted METS, and a metallurgical testwork program was developed and executed, resulting in eighty-seven percent (87%) leaching recovery of the REEs. In addition, process optimisation resulted in reduced OPEX and CAPEX. At the same time, a kaolin product was produced as a by-product.

4:45 Optimising Reagent Use in Clay Hosted Rare Earth Extraction

Jess Page, Manager, Data Analytics, WGA, Australia

Understanding what makes a project profitable in the design phase is crucial. We usually rely on existing data for benchmarking, but in this case, due to limitations on what data was available, we supported an extensive bench and pilot test work campaign with AR3 to create cost estimates and designs. As a result of our approach, our main focus in flowsheet development is finding ways to reduce operating costs, particularly by recycling reagents. This approach involved using a data science approach to quickly test different scenarios and pinpoint what drives profits the most.

5:10 Rare Earth Extraction with Lonquest 801

Chiara Francesca Carrozza, Technical Development Specialist, Italmatch Chemicals, Italy

Rare earth elements (REEs) are indispensable components in the manufacturing of high-tech devices, renewable energy technologies, and defense applications. As global demand for these elements continues to rise, there is a pressing need to optimise extraction processes for both efficiency and environmental sustainability. This study explores approaches to rare earth extraction using IONQUEST 801 and integrates predictive modelling to enhance process understanding and optimisation. We conducted a screening test, varying process parameters such as temperature, pH, and reagent concentrations systematically, to optimise extraction efficiency. Starting PLS solution was prepared in the lab with the following rare earth elements, La – Ce – Gd – Dy – Y at 0.02 M. The data obtained were used to develop empirical and mechanistic models to predict rare earth extraction yields and flowsheet. Further tests were performed, mixing specific concentration of different extractant and/or phase modifier. Our experimental results demonstrate the effectiveness of the proposed extraction methods, highlighting improvements in both yield and selectivity. The developed models successfully capture the complex relationships between process parameters and extraction efficiency, providing valuable insights for process optimisation.

5:35 Happy Hour in Exhibit Hall (Sponsorship Opportunity Available)

6:55 pm Close of Day

Friday, 31 May

8:30 am Registration & Arrival Tea

9:00 Chairperson’s Opening Remarks

9:05 Thermodynamic Modelling of Rare Earth Solvent Extraction

Brett Schug, Senior Simulation Consultant, SysCAD, Canada

Rare Earth Elements (REEs) are becoming increasingly important due to their critical role in energy transition. In recent times, there has been significant activity and investment in production from mining and recycling. A key area of difficulty for metallurgical production of REEs is their separation, largely due to their similar electron structures which makes them chemically similar. In this work, a thermodynamic model of solvent extraction (SX) is presented based solely upon experimental data in the open literature using the PHREEQC (USGS, 2021) interface with SysCAD. In previous work, Heppner (2021) calculated reaction equilibrium constants for the extraction of Nd and Pr based upon fitting to experimental data of Lyon et al. (2017). Here, that model is extended using separation factors published by Zhang et al. (2020) and references therein to estimate the equilibrium constants for all 15 REEs. Pitzer parameters and their temperature dependence are calculated for each cation-anion interaction in the REE chloride system from correlations published by Simoes et al. (2016, 2017). It is noteworthy that aqueous/organic exchange reactions are written in terms of free acid, not hydrochloric acid, and thus, are suitable for use in any acidic medium (e.g. chloride, sulphate, nitrate). A test of the model was performed where a solution containing REE chlorides was fed to an extraction, scrubbing, and stripping circuit with conditions typical for initial separation of light, medium, and heavy REE elements. Results of the test model show typical trends in the SX separation of REEs, confirming the validity of the approach. This fundamental approach enables a wider range of applicability for the model compared to the use of plant isotherms. This work focuses on the modelling methodology of the REE SX process, rather than the modelling of a specific processing plant. For this reason, the presented model requires validation against relevant plant data prior to use for plant design or optimization.

9:30 Precipitation of Rare Earth Element Salts of High Purity

Kerstin Forsberg, Professor, KTH Royal Institute of Technology, Sweden

Rare earth elements (REE) are essential in high performing permanent magnets used in e.g.; wind turbines and motors. A rising demand coupled with a scarcity of supply makes some of the REE identified as critical raw materials in many parts of the world. There is a need to develop more sustainable and competitive processes for REE extraction from primary and secondary resources. Magnets can be recycled via different approaches including reuse, direct recycling, or indirect recycling. In indirect or chemical recycling, the end-of-life products are processed to extract the REE and to make the elements available for new uses. Developing techniques to do this in an economically and environmentally sustainable way is vital to create a raw-materials circular economy for these materials. An important step is the precipitation of REE salts, which should be designed to obtain crystals of high quality in terms of crystal size, size distribution and purity. Antisolvent precipitation is a promising technique to obtain rare earth salts with high yield and of high quality. In this talk key aspects in the design of REE antisolvent precipitation processes for obtaining crystals of high quality will be presented. The focus will be on precipitation of mixed REE sulphates from impure leach liquors in the recycling of magnet waste. Different mechanisms for impurity incorporation will be discussed. Possibilities to control the precipitation process to avoid impurity incorporation will be presented. The findings can be directly applied to processes for recycling of magnet waste, but also to other hydrometallurgical processes where there is a need to recover REE salts of high quality.

9:55 Australia’s Only Rare Earths Project With In Situ Recovery Potential

Robert Blythman, Exploration Manager, Cobra Resources, Australia

The Boland Rare Earth Project is a new rare earth deposit style that is amendable to in situ recovery (ISR) mining. ISR is an established mining method for Uranium. ISR uranium mines dominate the lowest cost producers of uranium globally with CAPEX 10-15% of conventional mines and OPEX 30-40% lower than conventional mines (UXC,2023). Cobra has executed an exploration approach to identify a style of rare earth mineralisation type that allows for sustainable low-cost extraction of rare earths. Preliminary leach results completed by ANSTO demonstrate magnet rare earth recoveries of up to 58% and heavy rare earth recoveries of up to 65% at a pH of 3-4 over 30 minutes to 6 hours at ambient temperatures and utilising an AMSUL wash. Dissolution of gangue elements (Al, Ca, Fe U, Th) are low. Cobra is in the process of undertaking low pressure column leach testwork through ANSTO to confirm amenability to in situ recovery. A wellfield test pattern was installed in early 2024 to build an aquifer baseline dataset to support a future ISR trial. ISR circumvents challenges compared to conventional mining of clay deposits including particle size separation (beneficiation), heap or tank leaching, desliming and material management. The paleochannel geological setting is distinct from the Southern China weathered slope setting, allowing for greater reagent control in situ and post extraction aquifer remediation. Pregnant solution from the column leach test will be used to assess membrane desorption as a low-cost method to process and deliver higher value selective rare earth carbonates.

10:20 Lithium-ion Battery Shredding Challenges

Andreas Mönch, Principal Research Consultant, CSIRO, Australia

Lithium-ion batteries (LIBs) are increasingly becoming a significant waste stream, presenting substantial challenges for recycling and disposal. Due to their complex design and the variety of materials used, several steps are necessary before they can be reused or recycled. Initially, LIBs are sorted and typically undergo preprocessing, which includes discharge or deactivation, disassembly, and separation. After these steps, they can either be directly recycled or processed using pyrometallurgy, hydrometallurgy, or a combination of these methods. Each recycling process for lithium-ion batteries has its own advantages and disadvantages. While pyrometallurgy might seem like the simplest option due to its ability to handle a flexible feedstock, it has issues such as relatively low lithium recovery rates and the production of hazardous off-gases and fly ash residues. These challenges have led most recent recycling projects to shift towards hydrometallurgy processing routes. For safe processing, both pyrometallurgy and hydrometallurgy require the discharge and disassembly of larger battery packs. These packs are commonly used in rapidly growing markets such as electric vehicles (EV) and battery energy storage systems (BESS). Due to competitive manufacturing costs, these sectors are increasingly using battery packs as structural components and employing foam encapsulation for thermal management. This, however, inhibits access to the battery management system (BMS) and greatly complicates the discharge and disassembly of the packs. This manufacturing trend has meant that traditional wet shredding in air is increasingly not variable, due to the inherent inability to guarantee electric discharge, through the lack of access to the BMS, and the volatile organics used in the battery’s electrolyte which present significant fire and environmental risks. Current state-of-the-art employs dry shredding in an inert atmosphere using an airlock, to ensure safer operation. It also allows for the potential recovery of the electrolyte, either through non-aqueous organic washing, direct vacuum distillation, or a combination of both. While this method theoretically reduces fire and environmental hazards, it is practically impossible to ensure full discharge of LIBs due to inaccessible terminals and inherent voltage rebound. Our tests with a custom designed industrial shredder show that even when fully discharged, cells create thermal hotspots and release elevated temperature gases. Battery cells at low charge state will cause electrical arcing during the shredding process, and if oxygen levels cannot be kept below flammability limits, the cell’s electrolyte solvents are likely to ignite. Maintaining a near-inert atmosphere in an industrial shredder processing encapsulated EV or BESS packs is impractical due to the battery packs’ large geometry and corresponding volume of air trapped within the foam encapsulation, and inevitable process airlock leaks. This presentation will discuss the magnitude of the challenge and key safety insights from our experimental pilot shredder, which operates in a low oxygen atmosphere when shredding LIB cells at various discharge levels. It will also outline future research directions and suggest potential solutions for upstream manufacturing.

10:45 am Morning Tea in the Exhibit Hall

11:10 Impact of Organic Impurities on Acid Leaching of Valuable Metals from Used Li-ion Batteries

Mooki Bae, Researcher, Korea Institute of Geoscience and Mineral Resources (KIGAM), South Korea

As the usage of lithium-ion batteries (Li-ion) increases, the need for efficient recycling methods to recover valuable metals such as lithium, nickel, and cobalt becomes critical. Acid leaching is a commonly used technique for extracting metals from spent Li-ion batteries. However, the presence of organic impurities within the battery materials can significantly impact the leaching process. This study aims to investigate the influence of these organic impurities on the effectiveness of acid leaching processes. The spent Li-ion batteries underwent thermal treatment to eliminate organic components, including binders and separators, followed by sulfuric acid leaching to extract valuable metals. The thermal treatment was conducted at various temperatures, and the resulting black powder was analysed to observe changes in metal concentration post-leaching. The impact of organic impurities on the leaching process was assessed by comparing the leaching efficiency of samples with and without thermal treatment. The thermal treatment procedure involved exposing samples to temperatures of 0°C, 200°C, 400°C, 600°C, and 800°C in ambient air for 2 hours, followed by storage at room temperature for leaching purposes. For LCO-based batteries, primary reactions mostly reached equilibrium within an hour, with additional leaching observed after hydrogen peroxide supplementation. The leaching rate increased with higher thermal treatment temperatures, with differences of up to 20% observed. At 1000°C, the cobalt leaching rate reached 94.6%, while samples treated at 800°C, 600°C, 400°C, and 200°C exhibited cobalt leaching rates of 86.2%, 68.9%, 72.9%, and 72.9%, respectively. Untreated samples displayed a cobalt leaching rate of 77.4%. The provided NCM-based black powder underwent thermal treatment followed by sulfuric acid leaching. With increasing thermal treatment temperature, the anode material (C, graphite) and organic substances were removed, resulting in concentration changes from Ni 5.27 wt%, Co 1.37 wt%, Mn 0.43 wt%, Li 1.07 wt% to Ni 6.56 wt%, Co 2.82 wt%, Mn 0.63 wt%, Li 1.47 wt%. Although leaching rates remained mostly consistent, higher thermal treatment temperatures led to the extraction of relatively more valuable metals. For instance, samples treated at 800°C for 6 hours exhibited leaching of Ni 1002.4 mg/L, Co 537.6 mg/L, Mn 117.4 mg/L, and Li 274.8 mg/L. In conclusion, the study underscores the significance of thermal treatment in enhancing the efficiency of acid leaching processes for metal recovery from spent Li-ion batteries. The investigation sheds light on the intricate relationship between thermal treatment temperatures, organic impurities, and leaching efficiency, offering valuable insights for optimising recycling methodologies in the pursuit of sustainable battery management.

11:35 Lewatit Ion Exchange Resins for the Recycling of Lithium-ion Batteries

Dirk Steinhilber, Manager, Technical Marketing, LANXESS, Germany

The growing demand for high purity battery lithium, nickel, cobalt, and copper requires access to new resources. The most economic and environmentally friendly approach is the recycling of end-of-life batteries. Due to the high concentration of battery metals, they can be extracted and recycled with low carbon footprints and at low cost. Therefore, the European Union established strictly-regulated recycling targets and a minimum level of recycled battery metals content for the manufacturing of new batteries. As a result, processes with true circular economy are developed. A lot of cathode off-spec material is already available from cathode producers and more end-of-life batteries will be available within the next years. Lewatit ion exchange resins are crucial for many process steps in the hydrometallurgical recycling flow sheets. In this paper we describe three of the most important applications and the benefits of our resins in the field of battery recycling. Purification of black mass leachate recycling usually starts by discharging, dismantling, and shredding of lithium-ion batteries. In hydrometallurgical operations the solid black mass powder is separated by filtration because it contains the valuable metals lithium, nickel, cobalt, manganese. Leaching of the black mass with acid dissolves these valuable metals. However also impurities like Cu, Al, Zn, and Fe are usually contained in the concentrates, because mechanical separation cannot be performed perfectly. These impurities can be efficiently removed with selective chelating resin Lewatit MDS TP 260. We especially developed a new efficient Al regeneration technology with the use of NaOH and elution of the Al(OH)4- anionic complex. Thanks to the smaller size of our monodisperse small (MDS) resins and, in turn, shorter diffusion paths, they exhibit faster kinetics during exchange and regeneration. Not only does their high packing density make them ideal for chromatographic separation, but they also have a higher capacity utilisation and, in turn, longer service lives with lower requirements for regeneration chemicals. Since black mass contains a high concentration of battery metals, separation of the individual metals is usually performed by solvent extraction. The generated metal concentrates are most efficiently purified by our selective chelating resins, e.g;. Li with Lewatit MonoPlus TP 207, Ni with Lewatit TP 272, and Co with Lewatit VPOC 1026 and Lewatit MDS TP 220. Our selective chelating resins are especially suited for this separation task because of their high selectivity and loading capacity towards impurities, which ensures efficient removal below the specification limit. At the same time, they show low interaction towards valuable and concentrated battery metals nickel and cobalt, which pass the resin at high yield and recovery. Wastewater streams generated by battery metals recycling plants can be efficiently treated by Lewatit MonoPlus TP 207. This resin selectively removes toxic heavy metals in the presence of high concentrations of other constituents of the wastewater, e.g.; hardness. Valuable battery metals can additionally be recovered and recycled from the resin by selective regeneration. In conclusion, Lewatit ion exchange resins provide benefits including up to two times longer cycle times compared to conventional resins, combined with savings on regeneration chemical costs. Excellent exchange kinetics ensures contaminant removal down to trace levels and yields pure battery metal concentrates. Additionally, Lewatit chelating resins possess high resilience towards osmotic and mechanical stress and ensure long resin lifetimes.

12:00 pm Low-Carbon Footprint Bio-Diluents for Solvent Extraction in Lithium-ion Battery Recycling

Zubin Arara, Global Market Manager, TotalEnergies Fluids, France

TotalEnergies Fluids is a leader in the design, production, and sale of high-purity, biodegradable hydrocarbon solvents. Designed as aliphatic diluents dedicated to the solvent extraction (SX) process in hydrometallurgy, the Elixore range offers a choice of perfectly inert, colorless, and odorless solutions for metal extraction in battery recycling. From the same plant based in the north of France that pioneered the production of Sustainable Aviation Fuel (SAF) at TotalEnergies for the Aviation Industry, TotalEnergies Fluids now produce a range of bio-hydrocarbon solvents, under the name of Biolife range, coming from bio-feedstocks such as Used Cooking Oil (UCO) which offer low carbon footprint solutions to the industry. These products have been studied in detail over the last year at the Hydrometallurgical lab of CNRS, University of Lorraine, Nancy, France with the aim to design a single Universal Diluent that can be used in the multiple solvent extraction steps of a hydrometallurgical process of Recycling of EV Batteries for extraction of Cu, Al, Mn, Co, Ni, & Li. The results were recently published in a Technical Paper in the prestigious journal Royal Society of Chemistry*. One such low-carbon bio product commercialised in July 2023 after excellent results is “Elixore Biolife EV 205.” This presentation elucidates the distinctive features of this innovative product, emphasising its remarkably low carbon footprint; a detailed flowsheet illustrating the product’s integral role in the hydrometallurgical process of Battery Recycling will be showcased, underscoring its potential to significantly reduce Scope 3 emissions in Battery Recycling plants; and a live industrial project set to use Elixore Biolife EV 205.

12:25 Hydrometallurgical Process to Extract Metals from LFP-NMC Blackmass in Spent Lithium-Ion Batteries

Alexandre Chagnes, Professor, Université de Lorraine, France

Lithium-ion batteries are central to the global shift towards sustainable energy and electric transportation. As we witness the rise of gigafactories and recycling facilities worldwide, catering to the production and reclamation of batteries for electric vehicles, it becomes evident that a similar focus is required for smaller scale batteries, notably those utilized in electric bicycles, a swiftly expanding market. The processes involved in recycling these batteries may not mirror those of electric vehicle batteries due to disparities in material composition. While electric vehicle batteries predominantly consist of NMC (LiNixMnyCozO2) or LFP (LiFePO4) technologies, batteries for electric bicycles encompass a blend of NMC and LFP technologies. Hence, there arises a necessity to devise adaptable recycling processes capable of handling varying compositions. Moreover, the hydrometallurgical methods employed for treating these materials must effectively recover cobalt, nickel, manganese, and lithium, despite the presence of fluctuating concentrations of iron, a challenge inherent to hydrometallurgy. This presentation elucidates how leveraging the physicochemistry of transition metals in conjunction with phosphate enables the development of an efficient leaching process. Such a process selectively dissolves cobalt, nickel, manganese, and lithium from mixtures of NMC and LFP batteries, yielding a sufficiently pure leachate conducive to subsequent purification steps via liquid-liquid extraction post-leaching.

12:50 Networking Luncheon (Sponsorship Opportunity Available)

1:45 Chairperson’s Afternoon Remarks

1:50 Recent Technological Progress in Metals’ Recovery from Spent NCM Battery Promoted by New Separation Reagents

Shengxi Wu, Lecturer, Central South University, China

Valuable metals recovery from the spent lithium batteries (black mass) is of vital importance, since it eliminates the heavy metal pollution threat and provides an alternative solution for the supply crisis of critical metals (Ni/Co/Mn). However, traditional recovery technologies that consisted of leaching and individual element separation by solvent extraction still faced several challenges: separation difficulties between Ni2+(Co2+)/Mg2+, Mn2+/Ca2+, Li+/Ni2+, Li+/Na+(K+), and incomplete removal of fluorine due to the limited separation coefficient of previous methods. To solve these issues, a series of solvents including HBL-120 for Ca extraction from Mn, HBL-116 for Ni(Co) extraction from Mg and Li, HBL-121 for Li extraction from Na(K), and HBL-221 for F extraction from Ni(Co&Mn) were designed and synthesised.

(1) Ca separation from Mn with HBL-120 makes the preferential removal of Ca before impurities extraction with D2EHPA is possible, which eliminates CaSO4 scaling issue during stripping of impurities extraction with D2EHPA and directly produces pure MnSO4 product.

(2) Selective Ni(Co) extraction from Mg containing solutions shortens the Co extraction (HEHEHP) – Ni extraction (HEHEHP) – Mg extraction (Cyanex 272) into Ni(Co) extraction (HBL-116)-Mg precipitation, which saves >50% of labor and land.

(3) Fluorine originating from the electrolyte and adhesive cannot be completely removed via traditional methods and brought massive Ni(Co) loses in fluorine removal residue. Specific extractant HBL-221 binds fluorine and extracted Me-F complex into organic phase, with <5mg/L F left in raffinate and <0.1 Ni(Co&Mn) loss.

(4) Li generally reports into a concentrated Na2SO4 solution since all the extraction processes for Ni/Co/impurities adopted Na-saponification.

However, traditional carbonate precipitation-evaporating concentration process recovered only ~85% of Li (~10% Li loss in Na2SO4 crystal) and produced crude Li2CO3 entrained considerable Na2SO4. Selective Li extraction from Na(K) concentrated solutions with HBL-121 significantly elevated the Li recovery to >99% and produced Li2SO4 solution with Li/Na(K)>100. So far, all technologies mentioned above have been applied individually or packaged in many hydrometallurgical plants for spent LIBs recycling in China and USA (pilot test). Based on these new extractants, an alternative short process for metal recovery from the leaching solutions of NCM black mass was proposed, which includes Ca(Zn) extraction with HBL-120, impurities extraction with D2EHPA, fluorine extraction with HBL-221 (if needed), Co extraction with HEHEHP, Ni extraction with HBL-116 (or Ni/Co coextraction with HBL-116), Mg precipitation with NaOH, Li extraction with HBL-121. This process owns merits of high metal recovery, reagent saving, short process, and economy.

2:15 Optimised Nickel and Cobalt Recovery from Battery Waste Using Solvent Extraction

Leslie Miller, Senior Application Engineer, OLI Systems, USA

A new thermodynamic database has been developed for solvent extraction using DHEPA and Cyanex 272 for the purification of nickel and cobalt in battery recycling applications. The database was developed using a combination of experimental data and theoretical calculations. The experimental data included phase equilibrium data for the extraction of nickel and cobalt from sulfate and chloride solutions using DHEPA and Cyanex 272. The theoretical calculations were used to develop models for the prediction of phase equilibria and other thermodynamic properties of the system. The new database was used to model and optimise a hydrometallurgical battery recycling process. The process flowsheet included the following steps: 1. leaching of the spent lithium-ion batteries in a sulfuric acid solution, 2. separating the transition metals into the pregnant liquor (PL) using standard hydrometallurgy techniques, 3. solvent extraction of nickel and cobalt from the leach solution using DHEPA and Cyanex 272, and 4. stripping the separated nickel and cobalt from the organic phase: process simulation software was used to model the solvent extraction units. The model predicted the nickel and cobalt extraction performance as a function of the separation pH, temperature, solvent-PL mixing ratio, separation efficiency, extractant concentration in the diluent, and number of stages. The validated model was then used to optimise the operating conditions of the solvent extraction unit in order to maximise the extraction efficiency while minimising the co-extraction of impurities. The results of the modelling and optimisation study showed that the new thermodynamic database can be used to effectively predict the partitioning of Ni and Co between the water and organic phases. When coupled with a process simulation software, it accurately predicted the heat, mass, and speciation balance among the separation units, and optimised the processes within the constraints of the existing operating conditions.

2:40 Integrated Technologies for Efficient Recycling of Lithium-Ion Batteries

Leonel Yew, Process Engineer, Neometals, Australia

Lithium-ion batteries have become essential components in various industries, from consumer electronics to electric vehicles, leading to a surge in demand for efficient recycling processes. This presentation highlights the innovative integrated technologies developed by Neometals/Primobius for the recycling of lithium-ion batteries, emphasising the critical role of the interplay between the shredding and beneficiation spoke and a hydrometallurgy hub. The shredding and beneficiation spoke of our integrated system consists of advanced technology designed to efficiently disassemble and separate battery components, resulting in the generation of “Black Mass” as the output. This Black Mass serves as the high-quality input material for the subsequent processes in our hydrometallurgy hub. Our hydrometallurgy hub incorporates advanced techniques to extract and purify metals from the Black Mass with high efficiency and minimal environmental impact. This hub plays a pivotal role in closing the loop of the lithium-ion battery lifecycle by enabling the reclamation of critical metals for reuse in new battery production. Through the integration of these technologies, Primobius has established a comprehensive and sustainable approach to lithium-ion battery recycling, addressing the environmental concerns associated with e-waste and contributing to the circular economy. The presentation will showcase the technical aspects and benefits of our integrated system, demonstrating its potential to revolutionise the recycling industry and support the growing demand for clean energy technologies.

3:05 Afternoon Tea in the Exhibit Hall

3:30 Development of Aurubis’ Hydrometallurgical Li-ion Battery Recycling Process

Andrew Harris, Senior Research & Development Metallurgist, Aurubis AG, Germany

Aurubis AG, Europe’s largest Copper producer and globally the largest Copper recycler, has developed and patented a hydrometallurgical process to recycle both pyrolysed and un-pyrolysed Black Mass (BM) stemming from Li-ion batteries. This purely inorganic process, comprised of leaching, precipitation, and crystallisation processes, has been developed by Aurubis’ R&D Hydromet Department and piloted at our Hamburg site successfully since April 2022. The process developed by Aurubis centers on a lithium-first leach whereby most of the lithium is recovered as a sulphate solution which can be purified or converted into intermediates like lithium carbonate. Subsequently, a leach process targeting nickel and cobalt is relatively straightforward with impurity removal following. From this leach solution, cobalt, manganese and nickel are separated and recovered as saleable intermediates. The graphite-rich leach residue from the pilot plant has been used for flotation flowsheet development where concentrates of >92% carbon grade from locked cycle tests have already been recently presented. We will show the evolution of the Aurubis black mass treatment process by presenting the results from consecutive pilot plant campaigns. Specifically: major value element recoveries, accountabilities, and product purities achieved will be presented.

3:55 Matte Smelting and Purification Process for Recycling of EoL-LiB

Joon Sung Choi, Researcher, Research Institute of Industrial Science and Technology (RIST), South Korea

Recently, as the production of electric vehicles has rapidly increased, the production of lithium-ion batteries containing high-purity valuable metals (Ni and Co) is required. According to the rapidly increasing number of end-life lithium-ion batteries (EoL-LiB), there is a need to improve environmental issues. However, there are limits to process changes for removing impurities and achieving high purity of diversified recycled resources in hydrometallurgical process for recycling of EoL-LiB. Therefore, a transition to a hybrid process capable of mass production is required, and the research was conducted on matte smelting and purification process using recycled resources. Ni and Co contained in various resources were recovered using molten iron in high-temperature smelting process. The recovery behavior depending on the type of resource by carbon content was compared with the thermodynamic calculations using FactSage 8.2TM. The alloy containing Ni and Co was concentrated through addition of sulfur and oxygen-blowing, and smelted into matte with improved concentration of Ni and Co. An aqueous solution containing Ni and Co was obtained through a pressure oxidation leaching (POX), and it was confirmed that the Ni and Co recovery rates were closely related to the ORP and pH of the pregnant leaching solution (PLS). The leachate was highly purified into Ni and Co compound through a neutralisation process, and the impurity concentration in the Ni and Co compound was maintained below 0.5%. In order to develop the matte smelting and purification process utilising recycled resources, process condition was established by engineering software (METSIM).

4:25 CLOSING PANEL DISCUSSION

Track 2: 2024 Lithium-Battery Technology-Rare Earths Agenda

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