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Sustainable Urban Mining of Critical Elements from Magnet and Electronic Wastes Ames Laboratory Accepted Manuscripts Ames Laboratory 11-12-2019 Sustainable Urban Mining of Critical Elements from Magnet and Electronic Wastes Denis Prodius Ames Laboratory, [email protected] Kinjal Gandha Ames Laboratory, [email protected] Anja-Verena Mudring Ames Laboratory Ikenna C. Nlebedim Ames Laboratory, [email protected] Follow this and additional works at: https://lib.dr.iastate.edu/ameslab_manuscripts Part of the Other Materials Science and Engineering Commons, and the Sustainability Commons Recommended Citation Prodius, Denis; Gandha, Kinjal; Mudring, Anja-Verena; and Nlebedim, Ikenna C., "Sustainable Urban Mining of Critical Elements from Magnet and Electronic Wastes" (2019). Ames Laboratory Accepted Manuscripts. 545. https://lib.dr.iastate.edu/ameslab_manuscripts/545 This Article is brought to you for free and open access by the Ames Laboratory at Iowa State University Digital Repository. It has been accepted for inclusion in Ames Laboratory Accepted Manuscripts by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. Sustainable Urban Mining of Critical Elements from Magnet and Electronic Wastes Abstract A straightforward and environment-friendly process for acid-free leaching of rare-earth elements and cobalt, which are critical materials, from waste magnet materials has been developed. The process also allows for selective leaching of rare-earth elements from magnet-containing electronic wastes, such as end-of-life hard disk drives and electric motors. The use of copper salts eliminates the use of volatile toxic acids in the dissolution and separation processes, which allows for a more eco-friendly approach to recovering critical elements and a safer work environment. Recovered critical materials were shown to be suitable for reinsertion into the materials supply chain. Keywords Acid-free leaching, Rare-earth permanent magnets, Rare-earth recovery, Sustainability Disciplines Other Materials Science and Engineering | Sustainability This article is available at Iowa State University Digital Repository: https://lib.dr.iastate.edu/ameslab_manuscripts/ 545 Sustainable Urban Mining of Critical Elements from Magnet and Electronic Wastes Denis Prodius, Kinjal Gandha, Anja-Verena Mudring,†* and Ikenna C. Nlebedim* Critical Materials Institute, Ames Laboratory, U.S. Department of Energy, 2332 Pammel Drive, Ames, Iowa 50011, USA [email protected] ABSTRACT: A straightforward and environment-friendly pro- higher recovery rates of REEs, especially as oxides or in other non- cess for acid-free leaching of rare earth elements and cobalt, which metallic forms. Nevertheless, most hydrometallurgical approaches are critical materials, from waste magnet materials has been devel- are energy-intensive and require substantial amounts of hazardous oped. The process also allows for selective leaching of rare earth chemicals, especially strong mineral acids such as hydrochloric, elements from magnet-containing electronic wastes, such as end- sulfuric and nitric acids. High volumes of wastes including residual of-life hard disk drives (HDDs) and electric motors. The use of cop- strong mineral acids present obvious environmental problems. In- per salts eliminates the use of volatile toxic acids in the dissolution vestments to contain both the acids and their contaminated wastes and separation processes, which allows for a more eco-friendly ap- add to the cost of the process. Thus, there is an obvious need for a proach to recovering critical elements and a safer work environ- cost-effective, environment-friendly and energy-efficient method ment. Recovered critical materials were shown to be suitable for for recycling REEs-containing materials. reinsertion into the materials supply chain. Herein, we report a novel and safer process for leaching REEs and KEYWORDS: Acid-free leaching, Rare earth permanent mag- cobalt from permanent magnet materials. The chemical dissolution nets, Rare earth recovery, Sustainability method involves contacting the REEs-containing material and an aqueous solution of a copper(II) salt to dissolve magnet materials. INTRODUCTION The REEs are then precipitated from the aqueous solution, which then can be calcined to produce REE-oxides or other REE- The global need for rare earth elements (REEs) is increasing be- compounds. This process also enables selective leaching of the cause they are indispensable for a wide range of applications in- REEs contained in waste magnets from e-waste products such as cluding permanent magnets, lighting, lenses, catalytic converters shredded hard disk drives (HDDs) and crushed electric motors. 1-7 and many consumer electronics. New disruptive technologies Using copper(II) salts for the oxidative dissolution of magnets al- can increase the need for REEs and result in significant market un- lows for a selective and atom economy transfer of the relevant met- certainties. In magnet applications alone, the use of REEs is ex- als into solution. Moreover, it helps to avoid the use of strong min- pected to increase and has been forecasted to exceed $50 billion eral acids, hence eliminating the associated harsh reaction condi- 8 market value by 2022. Neodymium (Nd), dysprosium (Dy), ter- tions. The recycling process allows for the copper content of the bium (Tb), samarium (Sm) and praseodymium (Pr) are crucial for copper(II) salts to be recovered and reinserted into the value chain. high performance magnets which, in turn, are critical for technolo- Interestingly, a significant amount of global copper supply is ob- gies such as wind power generators, electric powertrains, mo- tained with the aid of microorganisms via bioleaching.19-21 tors/generators, and in everyday consumer products like computers, The recycling process was developed considering the application mobile phones, amongst many others. Nd, Tb and Dy are among of green chemistry principles (acid-free dissolution of magnets the elements which the U.S. Department of Energy9 and the Euro- through redox-dissolution with copper(II) salts). It was also devel- pean Commission10 classified as being at risk of supply disruption. oped in view of potential commercial adoption such that the recov- Cobalt (Co) is also critical for energy-related applications, includ- ered REEs and other recycling co-products are suitable for reinser- ing permanent magnets and lithium-ion batteries. Recovering these tion into the supply chain. Moreover, to maximize profit in the ap- critical elements from waste REEs-containing materials can be eco- plication, the process development included recovery and reinser- nomically and technically viable approach towards helping address tion of some of the chemicals back into the recycling process. the supply risk challenges.11 When properly done, recycling can help conserve natural resources, save energy and result in less toxic wastes being dumped in landfills. One approach to accomplishing EXPERIMENTAL SECTION 12 this is to follow the principles of Green Chemistry. Material. The recycling feedstock materials used for this work in- Recycling of REE-containing materials can be done either by di- clude: (a) Nd-Fe-B grinding swarfs from U.S. magnet plants (Sup- rectly reusing the materials or via chemical recovery of the rare plementary information, Fig. S1), (b) hydrogen decrepitated Nd- earth elements. The chemical recovery methods for REEs generally Fe-B magnets manually harvested from end-of-life HDDs, (c) Sm- involve either pyrometallurgical or hydrometallurgical ap- Co grinding swarfs also from U.S. magnet plants, (d) Nd-Fe-B con- proaches.13-18 In the pyrometallurgical approach, the REEs recov- tained in two types of e-waste materials: shredded HDDs (supplied ery rates are reduced by slag formation, due to the high affinity of by Dr. Tim McIntyre, Oak Ridge National Laboratory) and crushed the REEs with oxygen. Pyrometallurgical approaches also generate electric motors (from www.amazon.com, “Great Planes ElectriFly large amounts of solid wastes and can be quite energy-consuming, RimFire .10 35-30-1250” Outrunner Brushless Motor”). Swarfs are although they can have the advantage of recovering the REEs in the metal powders derived from post-manufacturing processing includ- form of metals, instead of oxides. Hydrometallurgical routes enable 1 ing grinding, cutting, etc. which are typically oxidized and contam- of 0.88 kg of copper(II) nitrate hemi(pentahydrate) in 3.5 L of water inated by grinding media and lubricants. Decrepitation was per- and stirred at 300 rpm for about 5 hours. The reaction proceeded formed in a stainless steel vessel at 4 bar of hydrogen pressure and exothermically with no heat applied. Afterward, residue found to room temperature. For making magnets using recovered REE ox- be a mixture of Cu2O/CuO/Fe2O3/Fe3O4 (see the PXRD pattern ide, the oxides were first reduced to Nd/Pr metal ingot at the Ames in Fig. S3 and EDX mapping in Fig. S10), was filtered off. The Laboratory Materials Preparation Center (MPC) using the estab- copper-containing precipitate can be used as a source for copper. 22, 23 lished Ames process. Part of the ingot was alloyed with 99.9% For recovering REEs from the filtrate, a two-step approach was ap- pure Fe and Cu (from MPC) and 99.5% pure boron (from AlfaAe- plied aiming to exclude the presence of iron in the final REE oxides sar) via arc melting (in Ar atmosphere) to produce a magnet feed- (Figs. S4, S13). In the first step, the filtrate was stirred together with stock with composition (Nd-Pr)2.3Fe14B + 0.5 wt.% Cu. The arc- an aqueous ammonia solution (28%) at 60 °C for 2 hrs which led melted material was used to prepare melt-spun ribbons by inductive to the precipitation of Fe(III) and RE(III) hydroxides. Then, a small melting in fused silica crucibles and ejection of the melt onto a sin- excess of solid crystalline H2C2O4·2H2O was added, followed by gle copper wheel at 30 m/s surface velocity through a 0.8 mm ori- heating to 80 °C and stirring until insoluble REE oxalate precipi- fice. Melt spinning was performed in 1/3 atmosphere of high purity tated and highly soluble double salt of iron-ammonium oxalate He gas.
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