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Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023

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A special issue of Metals (ISSN 2075-4701). This special issue belongs to the section "Extractive Metallurgy".

Deadline for manuscript submissions: closed (30 November 2023) | Viewed by 20107

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Dr. Srecko Stopic

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Guest Editor

IME Process Metallurgy and Metal Recycling Department, RWTH Aachen University, 52056 Aachen, Germany
Interests: environmental protection; recycling; metallurgy; mineral processing; nanotechnology; waste water treatment
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Prof. Dr. Bernd Friedrich

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Guest Editor

IME Process Metallurgy and Metal Recycling, RWTH Aachen University, 52056 Aachen, Germany
Interests: pyrometallurgy; process technology; metals; recycling; purification; alloying; WEEE; spent batteries; critical materials; circular economy; electrometallurgy
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Special Issue Information

Dear Colleagues,

The first volume of this Special Issue, “Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2021” contains 17 papers divided in six groups (prepared between 01.07.2020 and 31.01.2022):

Roasting (Thermal Decomposition and Kinetics of Pentlandite-Bearing Ore Oxidation in the Air Atmosphere).
Leaching (1.Processing Tests, Adjusted Cost Models and the Economies of Reprocessing Copper Mine Tailings in Chile; 2. NdFeB Magnets Recycling Process: An Alternative Method to Produce Mixed Rare Earth Oxide from Scrap NdFeB Magnets; and 3. Electrochemical Investigation of Lateritic Ore Leaching Solutions for Ni and Co Ions Extraction).
Purification of solution during adsorption, precipitation and neutralization (1. Selenate Adsorption from Water Using the Hydrous Iron Oxide-Impregnated Hybrid Polymer; 2. Synergism Red Mud-Acid Mine Drainage as a Sustainable Solution for Neutralizing and Immobilizing Hazardous Elements; and 3. Basic Sulfate Precipitation of Zirconium from Sulfuric Acid Leach Solution).
Electrochemical methods for metal refining and winning (1. Electrorefining Process of the Non-Commercial Copper Anodes and 2. Aluminium Recycling in Single- and Multiple-Capillary Laboratory Electrolysis Cells).
Synthesis of metallic, oxidic and composite methods using different methods (1. One Step Production of Silver-Copper (AgCu) Nanoparticles; 2. Synthesis of Silica Particles Using Ultrasonic Spray Pyrolysis Method; 3. Atomic Layer Deposition of a TiO₂ Layer on Nitinol and Its Corrosion Resistance in a Simulated Body Fluid; 4. Spray-Pyrolytic Tunable Structures of Mn Oxides-Based Composites for Electrocatalytic Activity Improvement in Oxygen Reduction;’ 5. Mixed Oxides NiO/ZnO/Al₂O₃ Synthesized in a Single Step via Ultrasonic Spray Pyrolysis (USP) Method); and 6. Synthesis and Characterization of a Metal Catalyst prepared by Ultrasonic Spray Pyrolysis as Pre-Definition Step for Titanium oxide- supported Platinum).
Characterisation and behaviour of the produced materials (Microstructural and Cavitation Erosion Behavior of the CuAlNi Shape Memory Alloy).

Finally, the combined processes for the winning of rare earth elements and their oxides from primary and secondary materials were presented in a review paper: Advances in Understanding of the Application of Unit Operations in Metallurgy of Rare Earth Elements, prepared by B. Friedrich and S. Stopic.

This new SI will be connected with the previous, and will present new information not only about previously mentioned operations but also other important metallurgical operations (solvent extraction, dry digestion, bioleaching, etc.).

Dr. Srecko Stopic
Prof. Dr. Bernd Friedrich
Guest Editors

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Publisher’s notice:

As stated above, the central purpose of this Special Issue is to present research from "Non-ferrous Extractive Metallurgy". Given this purpose, the Guest Editor's contribution to this Special Issue may be greater than outlined in MDPI’s Special Issue guidelines (https://www.mdpi.com/special_issues_guidelines). The Editorial Office and Editor-in-Chief of Metals has approved this Topic and MDPI’s standard manuscript editorial processing procedure (https://www.mdpi.com/editorial_process) will be applied to all submissions. As per our standard procedure, Guest Editors are excluded from participating in the editorial process for their submission and/or for submissions from persons with whom a potential conflict of interest may exist. More details on MDPI’s Conflict of Interest policy for reviewers and editors can be found here: https://www.mdpi.com/ethics#_bookmark22.

Keywords

hydrometallurgy
pyrometallurgy
electrometallurgy
leaching
digestion
solvent extraction
precipitation
electrolysis
molten salt electrolysis
cementation
roasting
smelting
refining
ultrasonic spray pyrolysis
microwave leaching
recycling

Published Papers (11 papers)

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Editorial

Jump to: Research, Review

6 pages, 387 KiB

Open AccessEditorial

Advances in Understanding of Unit Operations in Non-Ferrous Extractive Metallurgy in 2023

by Srecko Stopic and Bernd Friedrich

Metals 2024, 14(3), 304; https://doi.org/10.3390/met14030304 - 04 Mar 2024

Viewed by 879

Abstract

Metallic materials play a vital role in the economic life of modern societies; hence, research contributions are sought on fresh developments that enhance our understanding of the fundamental aspects of the relationships between processing, properties, and microstructures. Disciplines in the metallurgical field ranging from processing, mechanical behavior, phase transitions, microstructural evolution, and nanostructures, as well as unique metallic properties, inspire general and scholarly interest among the scientific community. Three of the most important elements are included in unit operations in non-ferrous extractive metallurgy: (1) hydrometallurgy (leaching under atmospheric and high-pressure conditions, mixing of a solution with a gas and mechanical parts, neutralization of a solution, precipitation and cementation of metals from a solution aiming at purification, and compound productions during crystallization), (2) pyrometallurgy (roasting, smelting, and refining), and (3) electrometallurgy (aqueous electrolysis and molten salt electrolysis). Advances in our understanding of unit operations in non-ferrous extractive metallurgy are required to develop new research strategies for the treatment of primary and secondary materials and their application in industry. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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Research

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21 pages, 6593 KiB

Open AccessArticle

Influence of Process Parameters in Three-Stage Purification of Aluminate Solution and Aluminum Hydroxide

by Vladimir Damjanovic, Radislav Filipovic, Zoran Obrenovic, Mitar Perusic, Dusko Kostic, Slavko Smiljanic and Srecko Stopic

Metals 2023, 13(11), 1816; https://doi.org/10.3390/met13111816 - 27 Oct 2023

Viewed by 938

Abstract

The influence of process parameters in the three-stage purification of aluminate solution from the Bayer process and aluminum hydroxide was considered in this paper. One of the ways of purification is treating the aluminate solution in order to reduce the concentrations in the starting raw material (solution) and then treating the aluminum hydroxide at a certain temperature and time in order to obtain an alumina precursor of adequate quality. The purification process itself is divided into three phases. The first phase involves the treatment of sodium aluminate with lime in order to primarily remove Ca²⁺ and (SiO₃)²⁻ impurities. Phase II aims to remove impurities of Zn²⁺, Fe²⁺, and Cu²⁺ by treatment with controlled precipitation using specially prepared crystallization centers. In Phase III, Na⁺ is removed by the process of hydrothermal washing of Al₂O₃ ∙ 3H₂O. In this work, parameters such as temperature (T), reaction time (t), and concentration of lime (c) were studied in order to remove the mentioned impurities and obtain the purest possible product that would be an adequate precursor for special types of alumina. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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14 pages, 6548 KiB

Open AccessArticle

Transformation of Iron (III) Nitrate from an Aerosol by Ultrasonic Spray Pyrolysis and Hydrogen Reduction

by Srecko Stopic, Ayadjenou Humphrey Hounsinou, Koffi Aka Stéphane, Tatjana Volkov Husovic, Elif Emil-Kaya and Bernd Friedrich

Metals 2023, 13(10), 1686; https://doi.org/10.3390/met13101686 - 02 Oct 2023

Viewed by 1135

Abstract

Due to their unique properties, iron nanoparticles find diverse applications across various fields, including catalysis, electronics, wastewater treatment, and energy storage. Nano-iron particles are mostly sub-micrometer particles that are highly reactive to both air (oxygen) and water, and in nanoparticles (size below 100 nm), it is even more rapid than the bulk material. This characteristic limits its use in inert environments. Iron nanoparticles are not toxic and are mostly used for wastewater treatment. Understanding the hydrogen reduction mechanisms and conditions that lead to the formation of metallic iron particles from iron (III)-nitrate from an aerosol is crucial for enabling their effective utilization. In this work, we studied the hydrogen reduction behavior of Fe₂O₃ in the absence and presence of additives (SiO₂ or Pt). The particles were prepared via ultrasonic spray pyrolysis and hydrogen reduction. The characterization was performed with a scanning electron microscope, energy-dispersive X-ray spectroscopy, and X-ray diffraction. In the absence of additives, the oxygen content of iron oxide particles decreased with increasing temperature from 700 to 950 °C but significantly increased with the doping of 10 mL (40 wt.%) of SiO₂. The inhibitory effect of Si on the hydrogen reduction of Fe₂O₃ formed was more pronounced at 950 °C than at 700 °C. In contrast, the doping of only 5 mL (15 wt.%) of Pt significantly decreased the oxygen concentration in the synthesized particles by catalyzing the reduction reaction of iron oxides at 700 °C. The metallic iron (Fe) product, obtained in the undoped iron oxides run at only 950 °C, was also formed at 700 °C in the Pt-doped Fe₂O₃ run. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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13 pages, 5050 KiB

Open AccessArticle

Feasibility of Recovering Valuable and Toxic Metals from Copper Slag Using Iron-Containing Additives

by Aleksandar M. Mitrašinović, Yang Yuankun, Srecko Stopic and Milinko Radosavljević

Metals 2023, 13(8), 1467; https://doi.org/10.3390/met13081467 - 15 Aug 2023

Viewed by 1119

Abstract

One of the greatest environmental challenges in metal extraction is the generation of a large amount of slag. Most of these slags contain insufficient amounts of valuable metals for economical revalorization, but these concentrations may be harmful for the environment. At present, more than 80% of the global copper products are obtained by the smelting process, where the major by-products are various slags containing a broad range of almost all known elements. In this study, valuable and potentially harmful elements were recovered from mining waste using gravity separation and gravity settling. The settling process was enhanced by injecting coke, ferrocarbon, ferrosilicon, and ferrosulfide. In total, 35 elements were detected in the samples using electron probe microanalysis. After the treatment, 89.4% of the valuable, toxic, and trace elements gathered in the newly formed matte after maintaining the copper slag for four hours at 1300 °C and adding ferrosilicon. The metallic constituents of slags could be an important source of raw materials and they could be considered an environmentally beneficial source of copper and other materials. Suggested practices can prevent harmful elements from entering the environment, generate value from the gathered metals, and make the remaining slag suitable for construction or mine backfill materials. The present article also assesses the challenges in slag processing by the pyrometallurgical route and provides a roadmap for further investigations and large-scale studies. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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12 pages, 2061 KiB

Open AccessArticle

Recovery of Rare Earth Elements from Spent NdFeB Magnets: Metal Extraction by Molten Salt Electrolysis (Third Part)

by Hanwen Chung, Laras Prasakti, Srecko R. Stopic, Dominic Feldhaus, Vesna S. Cvetković and Bernd Friedrich

Metals 2023, 13(3), 559; https://doi.org/10.3390/met13030559 - 10 Mar 2023

Cited by 1 | Viewed by 1823

Abstract

The results obtained from the work on a concept of a recycling process for NdFeB magnets to recover rare earth elements for remanufacturing similar magnets are presented. This paper investigates the viability of extracting rare earth metals from magnet recycling-derived oxide (MRDO) by means of molten salt electrolysis. The MRDO was produced from spent NdFeB magnets through oxidation in air and subsequently carbothermic reduction under an 80 mbar Ar gas atmosphere. This MRDO contained roughly 33 wt.% Nd and 10 wt.% Pr. The electrochemical reduction process of the MRDO on molybdenum electrodes in NdF₃ + LiF and NdF₃ + PrF₃ + LiF fused salts systems was investigated by cyclic voltammetry and chronoamperometry measurements. The resulting electrolytes and electrodes were examined after potentiostatic deposition by scanning electron microscopy (SEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), and X-ray diffraction (XRD) analysis. The electrodeposited metals appeared to accumulate on the cathode and X-ray diffraction analysis confirmed the formation of metallic Nd and Pr on the working substrate. The suitability of the obtained alloy intended for the remanufacturing of NdFeB magnets was then evaluated. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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13 pages, 26613 KiB

Open AccessArticle

Research of the Process of Purification of Sulfate Zinc Solution from Iron Ions Using Anodic Oxidation

by Lyazat Liakyn, Zhanar Onalbayeva, Natalya Kulenova, Gulzhan Daumova, Sergey Mamyachenkov and Olga Anisimova

Metals 2023, 13(1), 88; https://doi.org/10.3390/met13010088 - 31 Dec 2022

Cited by 1 | Viewed by 1500

Abstract

The possibility of using a membrane electrolytic cell for the electrochemical oxidation of Fe(II) and purification from impurities of real industrial solutions obtained by atmospheric leaching of low-grade zinc concentrates is considered. The average indicators for carrying out the electrooxidation process are given. The principal possibility of conditioning a zinc sulfate solution by hydrolytic purification with preliminary oxidation of iron in a membrane electrolytic cell with an anion-exchange membrane MA-41 TU 2255-062-05761695-2009 is considered. Carrying out direct electrooxidation of iron (II) in sulfate zinc solutions in the anode chamber of a flow membrane electrolyzer ensures good filterability of precipitates after hydrolytic precipitation of iron, since this solution does not contain Fe(II) ions, the presence of which leads to significant difficulties in the operations of separating solid and liquid phases. This makes it possible to exclude the thickening operation from the technological scheme. The degree of oxidation of iron during the test period was 99.8–99.9%. The residual concentration of iron after precipitation from solutions obtained after electrochemical oxidation in the form of oxide and hydroxide compounds was less than 0.01 g/dm³. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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23 pages, 4512 KiB

Open AccessArticle

A Multifocal Study Investigation of Pyrolyzed Printed Circuit Board Leaching

by Gvozden Jovanović, Mladen Bugarčić, Nela Petronijević, Srecko R. Stopic, Bernd Friedrich, Branislav Marković, Srđan Stanković and Miroslav Sokić

Metals 2022, 12(12), 2021; https://doi.org/10.3390/met12122021 - 25 Nov 2022

Cited by 1 | Viewed by 1257

Abstract

Electric waste from numerous devices that are put out of use every day has some form of printed circuit board that contains precious and valuable metals in their components. In order to extract these metals, the printed circuit boards were crushed and pyrolyzed into powder. The fine pyrolyzed printed circuit board (PPCB) powder was separated into fractions, and the fine metallic fraction was used as a raw material for metal leaching extraction. In order to better understand how various metal species react in leaching media, several leaching agents were used (sulfuric acid, nitric acid, glycine, and acid mine drainage-AMD) alone, and with the addition of hydrogen peroxide. Additionally, the influence of the S/L ratio and leaching temperature were investigated in sulfuric acid leaching solutions, as this is the one most widely used. In one case, the reactor was heated in a thermal bath, while in the other, it was heated in an ultrasonic bath. Lastly, several experiments were conducted with a (consecutive) two-pronged leaching approach, with and without applied pretreatment. The aim of this paper is to give a multifocal and detailed approach to how metals such as Al, Cu, Co, Zn, Sn, and Ca behave when extracted from fine PPCB powder. However, some attention is given to Nd, Pd, Pb, and Ba as well. One of the main findings is that regardless of the pretreatment or the sequence of leaching media applied, consecutive two-pronged leaching cannot be used for selective metal extraction. However, AMD was found to be suitable for selective leaching with very limited applications. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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15 pages, 9482 KiB

Open AccessArticle

Synthesis of Complex Concentrated Nanoparticles by Ultrasonic Spray Pyrolysis and Lyophilisation

by Lidija Simić, Srecko Stopic, Bernd Friedrich, Matej Zadravec, Žiga Jelen, Rajko Bobovnik, Ivan Anžel and Rebeka Rudolf

Metals 2022, 12(11), 1802; https://doi.org/10.3390/met12111802 - 24 Oct 2022

Cited by 3 | Viewed by 1377

Abstract

The development of new multicomponent nanoparticles is gaining increasing importance due to their specific functional properties, i.e., synthesised new complex concentrated nanoparticles (CCNPs) in the form of powder using ultrasonic spray pyrolysis (USP) and lyophilisation from the initial cast Ag₂₀Pd₂₀Pt₂₀Cu₂₀Ni₂₀ alloy, which was in the function of the material after its catalytic abilities had been exhausted. Hydrometallurgical treatment was used to dissolve the cast alloy, from which the USP precursor was prepared. As a consequence of the incomplete dissolution of the cast alloy and the formation of Pt and Ni complexes, it was found that the complete recycling of the alloy is not possible. A microstructural examination of the synthesised CCNPs showed that round and mostly spherical (not 100%) nanoparticles were formed, with an average diameter of 200 nm. Research has shown that CCNPs belong to the group with medium entropy characteristics. A mechanism for the formation of CCNPs is proposed, based on the thermochemical analysis of element reduction with the help of H₂ and based on the mixing enthalpy of binary systems. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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13 pages, 5327 KiB

Open AccessArticle

Recovery of Rare Earth Elements from Spent NdFeB-Magnets: Separation of Iron through Reductive Smelting of the Oxidized Material (Second Part)

by Hanwen Chung, Srecko Stopic, Elif Emil-Kaya, Sebahattin Gürmen and Bernd Friedrich

Metals 2022, 12(10), 1615; https://doi.org/10.3390/met12101615 - 27 Sep 2022

Cited by 7 | Viewed by 2194

Abstract

This paper proposes a pyrometallurgical recycling method for end-of-life NdFeB magnets by oxidizing them in air and subsequently smelting them. The smelting process enabled the recovery of rare earth elements (REEs), producing a new reach concentrate separating the iron as a metallic phase. From the products of smelting, the metallic phase showed a maximum Fe content of 92.3 wt.%, while the slag phase showed a maximum total REE (Nd, Pr, and Dy) content of 47.47 wt.%, both at a smelting temperature of 1500 °C. ICE-OES and XRD analysis were conducted on both phases, and results showed that the metal phase consists mainly of Fe and Fe₃C while the slag phase consists of the RE-oxides, leftover Fe₂O_3, and a mixture of Fe₆Nd_4. The obtained slag concentrate based on the oxides of rare earth elements is suitable for further pyrometallurgical or hydrometallurgical treatment in order to obtain rare earth elements. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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12 pages, 2809 KiB

Open AccessArticle

Recovery of Rare Earth Elements through Spent NdFeB Magnet Oxidation (First Part)

by Srecko Stopic, Buse Polat, Hanwen Chung, Elif Emil-Kaya, Slavko Smiljanić, Sebahattin Gürmen and Bernd Friedrich

Metals 2022, 12(9), 1464; https://doi.org/10.3390/met12091464 - 31 Aug 2022

Cited by 11 | Viewed by 3004

Abstract

Due to their remarkable magnetic properties, such as a high maximum energy product, high remanence, and high coercivity, NdFeB magnets are used in a variety of technological applications. Because of their very limited recycling, high numbers of spent NdFeB magnets are widely available in the market. In addition to China’s monopoly on the supply of most rare earth elements, there is a need for the recovery of these critical metals, as their high import price poses an economic and environmental challenge for manufacturers. This paper proposes a pyrometallurgical recycling method for end-of-life NdFeB magnets by oxidizing them in air as first required step. The main goal of this method is to oxidize rare earth elements from NdFeB magnets in order to prepare them for the carbothermic reduction. The experimental conditions, such as the oxidation temperature and time, were studied in order to establish the phase transformation during oxidation using the Factsage Database and experimental conditions. Our thermogravimetric analysis TGA analysis revealed an increased sample mass by 35% between room temperature and 1100 °C, which is very close to the total calculated theoretical value of oxygen (36.8% for all elements, and only 3.6% for rare earth elements REE), confirming the complete oxidation of the material. The obtained quantitative analysis of the oxidation product, in (%), demonstrated values of 53.41 Fe₂O₃, 10.37 Fe₃O₄; 16.45 NdFeO₃; 0.45 Nd₂O₃, 1.28 Dy₂O₃, 1.07 Pr₂O₃, and 5.22 α-Fe. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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Review

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12 pages, 1354 KiB

Open AccessReview

Options for Hydrometallurgical Treatment of Ni-Co Lateritic Ores for Sustainable Supply of Nickel and Cobalt for European Battery Industry from South-Eastern Europe and Turkey

by Srđan Stanković, Željko Kamberović, Bernd Friedrich, Srećko R. Stopić, Miroslav Sokić, Branislav Marković and Axel Schippers

Metals 2022, 12(5), 807; https://doi.org/10.3390/met12050807 - 07 May 2022

Cited by 3 | Viewed by 3875

Abstract

The automotive industry is in the process of transformation from the traditional production of vehicles with engines powered by the combustion of fossil fuels to vehicles powered by electric energy. This revolutionary transformation will generate a growing demand for metallic raw materials that are a crucial part of batteries—nickel and cobalt, among others. Providing enough raw materials for e-mobility in a sustainable way will be a challenge in the years to come. The region of South-Eastern Europe (SEE) and Turkey is relatively rich in lateritic Ni-Co deposits, and this region has the potential to partially replace the import of nickel and cobalt intermediates to the European Union from distant overseas locations. Possibilities for the sustainable sourcing of nickel and cobalt from the SEE region are reviewed in this paper, with an overview of the global demand and production of these metals, lateritic mineral resources of SEE, the current status of production, and the prospective development of nickel and cobalt production in this region. Full article

(This article belongs to the Special Issue Advances in Understanding of Unit Operations in Non-ferrous Extractive Metallurgy 2023)

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