Research

10 pages, 3333 KiB

Open AccessArticle

Iron Removal from Metallurgical Grade Silicon Melts Using Synthetic Slags and Oxygen Injection

by Xiao Long, Wenbo Luo, Guohong Lu, Falou Chen, Xiaoning Zheng, Xingfan Zhao and Shaolei Long

Materials 2022, 15(17), 6042; https://doi.org/10.3390/ma15176042 - 01 Sep 2022

Cited by 1 | Viewed by 1217

Abstract

Novel SiO₂-CaO-CaF₂-R₂O-MgO based synthetic slags (R₂O represents alkali metal oxides) with varied binary basicity values were used with oxygen injection to refine silicon melts and remove Fe from metallurgical-grade silicon. Silicon samples and slags at [...] Read more.

Novel SiO₂-CaO-CaF₂-R₂O-MgO based synthetic slags (R₂O represents alkali metal oxides) with varied binary basicity values were used with oxygen injection to refine silicon melts and remove Fe from metallurgical-grade silicon. Silicon samples and slags at the silicon-slag interfaces were obtained during refinement. The compositions of the silicon samples were analyzed, and the quenched slag samples and mild cooling slags from the final crucible were inspected using scanning electron microscopy and energy dispersive X-ray spectroscopy. After 15 min of refinement, the Fe removal rate ranged from 52.3 to 60.1 wt%. During the refining process, the Fe-concentrated phase formed within the silicon droplets and was then transferred to the silicon-slag interfaces and wetted with slags. The Fe-concentrated phase at the silicon-slag interface can dissolve directly in the slags. It can also be transferred into the slag phase in the form of droplets, which can be affected by the binary basicity of the slags. Ti removal demonstrated a similar mechanism. Fe-bearing crystals were not detected in the quenched slag samples obtained during refinement, while complex Fe-bearing phases were detected in the final slag. This study demonstrates Fe removal from metallurgical-grade Si using slag refining methods and reveals the removal mechanism during the refinement. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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10 pages, 5196 KiB

Open AccessArticle

Recovery and Separation of Dysprosium from Waste Neodymium Magnets through Cyphos IL 104 Extraction

by Wei-Sheng Chen, Guo-Cai Jian and Cheng-Han Lee

Materials 2022, 15(15), 5281; https://doi.org/10.3390/ma15155281 - 30 Jul 2022

Cited by 1 | Viewed by 1219

Abstract

In the present study, the extraction of rare earth elements (REEs) from waste neodymium magnets using phosphorus ionic liquid Cyphos IL 104 was investigated. The objective was to recover and separate the heavy REE (Dy) from light REEs (Nd and Pr). Therefore, the [...] Read more.

In the present study, the extraction of rare earth elements (REEs) from waste neodymium magnets using phosphorus ionic liquid Cyphos IL 104 was investigated. The objective was to recover and separate the heavy REE (Dy) from light REEs (Nd and Pr). Therefore, the experimental parameters of ionic liquid extraction, including contacting time, the initial pH value, extractant concentration, and O/A ratio, have been optimized. The highest separation factor α_Dy/Nd of 45.18 and α_Dy/Pr of 47.93 has been achieved. Following the ionic liquid extraction, the comparison of different stripping agents and the stripping parameters (the concentration of stripping agent and A/O ratio) were also explored. In short terms, this research demonstrates the optimal parameters of Cyphos IL 104 for selectively extracting high REE (Dy) and reveals its potential for recovering and separating REEs in real waste. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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12 pages, 8681 KiB

Open AccessArticle

Impact of Rotor Material Wear on the Aluminum Refining Process

by Tomáš Prášil, Ladislav Socha, Karel Gryc, Jana Svizelová, Mariola Saternus, Tomasz Merder, Jacek Pieprzyca and Martin Gráf

Materials 2022, 15(13), 4425; https://doi.org/10.3390/ma15134425 - 23 Jun 2022

Cited by 2 | Viewed by 1400

Abstract

The paper presents the results of tests carried out during the refining of the AlSi9Cu3(Fe) alloy in industrial conditions at the FDU stand. In the tests, three different rotors made of classical graphite, fine-grained graphite and classical graphite with SiC spraying were tested [...] Read more.

The paper presents the results of tests carried out during the refining of the AlSi9Cu3(Fe) alloy in industrial conditions at the FDU stand. In the tests, three different rotors made of classical graphite, fine-grained graphite and classical graphite with SiC spraying were tested for the degree of wear. A series of tests was conducted for five cases—0% to 100% of consumption every 25%—corresponding to the cycles of the refining process. The number of cycles corresponding to 100% wear of each rotor was determined as 1112. The results of the rotor wear profile for all types of graphite after the assumed cycles are presented. Comparison of CAD models of new rotors and 3D scans of rotors in the final stage of operation revealed material losses during operational tests. The study assessed the efficiency of the rotor in terms of its service life as well as work efficiency. It was estimated on the basis of the calculated values of the Dichte Index (DI) and the density of the samples solidified in the vacuum. The structure of samples before and after refining at various stages of rotor wear is also presented, and the results are discussed. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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16 pages, 3939 KiB

Open AccessArticle

Recycling Vanadium and Proton-Exchange Membranes from Waste Vanadium Flow Batteries through Ion Exchange and Recast Methods

by Wei-Sheng Chen, Yu-An Chen, Cheng-Han Lee and Yen-Jung Chen

Materials 2022, 15(11), 3749; https://doi.org/10.3390/ma15113749 - 24 May 2022

Cited by 2 | Viewed by 1560

Abstract

This study aims to provide a system to recycle vanadium resources and recover membranes from waste proton-exchange membranes. This research is divided into two parts. To begin, ion exchange batch and column experiments were applied to adsorb vanadium in a membrane. In this [...] Read more.

This study aims to provide a system to recycle vanadium resources and recover membranes from waste proton-exchange membranes. This research is divided into two parts. To begin, ion exchange batch and column experiments were applied to adsorb vanadium in a membrane. In this process, the waste membrane was initially dissolved in a 50% ethanol solution, and the suspension obtained by dispersing the membrane had 74 mg/L of vanadium. Then, Dowex G26 resin was used to adsorb vanadium from the membrane dispersion in the ion-exchange process. The adsorptive behavior and optimal parameters were explored in this study. The vanadium ions were then eluted by HCl to obtain an enrichment solution, and the V₂O₅ was received through precipitation and calcination methods. After obtaining the vanadium-free dispersion, the recycled membrane was prepared by recasting it in the second part. The characteristics of the recycled membrane, such as the moisture, FTIR spectra, ion-exchange capacity, and ion conductivity, are discussed. The results revealed that the adsorption capacity of vanadium through Dowex G26 was 81.86 mg/g. The eluting efficiency of HCl was 97.5%, and the optimal parameters of the precipitation and calcination processes were set as pH 5, NH₄Cl:V = 2:1, and 350 °C. The moisture of the recycled membrane was 25.98%, and the IEC was 0.565 meq/g. The consequences of FTIR and ion conductivity demonstrated that the vanadium in the recycled membrane was eliminated by the ion-exchange method; however, the microstructure of the recycled membrane was influenced during ion exchange and recasting. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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13 pages, 6803 KiB

Open AccessArticle

Modelling of the Flow in the Process of Washing Out Automotive Catalyst Carriers with the PbLi Alloy

by Mariola Saternus, Agnieszka Fornalczyk, Władysław Gąsior, Adam Dębski, Sylwia Terlicka, Sławomir Golak and Piotr Ciepliński

Materials 2022, 15(9), 3119; https://doi.org/10.3390/ma15093119 - 26 Apr 2022

Cited by 1 | Viewed by 1152

Abstract

The process of platinum recovery from used car catalysts is highly desirable for both economic and environmental reasons. From the many available methods of processing used car catalysts, the article conducted both numerical and experimental studies using a device based on the collector [...] Read more.

The process of platinum recovery from used car catalysts is highly desirable for both economic and environmental reasons. From the many available methods of processing used car catalysts, the article conducted both numerical and experimental studies using a device based on the collector metal method with lead as a modified medium through a magnetohydrodynamic pump for washing platinum from the channels of the ceramic catalyst carrier. It was assumed that lead alloys with the addition of lithium increase the extraction of platinum from thin catalytic layers and accelerate the platinum dissolution reaction in the Pb-Li alloy, which is the result of a greater affinity of lithium for platinum compared to lead. This assumption was verified by numerical simulations as well as laboratory tests. Tests were carried out for the secondary supply voltage range between 40 and 60 V and the catalyst flushing time between 240 and 480 s. Graphical results of the research were discussed. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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12 pages, 6478 KiB

Open AccessArticle

The Supported Boro-Additive Effect for the Selective Recovery of Dy Elements from Rare-Earth-Elements-Based Magnets

by Sangmin Park, Dae-Kyeom Kim, Javid Hussain, Myungsuk Song and Taek-Soo Kim

Materials 2022, 15(9), 3032; https://doi.org/10.3390/ma15093032 - 21 Apr 2022

Cited by 2 | Viewed by 1516

Abstract

Liquid metal extraction (LME) for recycling rare-earth elements from magnets is studied, in the present study, to examine its suitability as an environmentally friendly alternative for a circular economy. While Nd (neodymium) extraction efficiency can easily reach almost 100%, based on the high [...] Read more.

Liquid metal extraction (LME) for recycling rare-earth elements from magnets is studied, in the present study, to examine its suitability as an environmentally friendly alternative for a circular economy. While Nd (neodymium) extraction efficiency can easily reach almost 100%, based on the high reactivity of Mg (magnesium), Dy (dysprosium) extraction has been limited because of the Dy–Fe intermetallic phase as the main extractive bottleneck. In the present paper, the boro-additive effect is designed thermodynamically and examined in the ternary and quinary systems to improve the selectivity of recovery. Based on the strong chemical affinity between B (boron) and Fe, the effect of excess boron, which is produced by the depletion of B in FeB by Mg, successfully resulted in the formation of Fe₂B instead of Dy–Fe bonding. However, the growth of the Fe₂B layer, which is the reason for the isolated Mg, leads to the production of other byproducts, rare-earth borides (RB₄, R = Nd and Dy), as the side effect. By adjusting the ratio of FeB, the extraction efficiency of Dy over 12 h with FeB addition is improved to 80%, which is almost the same extraction efficiency of the conventional LME process over 24 h. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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16 pages, 8121 KiB

Open AccessArticle

Nitric Acid Dissolution of Tennantite, Chalcopyrite and Sphalerite in the Presence of Fe (III) Ions and FeS₂

by Oleg Dizer, Denis Rogozhnikov, Kirill Karimov, Evgeniy Kuzas and Alexey Suntsov

Materials 2022, 15(4), 1545; https://doi.org/10.3390/ma15041545 - 18 Feb 2022

Cited by 5 | Viewed by 1502

Abstract

This paper describes the nitric acid dissolution process of natural minerals such as tennantite, chalcopyrite and sphalerite, with the addition of Fe (III) ions and FeS₂. These minerals are typical for the ores of the Ural deposits. The effect of temperature, [...] Read more.

This paper describes the nitric acid dissolution process of natural minerals such as tennantite, chalcopyrite and sphalerite, with the addition of Fe (III) ions and FeS₂. These minerals are typical for the ores of the Ural deposits. The effect of temperature, nitric acid concentration, time, additions of Fe (III) ions and FeS₂ was studied. The highest dissolution degree of sulfide minerals (more than 90%) was observed at a nitric acid concentration of 6 mol/dm³, an experiment time of 60 min, a temperature of 80 °C, a concentration of Fe (III) ions of 16.5 g/dm³, and an addition of FeS₂ to the total mass minerals at 1.2:1 ratio. The most significant factors in the break-down of minerals were the nitric acid concentration, the concentration of Fe (III) ions and the amount of FeS₂. Simultaneous addition of Fe (III) ions and FeS₂ had the greatest effect on the leaching process. It was also established that FeS₂ can be an alternative catalytic surface for copper sulfide minerals during nitric acid leaching. This helps to reduce the influence of the passivation layer of elemental sulfur due to the galvanic linkage formed between the minerals, which was confirmed by SEM-EDX. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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9 pages, 2214 KiB

Open AccessArticle

Recovery of Tantalum and Manganese from Epoxy-Coated Solid Electrolyte Tantalum Capacitors through Selective Leaching and Chlorination Processes

by Wei-Sheng Chen, Chih-Yuan Hsiao and Cheng-Han Lee

Materials 2022, 15(2), 656; https://doi.org/10.3390/ma15020656 - 16 Jan 2022

Cited by 7 | Viewed by 1750

Abstract

Electronic products are ever growing in popularity, and tantalum capacitors are heavily used in small electronic products. Spent epoxy-coated solid electrolyte tantalum capacitors, containing about 22 wt.% of tantalum and 8 wt.% of manganese, were treated with selective leaching by hydrochloric acid and [...] Read more.

Electronic products are ever growing in popularity, and tantalum capacitors are heavily used in small electronic products. Spent epoxy-coated solid electrolyte tantalum capacitors, containing about 22 wt.% of tantalum and 8 wt.% of manganese, were treated with selective leaching by hydrochloric acid and chlorination after removing the epoxy resin, and the products converted, respectively, to Mn(OH)₂ and TaCl₅. The effects of acid type, acid concentration, liquid–solid ratio, and reaction time were investigated to dissolve the manganese. The optimal selective leaching conditions were determined as 3 mol/L of HCl, 40 mL/g at 25 °C for 32 min. Next, residues of selective leaching after washing and drying were heated with ferrous chloride to convert to pure TaCl₅. Mixing 48 wt.% of chloride and 52 wt.% of residues for a total of 5 g was conducted to complete the chlorination process in the tube furnace at 450 °C for 3 h. A total of 2.35 g of Ta was collected and the recovery of Ta achieved 94%. Finally, Mn(OH)₂ and TaCl₅ were separated and purified as the products. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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14 pages, 4086 KiB

Open AccessArticle

Modeling the Filler Phase Interaction with Solidification Front in Al(TiC) Composite Produced by the In Situ Method

by Dorota Kalisz, Paweł L. Żak and Olena Dan

Materials 2021, 14(24), 7560; https://doi.org/10.3390/ma14247560 - 09 Dec 2021

Viewed by 1114

Abstract

This paper presents simulation results of the interaction of TiC nanoparticle in liquid aluminum. The behavior of the TiC particle in the frontal interaction region stems from the operation of a system of such forces as gravity, viscous flow drag force, and Saffman [...] Read more.

This paper presents simulation results of the interaction of TiC nanoparticle in liquid aluminum. The behavior of the TiC particle in the frontal interaction region stems from the operation of a system of such forces as gravity, viscous flow drag force, and Saffman force. The difference in density between the TiC and the aluminum matrix makes the particle fall, regardless of the radius dimension; while the Saffman force—which accounts for the local velocity gradient of the liquid aluminum—causes that particles with the smallest radii considered in the calculations 6.4 × 10⁻⁸ m; 7 × 10⁻⁸ m; 7.75 × 10⁻⁸ m; 9.85 × 10⁻⁸ m are repelled from the solidification front and the particles with 15.03 × 10⁻⁸ m are attracted to it. The viscosity growth in the course of casting caused by the lowering temperature reduces this effect, though the trend is maintained. The degree to which the particle is attracted to the front clearly depends on the velocity gradient of the liquid phase. For a very small gradient of 0.00001 m/s, the particle is at its closest position relative to the front. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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18 pages, 6714 KiB

Open AccessArticle

Hydrothermal Treatment of Arsenopyrite Particles with CuSO₄ Solution

by Aleksei Kritskii and Stanislav Naboichenko

Materials 2021, 14(23), 7472; https://doi.org/10.3390/ma14237472 - 06 Dec 2021

Cited by 5 | Viewed by 1468

Abstract

The nature of the hydrothermal reaction between arsenopyrite particles (FeAsS) and copper sulfate solution (CuSO₄) was investigated in this study. The effects of temperature (443–523 K), CuSO₄ (0.08–0.96 mol/L) and H₂SO₄ (0.05–0.6 mol/L) concentrations, reaction time (1–120 [...] Read more.

The nature of the hydrothermal reaction between arsenopyrite particles (FeAsS) and copper sulfate solution (CuSO₄) was investigated in this study. The effects of temperature (443–523 K), CuSO₄ (0.08–0.96 mol/L) and H₂SO₄ (0.05–0.6 mol/L) concentrations, reaction time (1–120 min), stirring speed (40–100 rpm) and particle size (10–100 μm) on the FeAsS conversion were studied. The FeAsS conversion was significant at >503 K, and it is suggested that the reaction is characterized by the formation of a thin layer of metallic copper (Cu⁰) and elemental sulfur (S⁰) around the unreacted FeAsS core. The shrinking core model (SCM) was applied for describing the process kinetics, and the rate of the overall reaction was found to be controlled by product layer diffusion, while the overall process was divided into two stages: (Stage 1: mixed chemical reaction/product layer diffusion-controlled) interaction of FeAsS with CuSO₄ on the mineral’s surface with the formation of Cu¹⁺ and Fe²⁺ sulfates, arsenous acid, S⁰, and subsequent diffusion of the reagent (Cu²⁺) and products (As³⁺ and Fe²⁺) through the gradually forming layer of Cu⁰ and molten S⁰; (Stage 2: product layer diffusion-controlled) the subsequent interaction of CuSO₄ with FeAsS resulted in the formation of a denser and less porous Cu⁰ and S⁰ layer, which complicates the countercurrent diffusion of Cu²⁺, Cu¹⁺, and Fe²⁺ across the layer to the unreacted FeAsS core. The reaction orders with respect to CuSO₄ and H₂SO₄ were calculated as 0.41 and −0.45 for Stage 1 and 0.35 and −0.5 for Stage 2. The apparent activation energies of 91.67 and 56.69 kJ/mol were obtained for Stages 1 and 2, respectively. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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16 pages, 4381 KiB

Open AccessFeature PaperArticle

Kinetics of Zinc Evaporation from Aluminium Alloys Melted Using VIM and ISM Technologies

by Albert Smalcerz, Bartosz Wecki, Leszek Blacha, Jerzy Labaj, Maciej Jodkowski and Adrian Smagor

Materials 2021, 14(21), 6641; https://doi.org/10.3390/ma14216641 - 04 Nov 2021

Cited by 2 | Viewed by 1755

Abstract

Using a vacuum during the smelting and refining of alloys removes dissolved gasses, as well as impurities with high vapour pressure. When smelting is carried out in vacuum induction furnaces, the intensification of the discussed processes is achieved by intensive mixing of the [...] Read more.

Using a vacuum during the smelting and refining of alloys removes dissolved gasses, as well as impurities with high vapour pressure. When smelting is carried out in vacuum induction furnaces, the intensification of the discussed processes is achieved by intensive mixing of the bath, as well as an enhanced mass exchange surface (liquid metal surface) due to the formation of a meniscus. This is due to the electromagnetic field applied to the liquid metal. This study reports the removal of zinc from the Al-Zn alloy containing 6.3 wt.%. Zn. The experiments were carried out with the use of two types of metallurgical devices: the VIM and ISM furnaces. For the experiments carried out in the crucible induction furnace, reduction in the operating pressure in the furnace from 1000 Pa to 10 Pa, together with the increase in temperature from 953 K to 1103 K, is accompanied by a decrease in zinc content in the alloy from 6 to 96%, compared with the initial value. Simultaneously, the overall mass transfer coefficient k_Zn increases from 5.15 × 10⁻⁶ to −1.49 × 10⁻⁴ ms⁻¹. For the experiments carried out in the furnace with a cold crucible (T = 953 K), a reduction in the operating pressure in the furnace from 1000 Pa to 10 Pa resulted in a decrease in zinc content in the alloy from 18 to 80%, compared with the initial value. For comparison, the experiments carried out in the crucible induction furnace at 953 K showed a reduction in zinc content in the alloy from 6 to 50%, which means that more intense zinc evaporation is seen in the furnace with a cold crucible. Comparison of ISM and VIM technologies in the removal efficiency of the Al-Zn alloy indicates a higher removal efficiency using the first technology, which, using the same conditions, achieves 80% of the removal efficiency of the component. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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16 pages, 4371 KiB

Open AccessArticle

Studies on the Content of Selected Technology Critical Elements (Germanium, Tellurium and Thallium) in Electronic Waste

by Joanna Willner, Agnieszka Fornalczyk, Magdalena Jablonska-Czapla, Katarzyna Grygoyc and Marzena Rachwal

Materials 2021, 14(13), 3722; https://doi.org/10.3390/ma14133722 - 02 Jul 2021

Cited by 12 | Viewed by 2865

Abstract

The article draws attention to the problem of the presence of metals: germanium (Ge), tellurium (Te), thallium (Tl), and others (Cd, Ba, Co, Mn, Cr, Cu, Ni, Pb, Sr, and Zn) in selected waste of electrical and electronic equipment (WEEE). As a result [...] Read more.

The article draws attention to the problem of the presence of metals: germanium (Ge), tellurium (Te), thallium (Tl), and others (Cd, Ba, Co, Mn, Cr, Cu, Ni, Pb, Sr, and Zn) in selected waste of electrical and electronic equipment (WEEE). As a result of the growing demand for new technologies, the global consumption of TECs has also been increasing. Thus, the amount of metals in circulation, of which the impacts on the environment have not yet been fully understood, is constantly increasing. Due to the low content of these metals in WEEE, they are usually ignored during e-waste analyses. The main aim of this study was to determine the distribution of Ge, Te, and Tl (and other elements) in ground sieve fractions (1.0, 0.5, 0.2, and 0.1 mm) of selected electronic components (solar lamps, solar cell, LED TV screens, LCD screens, photoresistors, photodiodes, phototransistors) and to determine the possible tendency of the concentrations of these metals in fractions. This problem is particularly important because WEEE recycling processes (crushing, grinding, and even collection and transport operations) can lead to dispersion and migration of TCE pollutants into the environment. The quantitative composition of e-waste was identified and confirmed by ICP-MS, ICP-OES and SEM-EDS, and XRD analyses. It was found that Ge, Te, and Tl are concentrated in the finest fractions of ground e-waste, together with Cd and Cr, which may favor the migration of these pollutants in the form of dust during storage and processing of e-waste. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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14 pages, 2343 KiB

Open AccessArticle

On the Rate of Interaction of Sodium Borohydride with Platinum (IV) Chloride Complexes in Alkaline Media

by Magdalena Luty-Błocho, Marek Wojnicki, Edit Csapo and Krzysztof Fitzner

Materials 2021, 14(11), 3137; https://doi.org/10.3390/ma14113137 - 07 Jun 2021

Cited by 6 | Viewed by 2624

Abstract

In this work, sodium borohydride was used as a strong reductant of traces of platinum complex ions. The investigations of the kinetics of redox reaction between platinum(IV) chloride complex ions and sodium borohydride were carried out. For the first time, the kinetic experiments [...] Read more.

In this work, sodium borohydride was used as a strong reductant of traces of platinum complex ions. The investigations of the kinetics of redox reaction between platinum(IV) chloride complex ions and sodium borohydride were carried out. For the first time, the kinetic experiments were carried out in a basic medium (pH~13), which prevents NaBH₄ from decomposition and suppresses the release of hydrogen to the environment. The rate constants of Pt(IV) reduction to Pt(II) ions under different temperatures and concentrations of chloride ions conditions were determined. In alkaline solution (pH~13), the values of enthalpy and entropy of activation are 29.6 kJ/mol and –131 J/mol K. It was also found that oxygen dissolved in the solution strongly affects kinetics of the reduction process. Using collected results, the reduction mechanism was suggested. For the first time, the appearance of diborane as an intermediate product during Pt(IV) ions reduction was suggested. Moreover, the influence of oxygen present in the reacting solution on the rate of reduction reaction was also shown. Full article

(This article belongs to the Special Issue Research Progress on the Extractive Metallurgy)

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