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WO2025120065A1 - Injection de soufre dans des scories de plomb - Google Patents

Injection de soufre dans des scories de plomb Download PDF

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Publication number
WO2025120065A1
WO2025120065A1 PCT/EP2024/084888 EP2024084888W WO2025120065A1 WO 2025120065 A1 WO2025120065 A1 WO 2025120065A1 EP 2024084888 W EP2024084888 W EP 2024084888W WO 2025120065 A1 WO2025120065 A1 WO 2025120065A1
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WIPO (PCT)
Prior art keywords
slag
sulfur
process according
elemental sulfur
phase
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/EP2024/084888
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English (en)
Inventor
Tim Van Rompaey
Jeroen HEULENS
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Umicore NV SA
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Umicore NV SA
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Filing date
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Publication of WO2025120065A1 publication Critical patent/WO2025120065A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B3/00—General features in the manufacture of pig-iron
    • C21B3/04—Recovery of by-products, e.g. slag
    • C21B3/06—Treatment of liquid slag
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/02—Obtaining lead by dry processes
    • C22B13/025—Recovery from waste materials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0026—Pyrometallurgy
    • C22B15/0054—Slag, slime, speiss, or dross treating
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B2400/00—Treatment of slags originating from iron or steel processes
    • C21B2400/02—Physical or chemical treatment of slags
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the field of the present invention is the recovery of metals from Pb-bearing metallurgical slags.
  • a first step is often a smelting operation producing a Cu matte and a Pb-bearing slag. While a major part of the valuable metals reports to the Cu matte, an appreciable part of them also reports to the slag.
  • Such a slag may contain 20% by weight or more of Pb, together with metals such as Cu, Fe, and Zn. Further treatment is required to recover these valuable metals, especially Cu and Zn.
  • the slag is typically subjected to reducing conditions in a blast furnace or in an electric arc furnace to produce a metallic alloy containing the valuable metals, and a cleaned slag.
  • the required reducing conditions are obtained by adding carbon or carbohydrates to the furnace, in the form of cokes, or as a liquid or gaseous fuel.
  • the redox reactions lead to the formation of CO, and ultimately to CO2.
  • Yuan et al. (Powder Technology 230, 63-66, 2012) teaches the addition of sulfur to PbO. Intense cogrinding of the mixture at low temperature results in the partial conversion of Pb to PbS. The sulfides can be separated using flotation. The process may be applied to Pb-bearing wastes such as glasses, wherein Pb is present as an oxide.
  • CN116024438A describes the introduction of sulfur-containing vulcanizing agents in the form of gypsum, pyrite, or nickel sulfide ore to a molten Ni-rich slag to obtain, among others, a low nickel matte.
  • SO2 is relatively easy to capture. It can be converted to SO3, and then to sulfuric acid using a standard industrial process. Sulfuric acid is a widely used reactant, for example for manufacturing fertilizers. SO2 can also be converted to sulfur when the SO2 concentration in the off-gas is sufficiently high.
  • Environmentally friendly processes for example using the CaS - SO2 reaction (Environ. Sci. Technol. 2002, 36, 13, 3020-3024), have been developed to this end. In this way, a direct effect of the present scheme is the decarbonization of the industrial recovery process.
  • the new process results in the formation of a so-called matte, i.e. a sulfidic phase formed by metal sulfides, instead of the metallic phase, obtained when a traditional carbon-based reduction scheme is applied.
  • a first embodiment describes a process for the removal of Pb and Cu from a metallurgical slag, comprising the steps of:
  • molten bath comprising a slag phase depleted in Pb and Cu and a matte phase, SO2-bearing off-gas, and flue dust; and, - separating the matte phase from the slag phase.
  • elemental sulfur sulfur not combined with any chemical element other than sulfur itself.
  • This definition includes octasulfur (Sg), which is a major industrial form of elemental sulfur.
  • the metallurgical slags typically originate from industrial smelting and refining operations.
  • the most prominent metal in such slags is Pb. Amounts of between 20 and 40% are common. Therefore, in another embodiment, the metallurgical slag contains at most 40% of Pb by weight.
  • Amounts of more than 40% of Pb in such metallurgical slags are less common, as this would make the upstream processes less efficient. Amounts of less than 20% would make the slag viscosity too high and thus require additional fluxing agents.
  • the metallurgical slags according to the present invention typically originate from other industrial processes, in which the majority of the valuable copper has already been removed. Therefore, in another embodiment, the metallurgical slag contains 1 to 5% of Cu by weight. The upper limit of 5% characterizes "copper depleted" slags in contrast to other "copper rich” industrial slags, for which also other methods of refining may be more appropriate.
  • the metallurgical slag In addition to Pb and Cu, other metals, such as Fe, Ni, As, Bi, Sb, Sn and Zn can be present in the metallurgical slag. Therefore, in another embodiment, the metallurgical slag further contains one or more of Ni, As, Bi, Fe, Sb, Sn and Zn. Their respective percentages by weight are typically much lower than the above-mentioned amounts for Pb. All except Fe and Zn are considered as minor impurities with minor or no effect on the present process.
  • the metallurgical slag used at the start of the process can be referred to as "starting slag".
  • Fe will typically be present in an amount of at least 4% and at most 20% by weight in the starting slag. More common are amounts of 4 to 15%, or even 4 to 10%. Generally, Fe is seen as being uncritical and can report to the slag phase, typically in any of its oxide forms, or to the matte phase, typically as FeS. Nevertheless, amounts of more than 20% of iron are less preferred, as this would make the upstream recovery processes less efficient.
  • Zn will typically be present in an amount of at least 2% and at most 15% by weight in the starting slag. More common are amounts of 2 to 10%, or even 2 to 7%. High amounts of Zn are less desired, as Zn not only forms sulfides, but can also fume from the slag and report to the flue dust where it can lead to unwanted downstream condensation.
  • Fe and Zn if present in significant amounts, should be taken into account when estimating the amount of elemental sulfur to be added to the starting slag.
  • elemental sulfur to be added to the starting slag.
  • One reason forthat is that Fe and Zn have a higher chemical affinity for oxygen than for example Cu and Pb. Therefore, at the present process conditions of temperature and oxygen potential (pO2), the Fe and Zn, present in the initial metallurgical slag, will not convert fully to their respective metal sulfides, but they will remain partially in the depleted slag as metal oxides. It has been observed that an addition of sulfur corresponding to about 50% of the calculated stoichiometric amount for these two metals is sufficient in the present process.
  • metallurgical slags also contain slag formers.
  • Typical slag formers are silica (SiO2), alumina (AI2O3), calcium oxide (CaO) or magnesium oxide (MgO).
  • SiO2O3 silica
  • AI2O3 alumina
  • CaO calcium oxide
  • MgO magnesium oxide
  • such slag formers can typically be found in the following ranges:
  • magnesium oxide 0 to 10 % by weight of magnesium oxide.
  • Metallurgical slags may contain a combination of slag formers adding up to 40 to 60% by weight.
  • a slag containing a minimum of 40% of slag formers allows for a proper reaction with sulfur, and for an easy phase separation between slag phase and matte phase.
  • Lowering the amount of slag formers to less than 40%, or even to less than 30%, would result in overly concentrated metals, while increasing the amount of slag formers to more than 60%, or even to more than 70%, would result in a diluted overall composition, rendering the recovery of the metals uneconomical.
  • Metallurgical slags generally contain a rather complex mixture of slag formers and metals, typically in form of oxides. Moreover, other impurities can be present, such as P2O5, Na2O or BaO, largely depending on differences in the feed materials that have been used to produce the slag, and/or the applied process conditions.
  • the amounts of the different metals in the Pb-bearing slag are determined upfront by known analytical methods. Based on this, the required stoichiometric amount of sulfur can readily be derived from the above sulfidation reactions.
  • the calculated stoichiometric amount of sulfur is determined by the stoichiometric amount to convert 100% of Pb and Cu, and 50% of Fe and Zn to sulfides.
  • the kinetics of the sulfur reacting with metal oxides in the molten starting slag are limited. The kinetics depend, among others, on temperature and the intimacy of the mixing between the introduced sulfur and the metal oxides in the molten slag. Some sulfur will leave the molten slag unreacted, forming SO2 with any air present above the molten bath or further downstream in the gas cleaning circuit. To compensate for these losses and achieve the desired result of the present process, an excess of S is needed. It is thus required to add more than 100% of the calculated stoichiometric amount of sulfur, such as 110% or more, 120% or more, 130% or more, or 140% or more.
  • the amount of sulfur it is preferred to limit the amount of sulfur to at most 300%, preferably to at most 250%, more preferably to at most 200%, and most preferably to at most 150% of the calculated stoichiometric amount of sulfur.
  • limiting the excess of sulfur fed to the slag is advised due to the cost of the sulfur itself and also to avoid larger off-gas streams.
  • a preferred range for the amount of sulfur is therefore 120 to 150% of the calculated stoichiometric amount of sulfur.
  • Separating the matte phase from the slag phase is typically achieved by selective tapping, when both phases are still liquid. Alternatively, it is possible to tap both phases together, let them cool down and solidify, and separate them either mechanically or by flotation.
  • major part of an element is meant at least 50% by weight of the quantity of that element entering the process.
  • the furnace is an electric furnace.
  • electricity as a heat source, the need for carbon-based fuel is alleviated or eliminated. Assuming access to green electricity, the carbon footprint can thus remain remarkably low.
  • the furnace is a bath furnace or horizontal converter. This type of furnace lends itself well to the injection of sulfur, optionally using a carrier gas.
  • the partial pressure of oxygen, pO2 in a pyrometallurgical system affects the oxidation state and thermodynamic stability of the metal, slag and gas phases.
  • the pO2 is preferably in the range of 10’ ⁇ to lo
  • oxygen-bearing gasses such as air
  • a limited amount of oxygen can be useful if combined with an extra excess of sulfur, thus an additional amount beyond the calculated and required excess according to the above-mentioned stoichiometry for the conversion of metals to sulfides.
  • This additional excess of sulfur can be used as a heat source.
  • Non-reactive gasses such as nitrogen can be injected into the slag.
  • any amount of Pb reporting to the flue dust decreases the amount of Pb which can report to the matte phase. While other process conditions, such as amount of sulfur, amount of slag formers or temperature, remain the same, this alternative process step allows the skilled person not only to concentrate the Pb in the flue dust, but at the same time separating it from non-volatile other metals, such as copper or iron, which remain in the slag and/or matte phase.
  • Low operational temperatures around the melting point of a slag are preferred to limit refractory degradation in a furnace as much as possible.
  • operational temperatures are selected to avoid overheating of the slag too far above its melting point.
  • the operation temperature of the furnace is from 1150 to 1300 °C, preferably from 1180 to 1230 °C.
  • the elemental sulfur fed to the molten slag is in liquid form.
  • An advantage of using liquid sulfur is the established technology for its manipulation and transport in an industrial environment.
  • the liquid sulfur can be injected directly into the molten slag, having a positive impact on the process kinetics.
  • the elemental sulfur is fed by injection through one or more lances or tuyeres.
  • a lance is understood to be a tubular entity dipped from above into the molten bath.
  • a tuyere is understood to be a tubular entity piercing the wall or bottom of the furnace, below or above the level of the molten bath, and equipped with means for the injection of gasses, liquids or solids into the molten bath.
  • the sulfur fed to the molten slag is in the form of solid pellets or briquettes comprising elemental sulfur.
  • elemental sulfur is mixed with solid metallurgical slag of the same or similar composition as in the first embodiment, then pressed. Pressing increases the relative density of the pellets and improves the mixing of sulfur and metals in the molten bath of the furnace. This enhances the overall reactivity of the sulfur with those metals, making the process more efficient. Therefore, in another embodiment, the solid pellets comprising sulfur further comprise solid slag.
  • the solid slag used for making pellets has the same composition as the metallurgical slag according to the first embodiment.
  • the sulfur to slag ratio in this mixture has been tested, namely 4:1, 3:1, 2:1, 1:1, and 1:2.
  • a ratio of 2:1 is preferred. Therefore, in another embodiment, the sulfur to slag ratio in said pellets is from 4:1 to 1:2, preferably from 3:1 to 1:1, more preferably from 2.5:1 to 1.5:1.
  • PbS more than 80% of the Pb reports to the matte phase as PbS.
  • Pb remaining in the slag after addition of sulfur may result from insufficient addition of sulfur, ineffective reaction behavior between Pb in the molten slag and sulfur, unfavorable reaction kinetics and/or insufficient decantation in the step of separating the matte from the slag. The latter would result in Pb-containing matte droplets in the final/depleted slag and thus an overall higher than expected Pb-content in the slag, despite successful conversion to PbS.
  • the slag phase depleted in Pb and Cu contains less than 5% of Pb by weight, preferably less than 3%, and most preferably less than 2%.
  • the slag phase depleted in Pb- and Cu contains less than 0.5% of Cu by weight, preferably less than 0.25 %. It has been observed that Cu tends to react faster with the elemental sulfur than Pb. Therefore, very low concentrations of Cu have been observed in the final/depleted slag. Cu reports almost quantitatively to the matte phase as copper sulfide in the present process.
  • no carbon-based fuel or carbon-based reducing agent is added to the furnace. It is preferred to avoid the addition of carbon-based fuel or carbon-based reducing agent to the furnace. This would result in the formation of CO2, which is undesired when aiming at the decarbonization of the industrial recovery process. Moreover, CO2 is not only more difficult to capture than SO2, it would also make the recovery and re-use of SO2 more difficult due to diluting the latter.
  • the present process is further comprising a step of converting the SO2 from the SO2-bearing off-gas to H2SO4.
  • Modern industrial plants are often equipped with a conversion unit for the production of sulfuric acid.
  • the H2SO4 can for example be valorized or used in acidic leaching operations.
  • the present process is further comprising a step of converting the SO2 from the SO2-bearing off-gas to elemental sulfur.
  • An alternative to the production of sulfuric acid is the conversion of the SO2-bearing off-gas to elemental sulfur. This is particularly attractive in combination with an electric furnace, as the off-gas is not diluted by huge amounts of carbon-bearing off-gas, as it would be the case in furnaces burning fuel or cokes.
  • the higher concentration of SO2 in the off-gas of the present process facilitates this alternative conversion method.
  • the produced elemental sulfur can be re-used in the present process. Therefore, in another embodiment, the present process is further comprising a step of recirculating the elemental sulfur to the step of feeding elemental sulfur to the molten slag.
  • the present process is further comprising a step of recovering metals from the matte phase and/or from the flue dust.
  • Downstream refining processes of matte are known and can be combined with the present scheme.
  • One possibility for refining such a matte is to subject it to a converting process. This will produce a metallic phase, which then can be processed in the traditional way, and SO2, which can be captured and/or processed as explained above.
  • Other refining schemes are possible, e.g. using leaching or flotation.
  • S02 originating from a further refining of the obtained PbS and Cu2$-containing matte can be recovered and converted to either H2SO4 or elemental S in one of the above-mentioned conversion operations.
  • the total amount of sulfur added to the starting slag was doubled with respect to Example 1. 2625 g of starting slag with composition given in Table 2 was provided. The required stoichiometric amount of elemental sulfur for the sulfidation of this starting slag equals 420 g. In this example 250% of the required stoichiometric amount of sulfur was added to the starting slag, i.e. 1050 g.
  • Pellets containing both starting slag and sulfur were prepared.
  • the ratio sulfur to slag in this mixture was 2 to 1.
  • 525 g of starting slag was milled and sieved to below 2 mm.
  • the starting slag was mixed with 1050 g of elemental sulfur to prepare the briquetting mixture. From this mixture pellets were pressed.
  • a 1.5 I alumina crucible with 2100 g of starting slag was placed in an induction furnace and heated under an Argon atmosphere at 650 °C/h to a temperature of 1250 °C. Then, the sulfur-slag pellets were added in the course of 4 hours in regular intervals. At the end of the process, 1150 g of final slag and 1435 g of matte were present.
  • the composition of these phases is given in Table 2.
  • Pellets containing both starting slag and sulfur were prepared.
  • the ratio sulfur to slag in this mixture was 2 to 1.
  • 130 g of starting slag was milled and sieved to below 2 mm.
  • the starting slag was mixed with 260 g of elemental sulfur to prepare the briquetting mixture. From this mixture pellets were pressed.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne la récupération de métaux à partir de laitiers porteurs de Pb. Ce but est atteint par un procédé d'élimination de Pb et de Cu à partir d'un laitier métallurgique, comprenant les étapes consistant à : fournir un four de fusion ; fournir un laitier métallurgique contenant plus de 20 % en poids de Pb, et contenant en outre du Cu, du Fe et du Zn ; chauffer le laitier dans le four, ce qui permet d'obtenir un laitier fondu ; fournir une quantité de soufre élémentaire correspondant à au moins 110 % de la quantité stœchiométrique pour convertir 100 % de Pb et Cu, et 50 % de Fe et de Zn en sulfures ; introduire ladite quantité de soufre élémentaire dans le laitier fondu, ce qui permet d'obtenir un bain fondu comprenant une phase de laitier appauvrie en Pb et Cu et une phase mate, SO 2 -gaz de dégagement, et de la poussière de combustion ; et séparer la phase mate de la phase de laitier. Ce procédé offre un schéma alternatif pour la séparation et la récupération de métaux, en particulier Pb et Cu, à partir de scories par conversion de ceux-ci en sulfures métalliques. La substitution du carbone par du soufre entraîne la décarbonisation du processus de récupération industrielle.
PCT/EP2024/084888 2023-12-06 2024-12-05 Injection de soufre dans des scories de plomb Pending WO2025120065A1 (fr)

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EP23214650 2023-12-06
EP23214650.6 2023-12-06

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PCT/EP2024/085135 Pending WO2025120190A1 (fr) 2023-12-06 2024-12-06 Traitement de scories de plomb

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US3990889A (en) * 1973-05-03 1976-11-09 Q-S Oxygen Processes, Inc. Metallurgical process using oxygen
US5372630A (en) * 1990-11-14 1994-12-13 Mincorp Ltd Direct sulphidization fuming of zinc
CA3000805A1 (fr) * 2015-10-16 2017-04-20 Francisco Javier Cardenas Arbieto Procede d'extraction de metaux a partir des concentres de minerais sulfures les contenant par application d'une reduction directe avec regeneration et recyclage de l'agent reducte ur tel que du fer et du fondant tel que du carbonate de sodium
CA3055263A1 (fr) * 2017-04-10 2018-10-18 Metallo Belgium Procede ameliore de production de brasure brute
CN116024438A (zh) 2023-02-24 2023-04-28 浙江华友钴业股份有限公司 一种利用红土镍矿生产镍产品的方法

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DE112007001820B4 (de) 2006-08-01 2015-08-06 Outotec Oyj Bleischlackenreduzierung
JP7719771B2 (ja) 2019-11-22 2025-08-06 アウルビス ベーアセ 改善された銅製錬方法
CN113046550A (zh) 2021-03-11 2021-06-29 金川集团股份有限公司 一种用于降低贫化电炉渣中有价金属的硫化还原剂及其制备方法
CN113862489B (zh) 2021-09-26 2022-12-23 上海交通大学 一种低碳还原炼铅耦合碳富集的方法

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Publication number Priority date Publication date Assignee Title
US3990889A (en) * 1973-05-03 1976-11-09 Q-S Oxygen Processes, Inc. Metallurgical process using oxygen
US5372630A (en) * 1990-11-14 1994-12-13 Mincorp Ltd Direct sulphidization fuming of zinc
CA3000805A1 (fr) * 2015-10-16 2017-04-20 Francisco Javier Cardenas Arbieto Procede d'extraction de metaux a partir des concentres de minerais sulfures les contenant par application d'une reduction directe avec regeneration et recyclage de l'agent reducte ur tel que du fer et du fondant tel que du carbonate de sodium
CA3055263A1 (fr) * 2017-04-10 2018-10-18 Metallo Belgium Procede ameliore de production de brasure brute
CN116024438A (zh) 2023-02-24 2023-04-28 浙江华友钴业股份有限公司 一种利用红土镍矿生产镍产品的方法

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ENVIRON. SCI. TECHNOL., vol. 36, no. 13, 2002, pages 3020 - 3024
HAN ET AL.: "Selective Sulfidation of Lead Smelter Slag with Sulfur", METAL MATER TRANS B, vol. 47, 2016, pages 344 - 354, XP035944596, DOI: 10.1007/s11663-015-0526-4
VANPARYS ET AL.: "9th International Symposium on Lead and Zinc Processing. The Minerals, Metals & Materials Series", 2020, SPRINGER
YUAN ET AL., POWDER TECHNOLOGY, vol. 230, 2012, pages 63 - 66

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BE1032294A1 (nl) 2025-07-30
BE1032294B1 (nl) 2025-12-11

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