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WO2018109283A1 - Traitement de déchets industriels contenant des métaux - Google Patents

Traitement de déchets industriels contenant des métaux Download PDF

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Publication number
WO2018109283A1
WO2018109283A1 PCT/FI2017/050901 FI2017050901W WO2018109283A1 WO 2018109283 A1 WO2018109283 A1 WO 2018109283A1 FI 2017050901 W FI2017050901 W FI 2017050901W WO 2018109283 A1 WO2018109283 A1 WO 2018109283A1
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WO
WIPO (PCT)
Prior art keywords
solution
phase
metal
sulfides
process according
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.)
Ceased
Application number
PCT/FI2017/050901
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English (en)
Inventor
Pertti Koukkari
Jussi Rastas
Pekka Saikkonen
Väinö HINTIKKA
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VTT Technical Research Centre of Finland Ltd
Original Assignee
VTT Technical Research Centre of Finland Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by VTT Technical Research Centre of Finland Ltd filed Critical VTT Technical Research Centre of Finland Ltd
Priority to EP17880716.0A priority Critical patent/EP3555327A4/fr
Publication of WO2018109283A1 publication Critical patent/WO2018109283A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C22B7/02—Working-up flue dust
    • 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
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • 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
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
    • 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 present invention concerns the hydro metallurgical processing of industrial waste materials in order to separate fractions containing valuable metals therefrom.
  • the materials to be processed are obtained from the zinc or steel industries, or both.
  • Suitable waste materials that can be processed according to the invention, either separately or combined, are jarosite and goethite rejects of the zinc industry, as well as the zinc-containing dusts (such as electric arc furnace dusts, i.e. EAF dusts) of the steel industry.
  • the halogens are usually removed from the Walz oxide using a two- or three-fold wash with a Na 2 CC"3 solution, before the thus treated oxides can be fed to the electrolytic zinc process. It would pose a considerable advantage if the dusts of the steel industry could be processed in a manner facilitating early removal of halogens, taking place in a close vicinity to the zinc manufacturer.
  • valuable metals such as zinc, lead, iron, silver and gold
  • the suggested hydrometallurgical processing of the invention makes it possible to eliminate the halogen problem formed in connection with using the Walz process, while in a unique manner providing a procedure for the zinc industry for utilizing the jarosite precipitate, which has up to the present date been stored as hazardous waste, in connection with zinc production. Further, a concentrate containing significant amounts of lead, silver and gold is also obtained in the present process.
  • waste dust of the steel mills and jarosite or goethite waste of the zinc mills can be processed by hydrometallurgy, either separately or combined.
  • the products include the valuable metal fractions that these wastes contain, recovered as utilizable concentrates.
  • the invention provides an advantageous and environmentally friendly solution for recycling the zinc-containing waste dust of the steel mills in connection with the recovery of metals from the jarosite precipitate formed as a waste in the zinc mills.
  • FIGURE 1 is a block diagram illustrating the processing steps in accordance with at least some embodiments of the present invention.
  • FIGURE 2 is an alternative block diagram illustrating the process steps in accordance with at least one embodiment of the present invention.
  • the "hydrometallurgical processing" of the invention is intended to cover a multistep procedure for separating at least the valuable components from the starting material, i.e. the waste, the procedure including steps of acidifying, precipitating, concentrating and heat treating, as well as one or more steps of metals recovery.
  • waste is intended to cover all by-products of metal production industries, particularly the metal-containing by-products of the zinc and steel industries.
  • metal is intended to encompass the elements of the periodic table of elements that belong to the transition metals, post-transition metals and metalloids, the groups of transition and post-transition metals having the highest significance.
  • At least one precipitation step of said process is carried out using a "sulfur- containing chemical", which is intended to cover sulfates, sulfides, sulfur oxides and sulfites, which generate chemicals that easily can be reacted into a suitable form to be recycled, and optionally used in a sulfur dioxide treatment.
  • a sulfur- containing chemical which is intended to cover sulfates, sulfides, sulfur oxides and sulfites, which generate chemicals that easily can be reacted into a suitable form to be recycled, and optionally used in a sulfur dioxide treatment.
  • the process includes a series of precipitations using e.g. sulfur-containing chemicals selected from sulfates, sulfides, sulfur oxides and sulfites, and hydroxides, in order to obtain an aqueous sulfur-containing solution, which optionally is recycled in the process, whereafter a final precipitate is carried to a thermal step, for forming and separating solid oxides from the sulfates remaining in the solution phase.
  • Figure 1 illustrates a process scheme in accordance with an embodiment of the invention.
  • a sulfuric acid treatment using hot concentrated sulfuric acid is first carried out on an industrial zinc-containing dust, such as an electric arc furnace dust (an EAF dust).
  • an electric arc furnace dust an EAF dust
  • the acid is heated to a temperature of > 100°C, particularly to about 200°C, and is mixed with the preheated (e.g. 100-150°C) dust.
  • the temperature of the formed mixture then rises, typically to more than 250°C.
  • the oxides in the dust are sulfatized to form a sulfate phase, while the halogenides also contained therein are decomposed and sulfatized, generally at least to a degree of 70%.
  • the water and the halogen hydrides of the formed mixture are transferred to the gas phase, from where they can be removed, e.g. by compressing, preferably using water washing.
  • the reactions taking place in this process step include one or more, preferably all, of the following listing:
  • dehalogenated sulfatized dusts can be carried as such to be used in zinc processes.
  • the obtained solid sulfatized dust, optionally mixed with further metal- containing waste materials, such as jarosite and/or goethite waste, are fed to a S0 2 dissolution step.
  • the temperature during said dissolution step is preferably >50°C and
  • ⁇ 100°C most suitably about 90°C, whereby one or more of the reactions of the following listing take place, typically all of the reactions, as long as the relevant metals are present in the treated waste material.
  • This S0 2 solution phase is, according to the embodiment described in Fig. 1, processed further in later described steps, while the solid residue is carried to a
  • the dissolution residue is first suspended into water to form a slurry. Subsequently, sodium sulfide, or another similar sulfide reagent, is added to the sludge (see reactions (30) and (31)) in an amount equivalent to the lead and silver present in the residue, and the mixture is floated to give a first fraction of metal sulfides and a first S0 4 solution.
  • Typical products of this step are concentrates containing lead, silver and gold.
  • the remaining waste materials are preferably discarded as a sulfide waste residue, while the S0 4 solution can be recycled or combined with the previously obtained S0 2 solution.
  • the indium (In) and gallium (Ga), and possibly germanium (Ge) are separated from the S0 2 solution (optionally combined with the first S0 4 solution) by adjusting the pH to a level of 3.5-4, preferably using a solution containing magnesium hydroxide (Mg(OH) 2 ) as the pH adjustment agent (causing precipitation).
  • the temperature of the solution is between 80 and 90°C.
  • Other possible pH adjustment agents are zinc oxide (ZnO), Walz-oxide (or the ZnO therein), calcium oxide (CaO), calcium hydroxide (Ca(OH) 2 ) and calcium carbonate (CaC0 3 ).
  • this step can be called a hydroxide precipitation step.
  • the fractions obtained in this step are thus a second S0 4 solution and a solid phase containing a first residue of metal hydroxides.
  • solubility product values of the obtained hydroxides vary to some extent, depending on their source. If the solubility product values for the indium and gallium hydroxides are equal to or lower than 10(exp(-36)), and if the corresponding value for aluminium hydroxide is 10(exp(-31)), it is possible to obtain a sharp distinction. If the pH adjustment range is 3.5-4, the precipitate will, however, contain also aluminium hydroxide.
  • the precipitated hydroxides are separated from the second S0 4 solution, and are washed, whereby the washing solution can be added to the original second S0 4 solution.
  • the thus recovered precipitate will contain In, Ga, Ge and Al hydroxides.
  • the Indium, Gallium and Germanium can be separated using a liquid-liquid extraction.
  • the following step according to Fig. 1 is a sulfide precipitation, which is carried out by adding hydrogen sulfide (H 2 S) to the second S0 4 solution obtained in the previous step, while adjusting the pH of the solution, for example using Mg(OH) 2 , so that no significant amounts of iron (Fe 2+ ) is precipitated.
  • the reactions taking place during this step of the process preferably include the following:
  • This precipitate can then be treated further with a polysulfide solution, preferably an ammonium polysulfide solution, whereby the sulfides of the precipitate can be separated into a solid phase, containing a third fraction of metal sulfides, and a solution phase.
  • a polysulfide solution preferably an ammonium polysulfide solution
  • AS2S3, Sb 2 S3 and SnS dissolve as in the following reactions, whereas CuS, CdS and ZnS remain in solid form.
  • the obtained solid and solution phases are then separated, whereby the solid phase is washed using a solution based on ammonium polysulfide, and the washing solution is combined with the solution phase.
  • the solution phase and the dissolved metals therein are can then be treated by an addition of sulfuric acid, whereby the sulfides of arsenic, antimony and tin are precipitated (reactions (46) - (48)).
  • the solid residue obtained in the thermal step is preferably carried to a water washing step, where the soluble components are transferred to the solubilized sulfate phase, and the non- soluble oxide phase (mostly containing Fe 2 0 3 ) forms an iron concentrate.
  • the overall process includes the following steps:
  • jarosite material preferably including jarosite or goethite, or both, particularly being jarosite
  • Figure 2 illustrates an alternative process scheme in accordance with an embodiment of the present invention.
  • the process scheme of this Figure includes a step of roasting the solid phase obtained from the dissolution step, before sulfidization and flotation.
  • Said roasting step is intended to oxidize any elemental sulphur present in the solid phase obtained from the dissolution step, according to the following reaction (54):
  • This step can be essential in certain cases, since many zinc processes recently developed result in jarosite fractions that are rich in elemental sulphur, while sulphur in its elemental form would have a negative effect on the subsequent sulfidization and flotation step.
  • embodiment means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention.
  • appearances of the phrases “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment.
  • a numerical value using a term such as, for example, about or substantially, the exact numerical value is also disclosed.
  • the annual feed amounts of jarosite and dust have in the below calculations been selected to be 400,000 t/a and 20,000 t/a, respectively, and the processing time 8000 h/a.
  • a sulphuric acid treatment is carried out on the dust.
  • the sulphuric acid is heated to a temperature of 200°C and mixed with the preheated (100-150°C) dust.
  • the temperature of the formed mixture thus rises to more than 250°C.
  • the oxides in the dust are sulphatized, the halogenides are decomposed and sulphatized at least to a degree of 70%.
  • the water and the halogen hydrides are transferred to the gas phase, from where they are compressed using water washing.
  • the reactions of this sulphuric acid treatment are further described below, in Tables 3-5. Table 3. Reactions with sulfuric acid:
  • Jarosite and the sulphatized dust are fed to an S0 2 dissolution step.
  • the temperature in said dissolution is about 90°C, whereby the reactions of the following listing take place, affecting the components of the jarosite and the components of the sulphatized dust.
  • this reaction listing it has been assumed that all reactions (16) - (29) have a reaction degree between 0.95 and 1.00.
  • Example 4 The separation of indium, gallium ja germanium
  • the indium and gallium are separated from Solution 3 by a hydroxide precipitation, by adjusting the pH to a level of 3.5-4, using Mg(OH) 2 as the pH adjustment agent.
  • the temperature of the solution is between 80 and 90°C.
  • Other possible pH adjustment agents are ZnO, Walz-oxide (or the ZnO therein), CaO, Ca(OH) 2 or CaC0 3 .
  • the hydroxides In(OH) 3 and Ga(OH) 3 are less soluble compared to Al(OH) 3 , which is also one of the least soluble hydroxides of the solution phase (when no ferric ions are present).
  • solubility product values for the indium and gallium hydroxides are equal to or lower than 10(exp(-36)), and if the corresponding value for aluminium hydroxide is 10(exp(-31)), it is possible to obtain a sharp distinction. If the pH adjustment range is 3.5-4, the precipitate will contain also aluminium hydroxide.
  • Germanium (and gallium) can be precipitated completely from the solution in the form of a tannine.
  • indium, gallium and aluminium hydroxides are precipitated in a pure form, and germanium is precipitated in the form of its hydroxide, the following reactions take place:
  • the precipitated hydroxides are separated from the solution, and are washed.
  • the washing solution is added to the solution phase.
  • a precipitate containing In, Ga and Ge hydroxides is obtained, and a Solution 4.
  • the sulfide precipitation is carried out by adjusting the pH of the solution, for example using Mg(OH) 2 , so that no significant amounts of iron (Fe 2+ ) is precipitated.
  • the 5 reactions taking place during the precipitation include the following:
  • the obtained sulfide precipitate 1 is treated with an ammonium polysulfide solution, whereby AS2S3, Sb 2 S3 and SnS dissolve, whereas CuS, CdS and ZnS remain in solid form.
  • Solution 5 is concentrated by a multiphase evaporation crystallization.
  • the steam phase is cooled, compressed and returned to the
  • the salt phase is carried to a thermal phase, where the following reactions take place:
  • Certain components can be recirculated in the process, particularly in case all of the above mentioned process steps are carried out in series as described. These components include sulfur dioxide (S0 2 ), sulfuric acid (H 2 SO 4 ) and the sulfide solution containing ammonium sulfate ((NH 4 ) 2 S0 4 ) and hydrogen sulfide (H 2 S).
  • Silver and gold can, in turn be separated from the final waste, by treating it further using conventional techniques.
  • the Jarosite material used was selected from those containing large amounts of elemental sulfur, and obtained from the process applications, which utilize direct dissolving procedures.
  • the solid fraction is treated with thermal, calcination, treatment at about 500 °C to remove the elemental sulfur (Reaction (30)), and ZnS reacts according to Reaction (31).
  • the solid phase is flotated, with the sulfide phase and gold collected froth.
  • magnesium hydroxide is used as a neutralization agent at the temperature of 90 °C with very accurate pH-control.
  • Solution 5 is then concentrated by evaporation.
  • the vaporized phase is cooled down and returned back to the S02-solution.
  • the solid phase is washed with water.
  • the insoluble residue which contains mainly Fe 2 0 3 , can be collected as it is suitable for use as Iron making concentrate.
  • the present invention provides, among others, an environmentally friendly solution for recycling the zinc-containing waste dust of the steel mills in connection with the recovery of metals from the jarosite precipitate formed as a waste in the zinc mills.

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

Abstract

La présente invention concerne un procédé de séparation de métaux à l'aide d'une série de précipitations à partir de déchets de l'industrie du zinc ou de l'acier, ou des deux. Le procédé est caractérisé par la mise en œuvre des précipitations à l'aide d'hydroxydes ou de produits chimiques contenant du soufre choisis parmi les sulfates, les sulfures, les oxydes de soufre et les sulfites, ou les deux, afin d'obtenir des précipités métalliques ainsi qu'une solution aqueuse contenant du soufre, cette dernière étant éventuellement recyclée dans le procédé, après quoi un précipité final est transporté vers une étape thermique, en vue de la formation.
PCT/FI2017/050901 2016-12-15 2017-12-15 Traitement de déchets industriels contenant des métaux Ceased WO2018109283A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP17880716.0A EP3555327A4 (fr) 2016-12-15 2017-12-15 Traitement de déchets industriels contenant des métaux

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20165972 2016-12-15
FI20165972A FI128281B (en) 2016-12-15 2016-12-15 Processing of Industrial Metal-Containing Waste Materials

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WO2018109283A1 true WO2018109283A1 (fr) 2018-06-21

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977666A (zh) * 2018-08-30 2018-12-11 河南豫光锌业有限公司 一种湿法炼锌净化渣中锌钴的回收方法
WO2020222254A1 (fr) * 2019-05-01 2020-11-05 Malshe Vinod Utilisation efficace de déchets de jarosite
CN112080646A (zh) * 2020-08-26 2020-12-15 昆明理工大学 一种除去真空蒸馏处理锡精炼硫渣产物粗硫化亚锡中砷、锑的方法
WO2023089234A1 (fr) 2021-11-16 2023-05-25 Teknologian Tutkimuskeskus Vtt Oy Procédé hydrométallurgique pour des déchets issus des industries du zinc et de l'acier
EP4321650A1 (fr) 2022-08-10 2024-02-14 Xtract GmbH Procédé de dézingage de déchets d'acier galvanisé
WO2025125107A1 (fr) * 2023-12-13 2025-06-19 Amateq Holding Gmbh Procédé de production écologique d'acier et de fer de fonderie

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US4071422A (en) * 1976-04-15 1978-01-31 Cominco Ltd. Process for concentrating and recovering gallium
WO1988003911A1 (fr) * 1986-11-26 1988-06-02 Resource Technology Associates Procede de recuperation de metaux a partir de solides de jarosite
US5380354A (en) * 1993-05-04 1995-01-10 Sherritt Inc. Recovery of metals from sulphidic material
US5431713A (en) * 1994-07-19 1995-07-11 Metals Recycling Technologies Crop. Method for the reclamation of metallic compounds from zinc and lead containing dust
US8323377B2 (en) * 2004-03-25 2012-12-04 Intec, Ltd. Recovery of metals from oxidised metalliferous materials
WO2013079804A1 (fr) * 2011-12-02 2013-06-06 Jyväskylän Energia Oy Procédé de traitement de cendres, en particulier de cendres volantes

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BRPI0905473A2 (pt) * 2009-12-11 2011-08-02 Mineracao Tabipora Ltda processo fìsico-quìmico para recuperação de metais contidos em resìduo industrial siderúrgico
CA2854778A1 (fr) * 2014-06-18 2015-12-18 Guy Mercier Recuperation de zinc et de manganese a partir de boues ou de residus de pyrometallurgie

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Publication number Priority date Publication date Assignee Title
US4071422A (en) * 1976-04-15 1978-01-31 Cominco Ltd. Process for concentrating and recovering gallium
WO1988003911A1 (fr) * 1986-11-26 1988-06-02 Resource Technology Associates Procede de recuperation de metaux a partir de solides de jarosite
US5380354A (en) * 1993-05-04 1995-01-10 Sherritt Inc. Recovery of metals from sulphidic material
US5431713A (en) * 1994-07-19 1995-07-11 Metals Recycling Technologies Crop. Method for the reclamation of metallic compounds from zinc and lead containing dust
US8323377B2 (en) * 2004-03-25 2012-12-04 Intec, Ltd. Recovery of metals from oxidised metalliferous materials
WO2013079804A1 (fr) * 2011-12-02 2013-06-06 Jyväskylän Energia Oy Procédé de traitement de cendres, en particulier de cendres volantes

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See also references of EP3555327A4 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977666A (zh) * 2018-08-30 2018-12-11 河南豫光锌业有限公司 一种湿法炼锌净化渣中锌钴的回收方法
WO2020222254A1 (fr) * 2019-05-01 2020-11-05 Malshe Vinod Utilisation efficace de déchets de jarosite
CN113785080A (zh) * 2019-05-01 2021-12-10 维诺德·秦塔马尼·玛尔什 黄钾铁矾废物的有效利用
US12351891B2 (en) 2019-05-01 2025-07-08 Vinod Chintamani Malshe Effective utilization of jarosite waste
CN112080646A (zh) * 2020-08-26 2020-12-15 昆明理工大学 一种除去真空蒸馏处理锡精炼硫渣产物粗硫化亚锡中砷、锑的方法
WO2023089234A1 (fr) 2021-11-16 2023-05-25 Teknologian Tutkimuskeskus Vtt Oy Procédé hydrométallurgique pour des déchets issus des industries du zinc et de l'acier
EP4321650A1 (fr) 2022-08-10 2024-02-14 Xtract GmbH Procédé de dézingage de déchets d'acier galvanisé
WO2024033477A1 (fr) 2022-08-10 2024-02-15 Xtract Gmbh Procédé de dézingage de déchets d'acier galvanisés
WO2025125107A1 (fr) * 2023-12-13 2025-06-19 Amateq Holding Gmbh Procédé de production écologique d'acier et de fer de fonderie

Also Published As

Publication number Publication date
EP3555327A1 (fr) 2019-10-23
FI128281B (en) 2020-02-28
FI20165972A7 (fi) 2018-06-16
FI20165972L (fi) 2018-06-16
EP3555327A4 (fr) 2020-08-12

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