WO2005012582A1 - Traitement hydrometallurgique ameliore de materiaux contenant du manganese - Google Patents

Traitement hydrometallurgique ameliore de materiaux contenant du manganese Download PDF

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Publication number
WO2005012582A1
WO2005012582A1 PCT/AU2004/000854 AU2004000854W WO2005012582A1 WO 2005012582 A1 WO2005012582 A1 WO 2005012582A1 AU 2004000854 W AU2004000854 W AU 2004000854W WO 2005012582 A1 WO2005012582 A1 WO 2005012582A1
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WIPO (PCT)
Prior art keywords
manganese
leach
less
leach solution
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/AU2004/000854
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English (en)
Inventor
Christopher Brett Ward
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HITEC ENERGY Ltd
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HITEC ENERGY 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 HITEC ENERGY Ltd filed Critical HITEC ENERGY Ltd
Priority to AU2004260809A priority Critical patent/AU2004260809B2/en
Publication of WO2005012582A1 publication Critical patent/WO2005012582A1/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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • 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
    • C22B47/00—Obtaining manganese
    • C22B47/0018—Treating ocean floor nodules
    • C22B47/0045—Treating ocean floor nodules by wet processes
    • C22B47/0054—Treating ocean floor nodules by wet processes leaching processes
    • C22B47/0063—Treating ocean floor nodules by wet processes leaching processes with acids or salt solutions
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/40—Mixtures
    • C22B3/402—Mixtures of acyclic or carbocyclic compounds of different types
    • C22B3/404—Mixtures of acyclic or carbocyclic compounds of different types of organic acids and oximes
    • 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 relates to the improved hydrometallurgical processing of manganese containing materials. More particularly, the process of the present invention is intended to allow efficient hydrometallurgical processing of low-grade manganese dioxide feedstock to produce manganese chemicals, including electrolytic manganese dioxide, utilising a solvent extraction process route.
  • manganese may be leached from manganese dioxide containing ores using sulphur dioxide.
  • the sulphur dioxide leaching of manganese dioxide containing materials is also known to produce by-product dithionate ion levels of >5g/l. These levels may be far higher depending upon the amount of manganese being leached. For example, levels of about 20g/l are not uncommon.
  • the method for production of dithionate or dithionic acid is the reaction between sulphur dioxide or sulphite with manganese dioxide in the presence of acid.
  • the ability to recover manganese dioxide from low-grade feedstocks will avoid or at least reduce the need for further manganese ore mining and land disturbance, bringing various environmental benefits.
  • the utilisation of manganese tailings allows for conservation of existing resources.
  • the use of the relatively easily controlled hydrometallurgical route allows monitoring of the solution potential of the leach solution or slurry thereby indicating complete dissolution of Mn(IV).
  • the use of the sulphur dioxide leach provides complete conversion of Mn(IV) to Mn(ll), thereby avoiding the production of leachable manganese species in solid residues.
  • EMD electrolytic manganese dioxide
  • solutions containing elevated dithionate ion levels result in chemical reactions occurring that effect the quality and purity of the EMD produced in the electrowinning cells.
  • hydrogen sulphide is evolved, bringing with it certain occupational health and environmental issues.
  • the present applicant has previously proposed a hydrometallurgical processing route for manganese containing materials utilising a sulphur dioxide leach over 10 to 15 hours, during which a stoichiometric amount of sulphur dioxide is added to the leach solution to achieve a 95% dissolution of the manganese dioxide present, after which the reaction is halted, the dithionate ion levels are preferably maintained at less than about 5g/l, and preferably less than 1g/L, and the resulting leach solution is then processed by way of a jarositing step to reduce potassium and sodium levels as desired, and a goethiting step to reduce iron levels to sub- ppm levels, to provide an electrolyte that is passed to an electrowinning stage during which electrolytic manganese dioxide is deposited.
  • US Patent 4423012 describes a process whereby the concentration of a desired metal, such as manganese or zinc, with respect to certain impurities in an electrowinning feed stream, may be increased. This is said to be achieved by mixing an aqueous bleed stream from the feed stream with a solvent extraction agent (DEHPA), after which that bleed stream is subjected to solvent extraction over several counter-current stages, the resulting loaded organic then being stripped with spent electrolyte from the electrowinning circuit. That loaded strip solution is then recycled to the electrowinning circuit for recovery of manganese and zinc metal. Importantly, this process is applied to only a small bleed stream from a conventional roast reduction/acid leach EMD process, is not appropriate for saline leach solutions and the extractant utilised is a phosphoric acid.
  • DEHPA solvent extraction agent
  • a process for the improved hydrometallurgical processing of manganese containing materials characterised by the formation of a leach solution of manganese dioxide containing feedstock and acidic solution, passing a volume of sulphur dioxide gas through the leach solution whereby the levels of dithionate ion generated in the pregnant leach solution are less than about 5g/l, and subsequently passing the pregnant leach solution to a solvent extraction step.
  • the levels of dithionate ion generated in the leach solution are less than about 1g/l.
  • the pH of the leach solution is maintained at less than about 5. Still further preferably, the pH of the leach solution is maintained at less than about 3.
  • the leach is conducted at a temperature of less than about 60°C.
  • sufficient sulphur dioxide is passed through the leach solution to ensure that 95% of the manganese present is leached over a period of less than about 2 hours.
  • the manganese dioxide containing feedstock contains less than 40% manganese.
  • the ratio of ferric to ferrous may be monitored throughout the leach to ensure an oxidation reduction potential (ORP) of about 550mV, or above (vs Ag/AgCI reference electrode).
  • ORP oxidation reduction potential
  • the solvent extraction step is preferably followed by a stripping step, in which a loaded organic phase is contacted with a spent sulphuric acid electrolyte from an electrowinning step, providing a manganese sulphate solution that is in turn passed to the electrowinning step.
  • the dithionate ions present in the leach solution remain in the aqueous phase during solvent extraction.
  • Figure 1 is a schematic flow chart of a process for the production of an electrolytic manganese dioxide product from a low grade manganese feedstock in accordance with the present invention.
  • FIG. 1 there is shown a process 10 for the production of electrolytic manganese dioxide product in accordance with the present invention.
  • a manganese dioxide ore feedstock 12 containing less than about 40% manganese is ground and the resulting slurry passed to a leach 14 conducted in at least one agitated reactor, forming a 10% w/w leach solution.
  • Sufficient sulphur dioxide 16 (as a gas or a liquid) is passed through the leach solution at a pH of less than about 5, preferably less than about 3, at a temperature of less than about 60°C, preferably less than about 50°C.
  • the sulphur dioxide is passed through the leach solution at a rate to ensure that 95% of the manganese is leached in less than about 2 hours.
  • the ratio of ferric ion to ferrous ion in the leach 14 is monitored by the use of an
  • ORP Oxidation Reduction Potential
  • the leaching reaction is as below:
  • the reaction is halted by stopping the addition of further sulphur dioxide.
  • the pH of the solution is then increased to between pH 5 and 7 by the use of lime or limestone and the solid liquid separation step performed by the use of a thickener 18 and a filter (not shown).
  • the sulphur dioxide 16 may be provided as a waste gas from a smelting or an industrial process. Further, the sulphur dioxide may be added to the leach solution as a sulphite solution (SO 3 2" ).
  • the soluble manganese content is expected to be less than about 20 g/L at this stage but the concentration will be dependent upon the throughput used from the leach 14. It should also be noted that any manganese species in an aqueous solution can also be added to this stream at this stage and the manganese will be recovered and utilised to make extra EMD. Such streams can come from neighbouring mines and processing plants, or spillages from the manganese processing facility.
  • aqueous solution is contacted with a carboxylic acid extractant, for example Versatic 10TM, at a concentration of about 0.5M in an aliphatic diluent, for example Shellsol D70TM, in up to 5 extraction stages with an aqueous to organic ratio of approximately 2 to 1.
  • a suitable base such as Na OH, NH OH or Na 2 CO 3 , to between 4.5 and 7, preferably 5.5 and 6.5.
  • any chloride ions and the majority of the magnesium, calcium, potassium and iron remain in the aqueous phase and are not loaded onto the organic extractant.
  • the aqueous phase can then be either recycled back to the leach 14 for further manganese leaching or is rejected to a tailings dam 22 together with solids removed in the thickener 18.
  • a synergistic extractant, such as the oxime LIX63, may also be added to the Versatic 10TM extractant to assist in the separation of any calcium.
  • the loaded organic phase is stripped of the manganese by contacting it with sulfuric acid containing spent electrolyte 24 returning from a electrowinning step 26.
  • the stripping solution 24 is expected to be between about 40 and 70 g/L manganese and about 25 to 50 g/l sulphuric acid along with some other minor impurities.
  • the hydrogen ions generated in the electrowinning step 26 are replaced by the manganese ions from the organic phase and the pH rises towards a neutral pH.
  • the resulting solution is called the pregnant leach solution 28 and is passed through a range of filtration steps (not shown) to remove any residual organic components.
  • the solution 28 is then fed to a sulfiding step 30 for further purification by the addition of a sulfiding reagent to remove heavy metals, before a further filtration step 32.
  • the solution 28 is then ready for feeding to electrowinning cells of the electrowinning step 26, during which the manganese is plated for high quality electrolytic manganese dioxide (EMD), suitable for use by alkaline battery manufacturers.
  • EMD electrolytic manganese dioxide
  • the electrowinning step 26 proceeds utilising submerged titanium anodes, tubular copper cathodes and a totally wax free environment. Fully laden anodes are harvested on a two-weekly cycle with resulting EMD chip being passed to produce processing and packaging operations.
  • a small side or bleed stream may also be included, of the order of 5% of the flow from the electrowinning step, returning to the leach 14 to recover manganese and reject unwanted contaminants, such as sodium, and to further lower the recirculating calcium load so that the chance of gypsum precipitation is further reduced.
  • the loss of pregnant leach solution volume may be made up by the addition of demineralised water to the electrolyte circuit.
  • the process of the present invention may be applied to the processing of all types of manganese dioxide containing ores (including both high and low grade), mine tailings, fines, fumes and tailings of manganese ferro-alloy production facilities, ocean floor manganese nodules, ferromanganese nodules, wastes from zinc refinery cells and manganese dioxide contained in used or partially used alkaline or carbon zinc batteries.
  • the leach solutions generated by reprocessing such materials in accordance with the present invention can then be purified and used in the production of EMD, EMM and other manganese chemical products.
  • the improved hydrometallurgical processing of manganese containing materials described herein has a significantly reduced requirement for capital expenditure when compared with equivalent processes of the prior art, including the Applicant's prior art process described in International Patent Application PCT/AU03/01295 (WO 04/033738) and referred to hereinabove.
  • the relatively low temperature leach requires less steam and is able to utilise standard fibreglass (FRP) as the leach vessels.
  • FRP standard fibreglass
  • the less aggressive pH utilised in the process of the present invention has less impact on the equipment and requires significantly less acid than prior art processes.
  • the leach of the present invention is able to be performed in raw water, for example from the Kalgoorlie region of Western Australia, which consequently lowers any requirement for demineralised water in the process.
  • the process of the present invention does not require Jarositing and Goethiting steps.
  • the specific solvent extraction process utilised in the present invention including use of Versatic acid, rejects potassium. Further, no iron leach, nor any iron source is required. This provides further relative savings in relation to both capital and operating costs.
  • the leach tank utilised in the leach step will be a vessel suitable to accept a large range of manganese inputs (solid and liquid) irrespective of the anion attached to the manganese, if they were proven to lower cost inputs.
  • a bleed stream may be introduced back to the leach tank, whereby it is conceivable that the frequency of cathode cleaning to remove gypsum could be reduced dramatically, thereby providing a system to lower magnesium and sodium levels to even lower levels than previously considered. While magnesium is not a significant concern, the process of the present invention had no route to reduce Mg levels other than through solution losses and replacement with clean demineralised water. Lower gypsum deposition in pipe work and tankage will have a significant maintenance cost benefit, once the plant has reached equilibrium conditions.

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

Abstract

L'invention concerne un procédé pour le traitement hydrométallurgique amélioré de matériaux contenant du manganèse. Ce procédé est caractérisé par le fait que l'on forme une solution ou une boue de lixiviation d'une charge contenant du dioxyde de manganèse et une solution acide,l'on fait passer un volume de gaz de dioxyde de soufre à travers la solution de lixiviation, les niveaux d'ions dithionate générés dans le jus fort de lixiviation étant inférieurs à 5 g/l environ, et l'on fait passer subséquemment ce jus fort de lixiviation à l'étape d'extraction de solvant.
PCT/AU2004/000854 2003-07-30 2004-06-28 Traitement hydrometallurgique ameliore de materiaux contenant du manganese Ceased WO2005012582A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2004260809A AU2004260809B2 (en) 2003-07-30 2004-06-28 Improved hydrometallurgical processing of manganese containing materials

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2003903992 2003-07-30
AU2003903992A AU2003903992A0 (en) 2003-07-30 2003-07-30 Improved hydrometallurgical processing of manganese containing materials

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Publication Number Publication Date
WO2005012582A1 true WO2005012582A1 (fr) 2005-02-10

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CN (1) CN100376698C (fr)
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2296174C1 (ru) * 2005-07-04 2007-03-27 Государственное образовательное учреждение высшего профессионального образования "Российский университет дружбы народов" (РУДН) Раствор для выщелачивания оксидно-марганцевых руд
WO2009039560A1 (fr) * 2007-09-26 2009-04-02 Hitec Energy Limited Engrais à micronutriments et son procédé de fabrication
RU2441085C1 (ru) * 2010-07-23 2012-01-27 Государственное образовательное учреждение высшего профессионального образования "Башкирский государственный университет", ГОУ ВПО БашГУ Способ переработки карбонатных марганцевых руд
RU2441086C1 (ru) * 2010-12-23 2012-01-27 Государственное образовательное учреждение высшего профессионального образования "Башкирский государственный университет", ГОУ ВПО БашГУ Способ переработки марганцевых руд
CN103261121A (zh) * 2010-12-08 2013-08-21 美萨矿物有限公司 改进的微量营养素肥料及其生产方法
RU2607873C1 (ru) * 2015-09-28 2017-01-20 федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" Способ переработки железомарганцевых конкреций
CN108220595A (zh) * 2017-12-05 2018-06-29 中信大锰矿业有限责任公司大新锰矿分公司 利用木薯干粉和甲醛还原浸出氧化锰矿的方法
CN111111419A (zh) * 2020-01-02 2020-05-08 四川大学 利用碳酸锰矿脱除烟气中高浓度so2制备硫酸锰溶液的方法
WO2023148644A1 (fr) * 2022-02-04 2023-08-10 Tata Steel Limited Procédé de récupération de manganèse à partir de minerai de manganèse

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* Cited by examiner, † Cited by third party
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CN108928853A (zh) * 2018-08-15 2018-12-04 广西锰华新能源科技发展有限公司 一种锰矿浸出渣的综合回收利用方法
MX2022001716A (es) * 2019-08-09 2022-03-11 Umicore Nv Proceso de recuperacion de metales a partir de minerales oxidicos.

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2296174C1 (ru) * 2005-07-04 2007-03-27 Государственное образовательное учреждение высшего профессионального образования "Российский университет дружбы народов" (РУДН) Раствор для выщелачивания оксидно-марганцевых руд
WO2009039560A1 (fr) * 2007-09-26 2009-04-02 Hitec Energy Limited Engrais à micronutriments et son procédé de fabrication
RU2441085C1 (ru) * 2010-07-23 2012-01-27 Государственное образовательное учреждение высшего профессионального образования "Башкирский государственный университет", ГОУ ВПО БашГУ Способ переработки карбонатных марганцевых руд
CN103261121A (zh) * 2010-12-08 2013-08-21 美萨矿物有限公司 改进的微量营养素肥料及其生产方法
CN103261121B (zh) * 2010-12-08 2016-05-04 美萨矿物有限公司 改进的微量营养素肥料及其生产方法
RU2441086C1 (ru) * 2010-12-23 2012-01-27 Государственное образовательное учреждение высшего профессионального образования "Башкирский государственный университет", ГОУ ВПО БашГУ Способ переработки марганцевых руд
RU2607873C1 (ru) * 2015-09-28 2017-01-20 федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" Способ переработки железомарганцевых конкреций
CN108220595A (zh) * 2017-12-05 2018-06-29 中信大锰矿业有限责任公司大新锰矿分公司 利用木薯干粉和甲醛还原浸出氧化锰矿的方法
CN111111419A (zh) * 2020-01-02 2020-05-08 四川大学 利用碳酸锰矿脱除烟气中高浓度so2制备硫酸锰溶液的方法
CN111111419B (zh) * 2020-01-02 2021-03-23 四川大学 利用碳酸锰矿脱除烟气中高浓度so2制备硫酸锰溶液的方法
WO2023148644A1 (fr) * 2022-02-04 2023-08-10 Tata Steel Limited Procédé de récupération de manganèse à partir de minerai de manganèse

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CN100376698C (zh) 2008-03-26
CN1860243A (zh) 2006-11-08

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