EP0165166B1 - Procédé de traitement de minerais complexes de manganèse tels que les nodules marins - Google Patents

Procédé de traitement de minerais complexes de manganèse tels que les nodules marins Download PDF

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Publication number
EP0165166B1
EP0165166B1 EP85401080A EP85401080A EP0165166B1 EP 0165166 B1 EP0165166 B1 EP 0165166B1 EP 85401080 A EP85401080 A EP 85401080A EP 85401080 A EP85401080 A EP 85401080A EP 0165166 B1 EP0165166 B1 EP 0165166B1
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EP
European Patent Office
Prior art keywords
ore
pulp
process according
manganese
treatment
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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.)
Expired
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EP85401080A
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German (de)
English (en)
French (fr)
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EP0165166A1 (fr
Inventor
Odile Pinto
Henri Scoazec
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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    • 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
    • C22B47/00—Obtaining manganese
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S423/00—Chemistry of inorganic compounds
    • Y10S423/04—Manganese marine modules

Definitions

  • the present invention relates to a process for the treatment of complex manganese ores such as the manganiferous modules of the deep seabed.
  • Manganese nodules from the deep sea contain significant amounts of manganese and iron, minor amounts of nickel, cobalt and copper, and small amounts of other elements.
  • Nickel, copper and cobalt are high value metals which it is interesting to extract from these nodules with good yields since the known reserves of these metals decrease significantly.
  • cobalt is particularly difficult to extract by conventional processes with good yields without simultaneously obtaining significant solubilization of manganese.
  • manganese is a recoverable metal, it is not always desirable to recover all of the manganese present in the treated nodules.
  • Another aim is to create a new improved process for extracting cobalt, which process can also provide recovery of the nickel and copper elements with excellent yields.
  • Another aim is to create a new process allowing the selective extraction of cobalt, nickel and copper in sulfuric medium with good yields without dissolving the iron.
  • Another goal is to create a new process for extracting cobalt in sulfuric medium in addition to nickel and copper with good yields, without dissolving the manganese.
  • Another aim is to create a new process making it possible to extract cobalt, nickel, copper with good yields without dissolving the iron, without dissolving the manganese, without involving attack conditions as severe as a sulfuric attack in an autoclave at 250 ° C.
  • the present invention relates to a process for the treatment of complex manganese ores such as manganiferous nodules from the deep seabed, which overcomes this drawback.
  • the manganous ions used in the solution of manganous sulphate obtained in step e) are used in the solubilization of nickel, copper and cobalt, in conditions where these Mn 2 ions + should not be able to act as reducing agent for Mn0 2 and where the medium does not contain a reducing agent for manganese dioxide.
  • the manganous ions, in sulfuric medium allow the extraction of cobalt with good yields and improve the yields of nickel and copper, under operating conditions where sulfuric acid alone gives poor yields , especially in cobalt. It is assumed that in this case, it is a complex equilibrium involving an oxidation-reduction mechanism between, on the one hand, the cobalt in solution and the manganese of the ore or nodule and, on the other hand , cobalt adsorbed or trapped in the manganese of the ore or nodules and manganese in solution. Adding Mn 2+ ions to the sulfuric attack solution makes it possible to enrich this solution and thus to shift the balance in favor of the solubilization of the cobalt.
  • the yields of nickel and copper are favorably influenced, probably thanks to phenomena of ion exchanges existing in the presence of manganous ions.
  • the second part of the crushed ore is enriched with manganese before subjecting it to the treatment for dissolving nickel, copper and cobalt.
  • the second part of the ground ore is brought into contact with a manganous sulfate solution in order to fix on this ground ore at least a part of the manganese of this solution and thus to enrich the ground ore in manganese.
  • the manganous sulfate solution is saturated with HA.
  • the saturated H 2 S solution obtained at the end of step i) of treatment of the preceding batch is used as the manganous sulphate solution.
  • the manganous sulfate solution used to enrich the second part of the crushed ore coming from the second batch of ore with manganese consists of the solution obtained after recovery. nickel, copper and cobalt at the end of step i) of processing the first batch of ore.
  • step i) the nickel, copper and cobalt are generally separated from the liquid phase by precipitation of the corresponding sulfides by means of H 2 S and after separation of these precipitates, the end of treatment is obtained.
  • a solution of manganous sulfate saturated with H 2 S which can be reused for the treatment of the next batch of ore.
  • This manganous sulphate solution has a manganous sulphate content much lower than that which must be used for carrying out step g). Also, it would have been necessary to concentrate it in order to be able to use it in step g), but the concentration by evaporation is excluded because of the energy cost which it imposes.
  • this method implements an oxidation-reduction mechanism allowing the manganous ions to be concentrated in the form of Mn 2 0 3 by reaction with the manganese dioxide present in the complex manganese ore, then a mechanism of disproportionation of Mn 2 0 3 into Mn 2+ by passage through an acid medium during step g) of treatment for solubilization with sulfuric acid.
  • the manganous ions are oxidized by the manganous oxide Mn0 2 of the complex ore or of the nodules to Mn 2 0 3 according to the following reaction scheme:
  • a manganiferous nodule generally contains 29% of manganese essentially in the state of MnO 2 , the oxidation of a solution of manganous sulfate at pH 6 to 7 can be considered.
  • a saturation threshold of the manganese nodule which is a function of the concentration of manganous ions and of the pulp ratio, that is to say the ratio of the mass of solution to the mass of ground nodules.
  • step g) of treatment of the second pulp with hot sulfuric acid part of the manganous ions previously fixed on the nodules is resolubilized by disproportionation of Mn 2 0 3 into Mn 2+ and MnO 2 .
  • the presence of certain ions can totally or partially inhibit this disproportionation reaction and the solubilization yields obtained do not allow not to re-dissolve the total quantity of manganous ions fixed above, whatever the temperature and the quantity of sulfuric acid used in this step.
  • this mode of recycling makes it possible to reuse part of the manganous sulphate evacuated following step i) and to obtain following step h) a solid phase enriched in manganese from which it will be possible to recover the desired amount of manganese.
  • the second part is subjected ore crushed in a washing step with sulfuric acid at room temperature to remove most of the alkaline elements and alkaline earth elements, the solid phase is separated from the washing liquid phase and said second pulp is prepared for from the solid phase thus separated.
  • step d) of preparing a manganous sulphate solution is carried out by reacting the first pulp with an appropriate mineral or organic reducing agent such as SO 2 , H 2 S, carbohydrates and alcohols.
  • an appropriate mineral or organic reducing agent such as SO 2 , H 2 S, carbohydrates and alcohols.
  • this step is carried out by reacting the first pulp with sulfur dioxide.
  • this step can also be carried out by reacting the first pulp with sulfuric acid in the presence of an organic reducing agent consisting, for example, of a carbohydrate such as sucrose, other saccharides such as monosaccharides, oligosaccharides and polysaccharides, an alcohol, a polyalcohol, or even urea.
  • an organic reducing agent consisting, for example, of a carbohydrate such as sucrose, other saccharides such as monosaccharides, oligosaccharides and polysaccharides, an alcohol, a polyalcohol, or even urea.
  • the organic reducing agent is used to reduce the manganese from the oxidation state (IV) to the oxidation state (II).
  • manganese can be solubilized, which requires the consumption of sulfate ions and therefore the consumption of sulfuric acid.
  • the pH of the pulp increases, and, depending on the quantity of sulfuric acid initially present and the quantity of organic agent added to the pulp, the pH of the solution can be increased until the pH necessary for precipitation, in the form of iron hydroxide, of the solubilized iron from the ore. However, if this increase is significant, precipitation of the dissolved copper from the ore is also obtained.
  • quantities of sulfuric acid and organic reducing agent are used such that the precipitation pH of iron is reached (substantially 2) without reaching the precipitation pH of copper (approximately 4 to 5).
  • a powerful organic reducing agent is preferably used, for example an organic reducing agent having several reducing functions such as saccharides and polyalcohols.
  • sucrose is used.
  • the amounts of sucrose generally used are less than 500 kg per tonne of ore or nodules treated and, advantageously 200 to 400 kg per tonne of ore or nodules treated.
  • the amount of sulfuric acid used is preferably from 700 to 850 kg per tonne of ore or nodules treated if it is desired to dissolve nickel, copper, cobalt and manganese with a yield reaching practically 100%; otherwise, smaller amounts can be used.
  • the best results are obtained when 327 kg of sucrose and 750 to 800 kg of sulfuric acid are used per tonne of ore or nodules. It is specified that the solubilization of manganese alone requires 500 to 550 kg of sulfuric acid. There are therefore 200 to 250 kg of acid remaining for the other elements.
  • the reducing agent consists of methyl alcohol or ethyl alcohol
  • advantageously 100 to 700 kg of alcohol are used per tonne of ore treated and 700 to 850 kg of sulfuric acid per tonne of ore treaty.
  • a manganous sulphate solution also containing nickel, copper and cobalt present in the treated ore is obtained.
  • This solution can be used directly for step g) which consists in subjecting the second pulp to a treatment for dissolving nickel, copper and cobalt by reaction with sulfuric acid.
  • the manganiferous nodules are separated into two parts, a first part (at 3) which will be subjected to attack by SO 2 to dissolve the manganese and a second part (at 5) which will be subjected to the nickel solubilization treatment, copper and cobalt with H 2 SO 4 . Since the grinding is carried out in an aqueous medium, the first part is in the form of pulp and the pulp ratio is adjusted to the desired value by addition of water.
  • the pulp ratio is defined by the ratio of the mass of freshwater or seawater to the mass of ground nodules, and it should be such that the pulp behaves like a fluid, but preferably as low as possible so as to process minimum volumes of pulp.
  • this first pulp a pulp ratio ranging from 2 to 5 is used.
  • the first pulp is then reacted with sulfur dioxide (in 9) to obtain a manganous sulfate solution, which also leads to the solubilization of the nickel, copper and cobalt present in this first pulp.
  • This reaction is carried out at room temperature by injecting the desired quantity of sulfur dioxide into the pulp, for example by bubbling, while maintaining regular agitation of the pulp.
  • the quantity of sulfur dioxide injected is calculated by taking into account the stoichiometry of the reaction for the sulphation of manganese dioxide by sulfur dioxide so as to dissolve practically all of the manganese. Generally, a yield of 95% is obtained.
  • the solid phase is then separated (at 11) from the liquid phase, the solid phase is subjected to washing (at 13) by recycling (at 24) the washing water in the reduction step with SO z ; the residual solid phase which constitutes the waste rock is rejected (in 15); it generally contains around 5% of the manganese present in the nodules of the first pulp.
  • the second part 5 of the ground nodules which is also in the form of pulp, constitutes the second pulp. It is firstly enriched with manganese in a three-stage installation 6 in which it is brought into countercurrent contact with a manganous sulfate solution saturated with H 2 S arriving at 8. During this treatment, the solution aqueous depletes in manganese and enriches in alkaline and alkaline earth elements from the ground nodules. This solution is removed at 10. Following this treatment, the second pulp of ground nodules is subjected to the treatment for dissolving nickel, copper and cobalt carried out in the autoclave 17.
  • the pulp ratio must be such that the pulp behaves like a fluid, but preferably as low as possible, so as to treat minimum volumes of pulp. However, too low a pulp ratio limits the copper extraction yield. Generally, a pulp ratio ranging from 2 to 5 is used, and preferably a pulp ratio equal to 2 or 3.
  • the solubilization treatment of nickel, copper and cobalt is then carried out by reacting (at 17) this second pulp with sulfuric acid and the manganous sulphate solution from 11 obtained by treatment of the first pulp with SO 2 .
  • the amounts of manganese sulfate used for this reaction can vary over a wide range. However, above a certain threshold, the use of larger amounts does not improve the results obtained with regard to the extraction of cobalt.
  • the quantity of manganous sulphate present in solution during this treatment is from 50 to 400 kg per tonne of crushed ore, and preferably from 50 to 250 kg per tonne of crushed ore.
  • the amount of H 2 SO 4 is generally 150 to 500 kg per tonne of crushed ore, and preferably 300 to 500 kg per tonne of crushed ore. It can optionally be introduced so as to continuously maintain a low acid pH, since this is favorable to the non-solubilization of iron.
  • the hot solubilization treatment is carried out in an autoclave at medium or high pressure, for example under a pressure of 7 to 40 bars, and it is carried out at temperatures of 100 to 250 ° C., preferably from 150 to 200 ° C, and better still 180 ° C.
  • the autoclave is preheated to 100 ° C. with live steam, then the whole is heated to the desired final temperature with live steam so as to reach the pulp ratio favorable for good attack. This temperature is then maintained for the desired duration which is generally from 1 to 8 h, which makes it possible to obtain a satisfactory solubilization of the nickel, copper and cobalt.
  • the second pulp leaving the autoclave is then subjected to a separation (in 19) in order to obtain (in 21) a liquid phase containing mainly nickel, copper and cobalt.
  • the solid phase is then subjected to washing with water (at 22), the washing water being able to be recycled (at 23) completely or partly in the autoclave for the treatment of solubilization of copper, nickel and cobalt with sulfuric acid.
  • the washed solid phase 24 is then rejected in the form of waste rock which constitutes the manganiferous residues having a higher manganese content than the starting ore.
  • nickel, copper and cobalt can be recovered by various treatments. Generally, this is achieved by precipitation of the corresponding sulfides at 25.
  • a precipitation of the copper sulfide CuS is carried out using H 2 S, then the pH of the residual solution is adjusted using calcium carbonate to then precipitate the nickel and cobalt sulphides by the action of H 2 S. After the separation of the precipitates, the solution obtained which contains manganous sulphate is recycied (at 8) at the stage of preparation of the second pulp.
  • the quantities of crushed nodules distributed respectively in the first part and the second part of the crushed ore are chosen so as to have the desired quantity of manganous sulfate for the solubilization treatment stage.
  • nickel, copper and cobalt performed on the second pulp.
  • This quantity which is generally 50 to 250 kg of manganous sulphate in solution per tonne of crushed ore, is provided, on the one hand, by the solution for treating the first pulp with SO 2 , and by the manganous ions which iron in sulfuric solution and which come from the manganese enrichment of the ore used to prepare the second pulp.
  • the ore is generally divided into a first part which represents 10 to 15% by weight of the treated ore, the second part representing from 85 to 90% of the treated ore.
  • a tonne of ground nodules is treated, distributed as follows: 121 kg for the first part of nodules and 879 kg for the second part, which corresponds to manganese contents of 35 , 1 kg for the first part and 255 kg for the second part.
  • the yield is 95% and 33.3 kg of manganese go into solution.
  • the enrichment of the ore with the recycled manganous sulphate solution leads to a manganese content of 309 kg.
  • the solid phase recovered (at 24) has a manganese content of 35%, which corresponds to 288.3 kg of manganese.
  • the desired amount of manganese can be recovered from this solid phase, in the form of ferro or silicomanganese, by direct conventional pyrometallurgical treatments, after a pelletizing step.
  • a pulp can be prepared from the solid phase and subjected to reduction by an appropriate reducing agent such as SO 2 , H 2 S, a carbohydrate or an alcohol.
  • an appropriate reducing agent such as SO 2 , H 2 S, a carbohydrate or an alcohol.
  • this pulp can be reacted with sulfuric acid in the presence of an organic reducing agent such as a carbohydrate or an alcohol.
  • This example illustrates the fixation of the manganese present in a solution of manganous sulphate on ground nodules.
  • the ground nodules are brought into contact with the MnSO 4 solution against the current to obtain self-regulation of the pH by the basicity of the nodule.
  • the oxidation of the nodules by Mn 2+ releases an acidity equivalent to the quantity of sulfuric acid necessary for the neutralization of the alkali and alkaline earth metals present in the nodules.
  • This countercurrent contacting is carried out in three stages with a manganous sulphate solution containing 25 g -1 of manganese, a pulp ratio equal to 3 and a residence time of one hour in each stage.
  • a manganous sulphate solution containing 25 g -1 of manganese, a pulp ratio equal to 3 and a residence time of one hour in each stage.
  • the manganese fixing yield is 71%.
  • the manganese nodule content is then 32.6% and the Mn concentration of the outgoing solution is 7 gl -1 .
  • the disproportionation yield of manganese fixed on the nodules is studied, during the reaction with sulfuric acid, in an autoclave, at different temperatures, for 2 h, using different quantities of sulfuric acid and a ratio of pulp equal to 2.
  • step g) of dissolving the nickel, copper and cobalt on the second pulp were used to carry out step g) of dissolving the nickel, copper and cobalt on the second pulp.
  • the manganous sulphate introduced into the autoclave was partly produced by reduction of the first pulp by means of SO 2 and for the other part by re-solution in the autoclave of the fraction of manganese carried by the nodules enriched with manganese of the second pulp.
  • step d) of preparation of a manganous sulfate solution by treatment of the ground ore with sulfuric acid in the presence of sucrose.

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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)
  • Ocean & Marine Engineering (AREA)
  • Oceanography (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Extraction Or Liquid Replacement (AREA)
EP85401080A 1984-06-07 1985-05-31 Procédé de traitement de minerais complexes de manganèse tels que les nodules marins Expired EP0165166B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8408924 1984-06-07
FR8408924A FR2565600B1 (fr) 1984-06-07 1984-06-07 Procede de traitement de minerais complexes de manganese tels que les nodules marins

Publications (2)

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EP0165166A1 EP0165166A1 (fr) 1985-12-18
EP0165166B1 true EP0165166B1 (fr) 1988-03-02

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EP85401080A Expired EP0165166B1 (fr) 1984-06-07 1985-05-31 Procédé de traitement de minerais complexes de manganèse tels que les nodules marins

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US (1) US4620964A (enrdf_load_stackoverflow)
EP (1) EP0165166B1 (enrdf_load_stackoverflow)
JP (1) JPS613848A (enrdf_load_stackoverflow)
CA (1) CA1245458A (enrdf_load_stackoverflow)
DE (1) DE3561748D1 (enrdf_load_stackoverflow)
FR (1) FR2565600B1 (enrdf_load_stackoverflow)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2612173B1 (fr) * 1987-03-10 1991-04-19 Japan Metals & Chem Co Ltd Procede de preparation de composes de manganese de haute purete
KR100225477B1 (ko) * 1997-07-10 1999-10-15 이경운 망간단괴를 이용한 폐수중의 중금속 흡착,제거방법
RU2261923C1 (ru) * 2004-05-31 2005-10-10 Всероссийский научно-исследовательский институт минерального сырья им. Н.М. Федоровского (ВИМС) Способ переработки кобальтоносных железомарганцевых корковых образований
DE202008006167U1 (de) 2008-05-06 2008-07-17 Terex-Demag Gmbh Seitlich abgespannter Gittermast
CN105565387A (zh) * 2016-03-17 2016-05-11 仇颖莹 一种利用高炉灰制备饲料级硫酸锰的方法
CN111807598B (zh) * 2020-06-18 2022-03-11 西南科技大学 一种电场协同磷尾矿无害化处理电解锰渣渗滤液的方法

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2450870A (en) * 1945-09-20 1948-10-12 Chatham Chemical Company Process of making manganous sulfate
US2539823A (en) * 1949-11-22 1951-01-30 Lunsford Long W Manganese ore treatment
US3018234A (en) * 1959-02-09 1962-01-23 Peter S Litt Process for treating a manganese containing ore for the recovery of manganese values therefrom
US3085875A (en) * 1960-01-04 1963-04-16 Howe Sound Co Treatment of manganese ores
US3169856A (en) * 1962-05-22 1965-02-16 John L Mero Process for separation of nickel from cobalt in ocean floor manganiferous ore deposits
US3723095A (en) * 1970-07-16 1973-03-27 Kennecott Copper Corp Extraction of copper and nickel from manganese nodules
DE2150785C2 (de) * 1971-10-12 1973-07-12 Preussag Ag Verfahren zur Gewinnung eines Manganoxidkonzentrats,von metallischem Kupfer,Nickel und Kobalt aus Manganerzen
US3810827A (en) * 1972-05-08 1974-05-14 Deepsea Ventures Inc Method for separating metal values from ocean floor nodule ore
US3923615A (en) * 1972-07-17 1975-12-02 Deepsea Ventures Inc Winning of metal values from ore utilizing recycled acid leaching agent
FR2262699B1 (enrdf_load_stackoverflow) * 1974-02-28 1976-12-10 Commissariat Energie Atomique
CA1077725A (en) * 1975-02-27 1980-05-20 Kohur N. Subramanian Process for obtaining metal values by leaching raw sea nodules
CA1043576A (en) * 1975-06-10 1978-12-05 Inco Limited Two stage leaching of limonitic ore and sea nodules
CA1036829A (en) * 1975-07-30 1978-08-22 Kohur N. Subramanian Two stage sulfuric acid leaching of sea nodules
FR2492844A1 (fr) * 1980-10-29 1982-04-30 Pechiney Ugine Kuhlmann Valorisation de cuivre, nickel et cobalt par traitement de minerais oxydes a matrice manganifere
FR2533587A1 (fr) * 1982-09-27 1984-03-30 Commissariat Energie Atomique Procede de traitement de minerais complexes de manganese, en particulier de nodules manganiferes

Also Published As

Publication number Publication date
US4620964A (en) 1986-11-04
JPH0585623B2 (enrdf_load_stackoverflow) 1993-12-08
CA1245458A (en) 1988-11-29
EP0165166A1 (fr) 1985-12-18
FR2565600A1 (fr) 1985-12-13
DE3561748D1 (en) 1988-04-07
FR2565600B1 (fr) 1992-08-14
JPS613848A (ja) 1986-01-09

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