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WO2015009077A1 - Procédé de préparation de composé de manganèse et de sulfate de potassium à partir d'inclusion de potassium et de manganèse de faible pureté - Google Patents

Procédé de préparation de composé de manganèse et de sulfate de potassium à partir d'inclusion de potassium et de manganèse de faible pureté Download PDF

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Publication number
WO2015009077A1
WO2015009077A1 PCT/KR2014/006497 KR2014006497W WO2015009077A1 WO 2015009077 A1 WO2015009077 A1 WO 2015009077A1 KR 2014006497 W KR2014006497 W KR 2014006497W WO 2015009077 A1 WO2015009077 A1 WO 2015009077A1
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Prior art keywords
manganese
potassium
sulfate
leachate
purity
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PCT/KR2014/006497
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English (en)
Korean (ko)
Inventor
김명준
트란탐
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Industry Foundation of Chonnam National University
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Industry Foundation of Chonnam National University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/16—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/10—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention relates to a method for producing a high purity manganese compound and a high purity potassium sulfate from a low purity manganese and potassium content, and more particularly to a method for producing a high purity manganese compound and a high purity potassium sulfate through one process.
  • Manganese oxide is widely used in the production of a positive electrode, which is one of the components of the secondary battery, and the demand for this is also rapidly increasing.
  • Korean Patent Laid-Open Publication No. 10-2011-76109 discloses a method for the simultaneous production of a valuable metal compound and potassium sulfate from manganese nodules
  • Patent Publication No. 10-2012-93948 discloses MnSO from a low to medium quality MnO 2 ore. 4, and it discloses a method for producing a H 2 O
  • Laid-Open Patent Publication No. 10-2011-111057 discloses a manufacturing method of a crystalline sasanhwasam manganese, lithium-manganese oxide.
  • an object of the present invention is to economically produce high purity manganese compounds (manganese sulfate monohydrate, trimanganese tetraoxide and Electronic Manganese Metal) and high purity potassium sulfate simultaneously from low purity manganese and potassium content in one process.
  • high purity manganese compounds manganese sulfate monohydrate, trimanganese tetraoxide and Electronic Manganese Metal
  • potassium is added through a first solid-liquid separation after adding water to the low purity manganese and potassium content.
  • the sulfide includes at least one of sodium sulfide (Na 2 S), calcium sulfide (CaS) and hydrogen sulfide (H 2 S), the sulfide is 2 to the total molar amount of the first impurity 5 times may be added after dissolving in water to remove the first impurity.
  • the method may further include obtaining a second potassium leachate from which the first impurity is removed through solid-liquid separation after removing the first impurity.
  • It may include the step of obtaining high-purity potassium sulfate by precipitating with potassium sulfate by adding sulfuric acid or sodium sulfate of 0.1 to 3 times the potassium molar ratio to the second potassium leaching solution.
  • the high purity manganese compound includes at least one of manganese sulfate monohydrate (MnSO 4 ⁇ H 2 O), trimanganese tetraoxide (Mn 3 O 4 ), and electronic manganese metal (EMM).
  • Sulfuric acid added to the first solid may be added by dilution in water at a ratio of 0.1 to 3 times the molar content contained in the first solid.
  • calcium hydroxide may be added to pH 4 or more to remove iron in the second impurity.
  • the sulfide may be added at a ratio of 2 to 50 times the total molar amount of the second impurity other than the removed iron to remove the second impurity other than the iron.
  • the preparing of the high purity manganese compound may include obtaining potassium manganese sulfate solution by sequentially adding potassium hydroxide and sulfuric acid to the manganese leachate; Drying the aqueous manganese sulfate solution may comprise the step of preparing a high purity manganese sulfate monohydrate.
  • the potassium hydroxide may be added to pH 6 to pH 9 of the manganese leaching solution under a non-oxidizing atmosphere so that manganese hydroxide is precipitated.
  • the sulfuric acid may be added at a ratio of 0.1 to 3 times the molar content of manganese hydroxide contained in the manganese hydroxide to obtain an aqueous manganese sulfate solution.
  • the preparing of the high purity manganese compound may include obtaining potassium manganese sulfate solution by sequentially adding potassium hydroxide and sulfuric acid to the manganese leachate; It may include the step of producing an electronic manganese metal (EMM) using the electrolytic extraction method of the aqueous manganese sulfate.
  • EMM electronic manganese metal
  • the potassium hydroxide may be added to pH 6 to pH 9 of the manganese leaching solution under a non-oxidizing atmosphere so that manganese hydroxide is precipitated.
  • the sulfuric acid may be added at a ratio of 0.1 to 3 times the molar content of manganese hydroxide contained in the manganese hydroxide to obtain an aqueous manganese sulfate solution.
  • the heat treatment of the manganese hydroxide in an oxidizing atmosphere may include the step of quenching to prepare trimanganese tetraoxide.
  • the potassium hydroxide may be added to pH 6 to pH 9 of the manganese leaching solution under a non-oxidizing atmosphere.
  • the above object in the method for producing potassium sulfate from the low-purity manganese and potassium-containing, in which a potassium is included through the solid-liquid separation after adding water to the low-purity manganese and the potassium-containing Separating the potassium leach solution and the solid; Dissolving sulfide in the first potassium leachate by adding 2 to 5 times the total molar amount of impurities in water and then removing impurities; After obtaining the second potassium leaching solution from which the impurities have been removed through solid-liquid separation, high purity potassium sulfate is obtained by adding 0.1 to 3 times sulfuric acid or sodium sulfate of potassium molar ratio contained in the second potassium leaching solution and precipitating with potassium sulfate. It can be achieved by a method for preparing potassium sulfate from low purity manganese and potassium containing comprising the step of.
  • the above object in the method for producing manganese sulfate monohydrate from low-purity manganese and potassium containing, potassium is included through the solid-liquid separation after adding water to the low-purity manganese and potassium containing Separating the potassium leach solution and the solid; Converting the solid into manganese sulfate by roasting with the addition of sulfuric acid; Dissolving the manganese sulfate in water and then removing impurities using at least one of calcium hydroxide and sulfide to obtain a manganese leachate; Sequentially adding potassium hydroxide and sulfuric acid to the manganese leachate to obtain an aqueous manganese sulfate; It can be achieved by a method for preparing manganese sulfate monohydrate from a low purity manganese and potassium containing comprising drying the aqueous manganese sulfate solution to produce a high purity manganese sulfate monohydrate.
  • EMM Electronic Manganese Metal
  • potassium is added through solid-liquid separation after adding water to the low-purity manganese and potassium-containing Separating the potassium leach solution and the solid contained; Converting the solid into manganese sulfate by roasting with the addition of sulfuric acid; Dissolving the manganese sulfate in water and then removing impurities using at least one of calcium hydroxide and sulfide to obtain a manganese leachate; Sequentially adding potassium hydroxide and sulfuric acid to the manganese leachate to obtain an aqueous manganese sulfate;
  • the aqueous manganese sulfate solution may be achieved by a method of producing EMM (Electronic Manganese Metal) from low-purity manganese and potassium containing the step of producing an electronic manganese metal (EMM) using an electrolytic extraction method.
  • the above object in the method for producing trimanganese tetraoxide from a low-purity manganese and potassium-containing, potassium containing potassium through the solid-liquid separation after adding water to the low-purity manganese and potassium-containing Separating the leachate from the solid; Converting the solid into manganese sulfate by roasting with the addition of sulfuric acid; Dissolving the manganese sulfate in water and then removing impurities using at least one of calcium hydroxide and sulfide to obtain a manganese leachate; Precipitating manganese hydroxide using potassium hydroxide in the manganese leachate;
  • the manganese hydroxide may be achieved by a method of preparing trimanganese tetraoxide from low purity manganese and potassium containing the step of quenching the heat treatment in an oxidizing atmosphere to prepare trimanganese tetraoxide.
  • a high-purity manganese compound (manganese sulfate monohydrate, trimanganese tetraoxide and Electronic Manganese Metal (EMM) and high-purity potassium sulfate) can be economically obtained from a low-purity manganese and potassium-containing material in one process.
  • EMM Electronic Manganese Metal
  • Methods of making are provided.
  • FIG. 1 is a schematic flowchart of preparation of high purity manganese compound and high purity potassium sulfate according to an embodiment of the present invention
  • FIG. 3 is a flowchart of manufacturing a high purity manganese compound according to an embodiment of the present invention.
  • 1 is a schematic flowchart of preparation of high purity manganese compound and high purity potassium sulfate according to an embodiment of the present invention.
  • Sulfide is added to the first potassium leachate separated through the first solid solution separation to remove the first impurity (S130), and sulfuric acid or sodium sulfate is added to prepare high purity potassium sulfate (S140).
  • step S210 Adding sulfuric acid to the first solid separated in step S120 and roasting to convert it to manganese sulfate (S210), and adding sulfide and potassium hydroxide to remove the second impurity to obtain manganese leachate (S220);
  • step S230 Adding potassium hydroxide and sulfuric acid to the manganese leachate (S230), and drying the manganese sulfate solution to obtain a high purity manganese sulfate monohydrate (S240).
  • the potassium hydroxide used in steps S220 and S230 may be used using the first potassium leachate of step S120.
  • the manganese sulfate aqueous solution obtained in step S230 may be prepared by using an electrowinning method (Electrowinning) EMM (Electronic Manganese Metal) (S310).
  • EMM Electro Manganese Metal
  • step S410 the step of precipitating manganese hydroxide using potassium hydroxide in the manganese leachate obtained in step S220 (S410), and drying and quenching the manganese hydroxide to prepare a high-purity trimanganese tetraoxide (S420).
  • the potassium hydroxide of step S410 may also use the first potassium leach solution of step S120.
  • the present invention provides a method for producing potassium sulfate, manganese sulfate monohydrate, EMM and trimanganese tetraoxide from low purity manganese and potassium content through one process.
  • FIG. 2 is a flowchart of high purity potassium sulfate production according to an embodiment of the present invention.
  • the low-purity manganese and potassium-containing products leach potassium by adding water to low-purity manganese, potassium ore or by-product manganese, potassium dust.
  • potassium hydroxide is leached through a reaction as in Scheme 1 below.
  • the water is added in an amount that can be well stirred by adding about 2 to 4 times, preferably 2 to 3 times, more preferably about 2.5 times, by volume ratio of the low purity manganese and potassium containing.
  • the first solid solution separation is performed to separate the first potassium leachate containing the leached potassium hydroxide and the first solid (S120).
  • the first potassium leachate obtained through the first solid-liquid separation of S120 is used in the next step for the production of high purity potassium sulfate, or of the potassium hydroxide used for the production of high purity trimanganese tetraoxide or the production of high purity manganese sulfate monohydrate. It can be used as a material.
  • the first solid obtained through the first solid-liquid separation of S120 may be used as a material for manufacturing high purity trimanganese tetraoxide, manganese sulfate monohydrate, and EMM which are manganese compounds.
  • Sulfide is added to remove the first impurity in the first potassium leachate of S120 to precipitate the first impurity in the form of sulfide (S130).
  • the first impurity includes heavy metals such as lead (Pb), nickel (Ni), zinc (Zn), cobalt (Co) or copper (Cu).
  • the sulfide includes at least one of sodium sulfide (Na 2 S), calcium sulfide (CaS) and hydrogen sulfide (H 2 S), and is added after dissolving 2 to 5 times the total molar amount of the first impurity in water. Due to the addition of these sulfides, the first impurity precipitates in the form of sulfides (NiS, PbS, ZnS, CoS, CuS).
  • the sulfide slurry is discarded through a second solid-liquid separation to obtain a second potassium leachate from which the first impurity is removed (S131).
  • the second potassium leachate from which the first impurity of S131 is removed is used as a next step for the preparation of high purity potassium sulfate, or as a material of potassium hydroxide used for the production of high purity trimanganese tetraoxide or the preparation of high purity manganese sulfate monohydrate. Can be used.
  • the second potassium leachate of S131 is used as a material of potassium hydroxide used for the production of high-purity trimanganese tetraoxide or a high-purity manganese sulfate monohydrate.
  • Potassium sulfate is precipitated by adding sulfuric acid or sodium sulfate to the second potassium leachate (S141).
  • the sulfuric acid is added 0.1 to 3 times, preferably 0.5 to 2 times the potassium molar ratio.
  • a third solid-liquid separation may be performed to prepare high purity (more than 99%) potassium sulfate (K 2 SO 4 ) as a solid.
  • FIG. 3 is a flowchart of manufacturing high-purity manganese sulfate monohydrate according to an embodiment of the present invention.
  • sulfuric acid is added to the first solid obtained in step S120 of FIG. 2 to be roasted and converted to manganese sulfate (S210).
  • the sulfuric acid to be added is preferably a diluted sulfuric acid, for example, the sulfuric acid in a ratio of 1 to 3 times the molar content of manganese contained in the first solid, preferably in a ratio of 1.5 to 3 times Dilute in water and add.
  • the roasting temperature is roasted to 300 °C to 1000 °C, preferably 500 °C to 800 °C by converting the first solid to manganese sulfate, the reaction scheme is as follows.
  • Manganese leachate is obtained by adding sulfide and potassium hydroxide to manganese sulfate obtained in step S210 to remove the second impurity (S220).
  • This step may include more detailed steps as follows.
  • the first manganese leachate is obtained by adding water to the manganese sulfate obtained in step S210 (S221).
  • a second manganese leachate from which iron is removed is obtained (S223).
  • Calcium hydroxide may be added to remove the iron so that the pH of the first manganese leachate is at least pH4, preferably pH4 to pH5.
  • the iron is removed in the form of Fe (OH) 3 or FeOOH, the reaction is shown in the following scheme.
  • Sulfide is added to the second manganese leachate from which iron is removed to obtain a third manganese leachate from which impurities other than iron are removed (S225).
  • the second manganese leachate from which the iron is removed may further include impurities such as nickel (Ni), lead (Pb), zinc (Zn), cobalt (Co), and copper (Cu) other than iron. Accordingly, sulfides may be added to the second manganese leachate to precipitate and remove impurities other than iron in the form of sulfides.
  • the sulfide comprises sodium sulfide (Na 2 S), calcium sulfide (CaS) and hydrogen sulfide (H 2 S) at least one, the sulfide is a ratio of 2 to 50 times the total molar amount of impurities other than iron, preferably 2 It may be added in a ratio of 10 to 10 times, more preferably in a ratio of 3 to 6 times.
  • the sulfide slurry may be discarded through solid-liquid separation to obtain a third manganese leachate from which impurities other than iron are removed.
  • Potassium hydroxide and sulfuric acid are sequentially added to the third manganese leachate from which the impurities are removed to obtain an aqueous manganese sulfate solution (S230).
  • This step may include more detailed steps as follows.
  • Potassium hydroxide is added to the third manganese leachate to precipitate into manganese hydroxide (S231).
  • Manganese leaching liquid obtained in step S225 is dissolved manganese, magnesium, calcium, potassium, etc., it is necessary to selectively precipitate manganese. Accordingly, the potassium hydroxide solution is diluted to 1 M or more, and added to the third manganese leachate at a temperature of 60 ° C. to 70 ° C. to a pH 6 to pH 9 to precipitate manganese in the form of manganese hydroxide (Mn (OH) 2 ). Be sure to If the pH is lower than the appropriate pH, the recovery of manganese (Mn) is lowered. If the pH is higher than the pH, impurities may be precipitated.
  • the manganese hydroxide may further comprise the step of washing with water in a non-oxidizing atmosphere at a temperature of 60 °C to 90 °C (not shown).
  • the washing may also have the effect of further removing other impurities in the manganese hydroxide.
  • Manganese hydroxide precipitated through the solid-liquid separation is obtained and used in the next step, the solution remaining after obtaining manganese hydroxide may be used in place of water for potassium leaching in step S110.
  • the method may further include neutralizing the solution redissolved with sulfuric acid (not shown).
  • the reagent for the neutralization reaction may use manganese hydroxide in step S231, and the manganese hydroxide used for the neutralization reaction may be neutralized such that the pH of the re-dissolution solution is pH4 to pH6.
  • the obtained manganese sulfate aqueous solution may be dried to obtain a high purity manganese sulfate monohydrate (S240).
  • the drying process may include preparing a high purity manganese sulfate monohydrate by crystallizing the aqueous manganese sulfate solution by performing vacuum evaporation.
  • the appropriate saturated steam pressure for the vacuum evaporation is 0.57 ⁇ 0.7kgf / cm 2 , preferably 0.6 ⁇ 0.6.5kgf / cm 2 , it can be carried out under a temperature of 85 to 90 °C vacuum evaporation.
  • the evaporation point may be lower than 80 ° C., thereby producing manganese sulfate pentahydrate (MnSO 4 ⁇ 5H 2 O) instead of manganese sulfate monohydrate (MnSO 4 ⁇ H 2 O).
  • the edge efficiency may be lowered, thereby lowering the economic efficiency.
  • the manganese sulfate solution obtained in step S233 may be used in the manufacture of EMM.
  • the manganese sulfate aqueous solution obtained in step S233 may be prepared by using an electrowinning method (Electrowinning).
  • the manganese hydroxide obtained in the step S231 can be produced in high purity three manganese tetraoxide.
  • the manganese hydroxide obtained in step S231 may be heat-treated at a temperature of 800 ° C. to 1100 ° C. after drying using a dryer. Heat treatment is performed by using equipment such as rotary kiln incinerator, and it is well stirred so that the sample can react sufficiently during heat treatment, so that the oxidizing atmosphere can be achieved. In addition, the quenching treatment is performed after the heat treatment. Manganese from which impurities are removed by the heat treatment is reduced to Mn 2 O 3 , and rapid cooling is performed to oxidize it to Mn 3 O 4 manganese compound. After performing the heat treatment can be cooled to room temperature within a short time. Through this, tri- manganese tetraoxide (Mn 3 O 4 ) that can be used in a secondary battery can be obtained with high purity, and the reaction is shown in the following reaction formula.
  • Mn 3 O 4 tri- manganese tetraoxide
  • the concentration of sulfide is as follows.
  • Sulfide is added at a rate of 10 to 50 times the total molar amount of impurities other than iron, preferably at a rate of 15 to 45 times, more preferably at a rate of 30 to 35 times, and the pH of the added sulfide is pH7 To pH8, preferably adjusted to pH8. After the sulfide is added, the reaction may be performed for about 10 to 100 minutes, preferably 20 to 80 minutes, more preferably 30 to 60 minutes.
  • potassium hydroxide is added so that the pH of the iron-containing manganese leachate is pH 5 to pH 6, about 10 minutes to 60 minutes, preferably 10 minutes to 40 minutes, more preferably Can react for 20 to 30 minutes. That is, when pH is adjusted by adding potassium hydroxide after addition of sulfide, impurities such as nickel, lead, zinc, cobalt, and copper, which are impurities other than iron, form sulfides (NiS, PbS, ZnS, CoS, CuS). It can help to settle, and thus be more effective in removing impurities in the form of sulfides.
  • the method for producing manganese compounds and potassium sulfate from the low purity manganese and potassium content of the present invention can be used for the production of secondary batteries such as portable electronic devices.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention porte sur un procédé de préparation de composés du manganèse à pureté élevée et de sulfate de potassium à pureté élevée à partir d'une inclusion de potassium et de manganèse de faible pureté. Le procédé de préparation de composés de manganèse à pureté élevée et de sulfate de potassium à pureté élevée à partir d'une inclusion de potassium et de manganèse de faible pureté selon la présente invention consiste : à ajouter de l'eau à une inclusion de potassium et de manganèse de faible pureté et ensuite séparer un premier lixiviat de potassium contenant du potassium et un premier solide grâce à un premier processus de séparation solide-liquide ; à ajouter du sulfure de potassium au premier lixiviat de potassium pour enlever une première impureté et préparer du sulfate de potassium à pureté élevée à l'aide d'acide sulfurique ; à ajouter de l'acide sulfurique au premier solide, à griller le mélange pour convertir le mélange en sulfate de manganèse, à enlever une seconde impureté à l'aide de sulfure et/ou hydroxyde de calcium et ensuite obtenir un lixiviat de manganèse grâce à un second processus de séparation solide-liquide ; et à préparer des composés de manganèse à pureté élevée à partir du lixiviat de manganèse. Ainsi, les composés de manganèse à pureté élevée (sulfate de manganèse monohydraté, tétraoxyde de manganèse et manganèse métallique pour l'électronique (EMM)) et le sulfate de potassium à pureté élevée peuvent être simultanément produits à partir de l'inclusion de potassium et de manganèse de faible pureté d'une manière économique.
PCT/KR2014/006497 2013-07-18 2014-07-17 Procédé de préparation de composé de manganèse et de sulfate de potassium à partir d'inclusion de potassium et de manganèse de faible pureté Ceased WO2015009077A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20000013629A (ko) * 1998-08-11 2000-03-06 윤대근 정제 망간염의 제조방법
JP2003272629A (ja) * 2002-03-19 2003-09-26 Toda Kogyo Corp 非水電解質二次電池用正極活物質及びその製造法
KR20100002046A (ko) * 2008-06-25 2010-01-06 동부정밀화학 주식회사 전기로 분진에 포함된 망간 함유 화합물의 회수방법
JP2013076109A (ja) * 2011-09-29 2013-04-25 Jx Nippon Mining & Metals Corp 金属マンガンの電解採取による製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20000013629A (ko) * 1998-08-11 2000-03-06 윤대근 정제 망간염의 제조방법
JP2003272629A (ja) * 2002-03-19 2003-09-26 Toda Kogyo Corp 非水電解質二次電池用正極活物質及びその製造法
KR20100002046A (ko) * 2008-06-25 2010-01-06 동부정밀화학 주식회사 전기로 분진에 포함된 망간 함유 화합물의 회수방법
JP2013076109A (ja) * 2011-09-29 2013-04-25 Jx Nippon Mining & Metals Corp 金属マンガンの電解採取による製造方法

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