WO2005098062A1 - Extraction hydrometallurgique sans dechets de magnesium et d'autres metaux a partir de formations rocheuses a teneur d'olivine variable - Google Patents

Extraction hydrometallurgique sans dechets de magnesium et d'autres metaux a partir de formations rocheuses a teneur d'olivine variable Download PDF

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Publication number
WO2005098062A1
WO2005098062A1 PCT/AM2005/000001 AM2005000001W WO2005098062A1 WO 2005098062 A1 WO2005098062 A1 WO 2005098062A1 AM 2005000001 W AM2005000001 W AM 2005000001W WO 2005098062 A1 WO2005098062 A1 WO 2005098062A1
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WIPO (PCT)
Prior art keywords
metals
magnesium
dissolution
rocks
rock
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PCT/AM2005/000001
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English (en)
Inventor
Hovhannes Hovhannisyan
Stepan Abovyan
Gagik Karamyan
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Hovhannes Hovhannisyan
Stepan Abovyan
Gagik Karamyan
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Application filed by Hovhannes Hovhannisyan, Stepan Abovyan, Gagik Karamyan filed Critical Hovhannes Hovhannisyan
Publication of WO2005098062A1 publication Critical patent/WO2005098062A1/fr

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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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/04—Blast roasting
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
    • 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
    • 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
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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

  • This invention relates to the methods of extraction of metals, their chlorides, oxides, hydroxides from the rocks and can be used for wasteless, complete and environmentally sound extraction of valuable products from ultrabasic rocks and their metamorphic varieties such as serpentinites, hardwoods, etc, as well as basic rocks which are transient from ultrabasic to basic, wherein content of olivine and its varieties is from 5 to 50 %.
  • the most related method by technical essence consists in processing of metamorphic formation of ultramafic rocks and minerals, namely serpentinite and forsterite, by their crushing and grinding, and subsequent dissolution in hydrochloric acid resulting in dissolved fraction in the form of magnesium chloride, and undissolved fraction in the form of silicon dioxide [2].
  • magnesium chloride is transformed into magnesium hydroxide which is saturated by carbon dioxide to form MgCO 3 .
  • MgCO 3 magnesium hydroxide which is saturated by carbon dioxide to form MgCO 3 .
  • the disadvantage of this method is the limited utility conditioned by extraction and enrichment of only serpentinite and forsterite rocks containing 90% of magnesium and silicon compounds. Besides, in mentioned method the most useful products obtained after dissolution of the rock remain untapped.
  • the objective of presented invention is integrated extraction of all useful products from the ultrabasic rocks and their metamorphic varieties, such as serpentinites, hardwoods, etc., as well as basic transition (from ultrabasic to basic) rocks, such as norites, habro-norites, olivinic habro, anorthosites and troctolites, wherein the amount of rockforming mineral, olivine (Mg,Fe) 2 SiO 4 , and its metamorphic varieties is in the range 5 - 50 %. Disclosure of the Invention
  • the essence of the invention consists in wasteless method of metals and their compounds extraction from ultrabasic and transition (from ultrabasic to basic) rocks, comprising the stages of crushing and grinding of said rocks with following dissolution in hydrochloric acid and obtaining the dissolved part in the form of chlorides of magnesium and other metals, and undissolved part in the form silicon dioxide and other minerals, according to the invention, the silicate part of the rockforming mineral olivine and its metamorphic varieties are subjected to dissolution, said minerals before dissolution they are calcined, the mixture obtained in the result of dissolution is separated by precipitation on dissolved and solid undissolved parts, magnesium chloride and other salts are separated and transferred into corresponding oxides and hydroxides, which then are reduced to the metallic form, while undissolved part of the rock is separated, from which SiO 2 is extracted, washed, dewatered and dried.
  • the original rock is grinded up to grain size less than 1 mm that is calcined at temperatures bellow 1000 °C during time interval 5 - 120 min.
  • Magnesium chloride and other salts are separated and purified by the methods of electro-membrane separation or chemical precipitation. The separation of undissolved part is performed by chemical, gravitational or electromagnetic methods. With the aim of production of pure and extrapure metals the obtained hydroxides and oxides are subjected to selective reduction by the methods of hydrogen, cathodic or high temperature metallurgical vacuum electron-beam reduction and casting depending on nature of metal and necessary purity.
  • ED* - electro-membrane The embodiment of the invention can be illustrated as following.
  • Basic and ultrabasic rocks manifested by massifs containing from 50 to 95 % of rockforming mineral olivine, with depth occurrence of 2000 m and more, are recovered from the deposit by known methods, like excavation, whereupon they are crushed, grinded up to particle size less than 1 mm, calcined if necessary, for water removal and activation at temperature up to 1000 °C during time interval from 5 to 120 min.
  • silicate part of the of rockforming mineral olivine and its metamorphic varieties is dissolved in diluted hydrochloric acid having concentration of 10 - 30 % of concentrated acid, predominantly 20%.
  • Dissolution of the rockforming mineral olivine (Mg,Fe) 2 SiO 4 by hydrochloric acid may be presented by following general formula:
  • the process of dissolution is carried out in closed cycle during time interval from 5 to 300 min depending on extent of rock powdering, its activity and acid concentration.
  • hydrochloric acid is regenerated and recycled by special pipeline back to the dissolution stage.
  • Silicon dioxide and undissolved metals and minerals are separated by modern separation technique such as gravitational, chemical, electromagnetic, while SiO 2 intended for production as 99 % purity powder is washed, dewatered, dried and stored.
  • SiO 2 is subjected to additional chemical purification and directed into the vacuum electron-beam furnace.
  • Other undissolved mineral species and native metals amounting 0.1 - 1.0 % of the rock are subjected to selective enrichment by the gravitational, electromagnetic and chemical methods, then with the aim of production of pure and extrapure metals, these materials are subjected to selective reduction by the methods of hydrogen, cathodic, or high temperature metallurgical vacuum electron-beam reduction and casting.
  • Dissolved rock species in the form of chlorides of magnesium and other metals are separated and purified by the methods of electro-membrane separation or chemical precipitation, therewith MgCl 2 is transferred to Mg(OH) 2 and then to MgO.
  • Remaining metal chlorides similar to above mentioned process are converted into corresponding hydroxides and oxides with subsequent electrochemical regeneration and recovering of hydrochloric acid and water back to the dissolution stage.
  • the hydroxides and oxides including MgO are subjected to selective reduction by the methods of hydrogen, cathodic, or high temperature metallurgical vacuum electron-beam reduction and casting depending on nature of metal and necessary purity.
  • Produced MgO after high temperature treatment can be used for production of refractory materials, dead-burned magnesia for medicine and agriculture as high quality mineral fertilizer, or in combination with MgCl 2 for Sorel cement production.
  • Dunites represent about 15% of the all ultrabasic rocks.
  • dunite was used from rock pieces with the size of 200 - 500 mm.
  • it is grinded by jaw and conic breakers up to average size of 20 mm.
  • humidity of the crushed rock was determined by drying of definite mass in the oven at temperature of 120 °C up to constant weight. If humidity is more than 2 %, the crushed rock before further powdering is calcined up to 600 °C during 2 hours for full dewatering and activation, then the preliminary crushed rock is grinded up to particle size of 0.9 mm in ball mill.
  • the undissolved part of rock is separated onto 400 g of SiO 2 and 8 g of chromospinelides (FeCr 2 O 4 ) which were dried in oven during 2 hours.
  • the resulting product is 99 % silicon dioxide and pure chromospinelide in the form of powder with micronsize particles.
  • Dissolved rock components mainly MgCl 2 and FeCI 2 , were separated by addition of ammonium hydroxide NH 4 OH (about 50 g) up to solution pH of 5-6 resulting in precipitation of iron hydroxide, Fe(OH) 2 , which is extracted by separation on the centrifuge.
  • the solution is returned back for further extraction of magnesium hydroxide, Mg(OH) 2 by increasing of pH value up to 1 1-12 which is performed by addition of ammonium hydroxide in amount of 100 g.
  • the obtained magnesium hydroxide is subjected to treatment in electrodialysis apparatus with applied voltage of 8 - 10 V.
  • the pure and extrapure magnesium hydroxide is obtained.
  • the pure and extrapure iron hydroxides Fe(OH) 2 are produced by cleaning them from impurities.
  • the content of magnesium and iron hydroxides is 75 and 20% of all dissolved part.
  • the ions of other metallic admixtures which amount is less than 1 % can be extracted by the same method.
  • the magnesium and iron hydroxides are subjected to heat treatment at temperatures over 600 °C, whereupon 420 g of MgO and 95 g of Fe O 3 are obtained in the form of pure fine powder with particle size of 10 microns.
  • the extracted oxides in the form of powder are filled into the molds positioned into the vacuum furnace. After evacuation up to pressure of 10 "4 torr the furnace was heated up to melting temperatures, 1 100 °C for iron and 1900 °C for magnesium. After cooling up 65 g of reduced iron and 250 g of magnesium were removed from the molds in the form of ingots with purity of 99.99%.
  • the troctolite was selected in the form of pieces with dimensions of 300-700 mm.
  • it is crushed by jaw and conic breakers up to average size of 20 mm.
  • humidity of the crushed rock was determined by drying of the definite mass in the oven at temperature of 120 °C up to constant weight. If humidity is more than 2%, the crushed rock before further powdering is calcined up to 800 °C during 2 hours for full dewatering and activation, then the preliminary crushed rock is grinded up to particle size of 0.7 mm in ball mill.
  • the extracted silicon dioxide and small admixtures amounting about 2 % and consisting mainly from chromospinelides with high quantity of aluminum (about 17% of the total chemical content) were separated on the gravitational table SKO-5 with simultaneous washing and with subsequent water cleaning and turning back.
  • the undissolved part of rock is separated onto 360 g of SiO 2 and 20 g of chromospinelides (FeCr 2 O 4 ) which were dried in oven at 200 °C during 2 hours.
  • the resulting product is 99 % silicon dioxide and pure chromospinelide in the form of powder with micronsize particles.
  • Dissolved rock components mainly MgCl 2 and FeCI , were separated by addition of ammonium hydroxide NH OH (about 50 g) up to solution pH of 5-6 which results in precipitation of iron hydroxide, Fe(OH) 2 , which were extracted by separation on the centrifuge.
  • ammonium hydroxide was introduced into the solution changing pH value up to 8 resulting in aluminum hydroxide precipitation. Then centrifugal extraction of these metal hydroxides is carried out, first iron and then aluminum.
  • Solution containing MgCl 2 is returned back and subjected to further treatment for extraction of magnesium hydroxide, Mg(OH) 2 by increasing of pH value up to 1 1-12 which is performed by addition of ammonium hydroxide in amount of 100 g.
  • Mg(OH) 2 For obtaining pure (99%) and extrapure (99.99%) hydroxides the obtained magnesium hydroxide is subjected to treatment in electrodialysis apparatus.
  • pure and extrapure iron and aluminum hydroxides are produced by cleaning them from impurities.
  • 30% of Mg(OH) 2 45% of AI(OH) 3 and 15% of Fe(OH) 2 are obtained.
  • the ions of other metallic admixtures which amount is less than 1.5 % of overall rock content may be extracted by the same method.
  • the magnesium, aluminum and iron hydroxides are subjected to heat treatment at temperatures over 700 °C.
  • 150 g of MgO, 220 g Al O 3 and 70 g of Fe 2 O 3 are obtained in the form of pure fine powder with particle size of 10 microns.
  • the extracted oxides in the powder form are filled into the mold positioned into the vacuum oven. After evacuation up to pressure of 10 "4 torr the furnace was heated up to melting temperatures, 1 100 °C for iron, 1750 °C for aluminum and 1900 °C for magnesium.
  • proposed method provides integrated extraction of all valuable products from ultrabasic rocks and their metamorphic varieties such as serpentinites, hardwoods, etc, as well as from basic transient rocks including norites, habro-norites, olivinic habro, anortosites and troctolites, wherein the content of rockforming mineral olivine (MgFe) SiO 4 and its metamorphic varieties varies from 5 to 50 %.
  • rockforming mineral olivine (MgFe) SiO 4 and its metamorphic varieties varies from 5 to 50 %.
  • the invention has been made owing to versatile geological, petrographycal, mineralogical, physical and chemical methods of rock investigations, as well as studying of heterogeneous processes simulating geomorphology of minerals in the nature, which made it possible to understand the mechanisms of the dissolution processes of various mineral including basic rocks.

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

Abstract

La présente invention a trait à des procédés d'extraction de métaux, de leurs chlorures, oxydes et hydroxydes à partir de roches ultrabasiques et basiques. Ce procédé exempt de déchets comprend les étapes suivantes : le broyage et la pulvérisation des roches, suivie d'une lixiviation dans l'acide chlorhydrique avec obtention d'une partie dissoute sous forme de chlorures de magnésium et d'autres métaux, et d'une partie solide non dissoute sous forme de dioxyde de silicium et d'autres minéraux. Selon l'invention, la partie silicate d'olivine minérale formant les roches et ses variétés métamorphiques est, de préférence, calcinée préalablement à la dissolution. Le mélange de lixiviation obtenu dans le procédé de dissolution est séparé par précipitation en fractions liquide et solide. Ensuite, la fraction dissoute est transformée en oxydes et hydroxydes, qui sont alors réduits en métaux élémentaires, tandis que le dioxyde de silicium est séparé de la partie non dissoute, lavé et séché. L'invention permet une extraction intégrée de tous les produits de valeur à partir desdites roches et leurs variétés métamorphiques.
PCT/AM2005/000001 2004-04-05 2005-03-22 Extraction hydrometallurgique sans dechets de magnesium et d'autres metaux a partir de formations rocheuses a teneur d'olivine variable WO2005098062A1 (fr)

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AMP20040044 2004-04-05

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2451567A1 (es) * 2012-09-26 2014-03-27 Pasek Minerales, S.A.U. Procedimiento de obtención de óxido e hidróxido de magnesio de alta pureza a partir de dunitas
US11718558B2 (en) 2019-08-13 2023-08-08 California Institute Of Technology Process to make calcium oxide or ordinary Portland cement from calcium bearing rocks and minerals

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54134097A (en) * 1978-04-11 1979-10-18 Kimura Kakoki Co Ltd Method of recovering silicic acid from waste water
GB2068348A (en) * 1979-12-06 1981-08-12 Veitscher Magnesitwerke Ag A process for the separation of ferrous, aluminous and manganous contaminations from hydrochloric magnesium chloride solutions
RO81088A2 (fr) * 1979-05-16 1983-02-01 Centrul De Chimie,Ro Procede d'obtention de l'oxyde de magnesium de serpentinite
CN1041740A (zh) * 1988-10-08 1990-05-02 张天中 以蛇纹石为原料生产碳酸镁和/或氧化镁及多孔性二氧化硅的方法
US4944928A (en) * 1987-06-26 1990-07-31 Veitscher Magnestiwerke-Actien-Gesellschaft Process for producing pure magnesium oxide
EP0434053A1 (fr) * 1989-12-20 1991-06-26 Nisshin Steel Co., Ltd. Procédé de traitement de minerais de nickel-magnésium silicatés
RU2109078C1 (ru) * 1992-11-16 1998-04-20 Минерал Дивелопмент Интернешнл А/С Способ получения металлического магния, способ получения чистого оксида магния (варианты) и способ переработки исходного материала
US5900151A (en) * 1996-11-13 1999-05-04 Norsk Hydro Asa Method for sulphate removal magnesium chloride brine

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54134097A (en) * 1978-04-11 1979-10-18 Kimura Kakoki Co Ltd Method of recovering silicic acid from waste water
RO81088A2 (fr) * 1979-05-16 1983-02-01 Centrul De Chimie,Ro Procede d'obtention de l'oxyde de magnesium de serpentinite
GB2068348A (en) * 1979-12-06 1981-08-12 Veitscher Magnesitwerke Ag A process for the separation of ferrous, aluminous and manganous contaminations from hydrochloric magnesium chloride solutions
US4944928A (en) * 1987-06-26 1990-07-31 Veitscher Magnestiwerke-Actien-Gesellschaft Process for producing pure magnesium oxide
CN1041740A (zh) * 1988-10-08 1990-05-02 张天中 以蛇纹石为原料生产碳酸镁和/或氧化镁及多孔性二氧化硅的方法
EP0434053A1 (fr) * 1989-12-20 1991-06-26 Nisshin Steel Co., Ltd. Procédé de traitement de minerais de nickel-magnésium silicatés
RU2109078C1 (ru) * 1992-11-16 1998-04-20 Минерал Дивелопмент Интернешнл А/С Способ получения металлического магния, способ получения чистого оксида магния (варианты) и способ переработки исходного материала
US5900151A (en) * 1996-11-13 1999-05-04 Norsk Hydro Asa Method for sulphate removal magnesium chloride brine

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
DATABASE COMPENDEX [online] October 1968 (1968-10-01), YAMADA T. ET AL.: "Extraction of magnesia from calcined serpentine", XP002331926, Database accession no. EIX19690025214 *
DATABASE WPI Section Ch Week 197948, Derwent World Patents Index; Class A60, AN 1979-86526B, XP002331888 *
DATABASE WPI Section Ch Week 198335, Derwent World Patents Index; Class A97, AN 1983-751197, XP002331927 *
DATABASE WPI Section Ch Week 199106, Derwent World Patents Index; Class E33, AN 1991-037189, XP002331928 *
GABRA G: "A PROCESS FOR THE PRODUCTION OF MAGNESIUM OXIDE FROM SERPENTINE BY SULFUR DIOXIDE LEACHING AND SOLVENT EXTRACTION", HYDROMETALLURGY, ELSEVIER SCIENTIFIC PUBLISHING CY. AMSTERDAM, NL, vol. 13, no. 1, October 1984 (1984-10-01), pages 1 - 13, XP001165313, ISSN: 0304-386X *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2451567A1 (es) * 2012-09-26 2014-03-27 Pasek Minerales, S.A.U. Procedimiento de obtención de óxido e hidróxido de magnesio de alta pureza a partir de dunitas
US11718558B2 (en) 2019-08-13 2023-08-08 California Institute Of Technology Process to make calcium oxide or ordinary Portland cement from calcium bearing rocks and minerals

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