WO2013170370A1 - Procédés de récupération d'éléments de terre rare provenant de divers matériaux - Google Patents

Procédés de récupération d'éléments de terre rare provenant de divers matériaux Download PDF

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Publication number
WO2013170370A1
WO2013170370A1 PCT/CA2013/000492 CA2013000492W WO2013170370A1 WO 2013170370 A1 WO2013170370 A1 WO 2013170370A1 CA 2013000492 W CA2013000492 W CA 2013000492W WO 2013170370 A1 WO2013170370 A1 WO 2013170370A1
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WO
WIPO (PCT)
Prior art keywords
leaching
leachate
rare earth
earth element
acid
Prior art date
Application number
PCT/CA2013/000492
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English (en)
Inventor
Richard Boudreault
Claudia GRAVEL-ROULEAU
Denis PRIMEAU
Marie-Maxime LABRECQUE-GILBERT
Original Assignee
Orbite Aluminae Inc.
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
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Application filed by Orbite Aluminae Inc. filed Critical Orbite Aluminae Inc.
Publication of WO2013170370A1 publication Critical patent/WO2013170370A1/fr

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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
    • 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
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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
    • 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
    • C22B58/00—Obtaining gallium or indium
    • 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
    • C22B59/00—Obtaining rare earth metals
    • 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 disclosure relates to improvements in the field of chemistry applied to the recovery, extraction and/or isolation of rare earth elements (REE).
  • REE rare earth elements
  • such processes are useful for obtaining rare earth elements from various materials and derivatives thereof such as aluminum-bearing materials and derivatives, zinc-bearing materials and derivatives thereof, copper-bearing materials and derivatives thereof, nickel- bearing materials and derivatives thereof, and titanium-bearing materials and derivatives thereof.
  • a process for recovering at least one rare earth element and/or at least one rare metal from at least one material comprising : leaching the at least one material with at least one acid, at least once, the at least one acid having a low concentration, thereby obtaining a leachate comprising the at least one rare earth element and/or at least one rare metal and at least one metal ion, and a solid comprising at least one metal, and separating the leachate from the solid; at least substantially selectively removing the at least one metal ion from the leachate and obtaining a precipitate; and substantially selectively removing the at least one rare earth element and/or the at least one rare metal from the leachate, thereby obtaining the at least one rare earth element and/or the at least one rare metal and a liquid depleted in the at least one rare earth element and/or the at least one rare metal.
  • a process for recovering at least one rare earth element and/or the at least one rare metal from at least one material comprising:
  • a process for extracting at least one rare earth element and/or at least one rare metal from at least one material comprising : leaching the at least one material with HCI, at least once, the HCI having a concentration below 10 % by weight, thereby obtaining a leachate comprising the at least one rare earth element and/or the at least one rare metal and at least one metal ion, and a solid comprising at least one metal, and separating the leachate from the solid; at least substantially selectively removing the at least one metal ion from the leachate by carrying out an hydrolysis of the at least one metal ion contained in the leachate, thereby obtaining a precipitate comprising the at least one metal ion and a liquid; and separating the liquid from the precipitate, thereby obtaining a composition comprising the at least one rare earth element and/or the at least one rare metal.
  • a process for extracting at least one rare earth element and/or at least one rare metal from at least one material comprising:
  • Leaching for example at room temperature and atmospheric pressure, the at least one material with HCI, at least once, the HCI having a concentration below 10 or 5 % by weight, thereby obtaining a leachate comprising the at least one rare earth element and/or the at least one rare metal and at least one metal ion, and a solid comprising at least one metal, and separating the leachate from the solid; at least substantially selectively removing the at least one metal ion from the leachate by carrying out an hydrolysis of the at least one metal ion contained in the leachate, thereby obtaining a precipitate comprising the at least one metal ion and a liquid; and separating the liquid from the precipitate, thereby obtaining a composition comprising the at least one rare earth element and/or the at least one rare metal.
  • Fig. 1 shows a bloc diagram of an example of process for extracting at least one rare earth element according to the present disclosure
  • At least one aluminum ion refers, for example, to at least one type of aluminum ion chosen from all possible forms of Al ions.
  • the at least one aluminum ion can be Al 3+ .
  • At least one iron ion refers, for example, to at least one type of iron ion chosen from all possible forms of Fe ions.
  • the at least one iron ion can be Fe 2+ , Fe 3+ , or a mixture thereof.
  • the expression "at least one zinc ion”, as used herein refers, for example, to at least one type of zinc ion chosen from all possible forms of Zn ions.
  • the at least one zinc ion can be Zn 2+ .
  • the expression "at least one copper ion”, as used herein refers, for example, to at least one type of copper ion chosen from all possible forms of Cu ions.
  • the at least one copper ion can be Cu 1+ or Cu 2+ , or a mixture thereof.
  • At least one nickel ion refers, for example, to at least one type of nickel ion chosen from all possible forms of Ni ions.
  • the at least one nickel ion can be Ni 2+ or Ni 3+ , or a mixture thereof.
  • At least one titanium ion refers, for example, to at least one type of titanium ion chosen from all possible forms of Ti ions.
  • the at least one titanium ion can be Ti 3+ or Ti 4+ , or a mixture thereof.
  • At least one rare earth element refers, for example, to at least one type of rare earth element chosen from all the rare earth elements described in the present disclosure in all their possible forms.
  • Ga-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of gallium.
  • Ce-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of cerium.
  • Sc-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of scandium.
  • Sm-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of samarium.
  • Eu-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of europium.
  • Gd-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of gadolinium.
  • Y-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of yttrium.
  • Pr-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of praseodymium.
  • Neodymium refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of neodymium.
  • La-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of lanthanum.
  • Er-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of erbium.
  • Dy-free solution refers, for example, to a solution that comprises about less than 5 %, 2 % or 1 % w/v of dysprosium.
  • rare earth element refers, for example, to a rare element chosen from scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium, and/or a rare metal chosen from indium, zirconium, lithium, and gallium.
  • These rare earth elements and rare metals can be in various form such as the elemental form (or metallic form), under the form of chlorides, oxides, hydroxides etc.
  • the at least one rare earth element refers, for example, to a at least one rare element chosen from scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium, and/or to at least one rare metal chosen from indium, zirconium, lithium, and gallium.
  • These rare earth elements and rare metals can be in various form such as the elemental form (or metallic form), or under the form of chlorides, oxides, hydroxides etc.
  • the at least one acid can have has a concentration of about 1 to about 10 weight %, about 8 to about 10 weight %, about 9 weight%, about 1 to about 8 weight %, about 1 to about 7 weight %, about 2 to about 8 weight %, about 2 to about 6 weight %, about 1 to about 5 weight %, about 1 to about 3 weight %, about 2 to about 3 weight %, about 2 to about 4 weight %, or about 2.0 to about 2.5 %. It can also be below 10, 9, 8, 7, 6, 5, 4, 3, or 2 weight %.
  • leaching can be carried out at a temperature of about 10 to about 60 °C, about 15 to about 40 °C, about 20 to about 35 °C, about 15 to about 25 °C, about 20 to about 30 °C, about 20 to about 25 °C, about 20 to about 40 °C, about 20 to about 30 °C, about 15 to about 35 °C, about 15 to about 30 °C, about 80 to about 140 °C, about 80 to about 90 °C, about 90 to about 130 °C, or about 100 to about 120 °C.
  • the leaching can be carried out at a pressure of about 5 to about 100 psig or about 15 to about 50 psig.
  • the leaching can be carried out at atmospheric pressure.
  • the leachate can comprise the at least one rare earth element under the form of a chloride and the at least one metal ion under the form of a chloride.
  • the leachate can comprise the at least one rare earth element under the form of a chloride and the at least one metal ion under the form of a chloride.
  • the at least one metal under the form of a chloride can be AI, Fe, Mg, Ni, Na, Ca, Li, K.
  • the at least one metal ion under the form of a chloride is Fe 2+ and/or Fe 3+ .
  • the at least one metal ion under the form of a chloride can be Al 3+ .
  • the at least one material contains iron and after the leaching, the leachate contains less than about 5, 4, 3, 2, or 1 weight % of the total amount of iron that was contained in the at least one material prior to leaching.
  • the at least one material contains iron and after the leaching, the at least one material comprises about 1 to about 3 weight % of the total amount of iron that was contained in the at least one material prior to leaching.
  • the at least one material contains aluminum and after the leaching, the leachate contains less than about 3, 2, 1.5, 1 , 0.8, 0.7 or 0.5 weight % of the total amount of aluminum that was contained in the at least one material prior to leaching.
  • the at least one metal ion under the form of a chloride can be an ion of a metal chosen from Al, Fe, Ca, Na, Ti, Mg, No, Pd, Pt, Zn, Cu, Au, Ag, Co, Li, Ni, Mn,Th, K, Si and mixtures thereof.
  • the leachate can be hydrolyzed so as to substantially selectively remove the at least one metal ion from the leachate and obtaining the precipitate.
  • the leachate can be hydrolyzed so as to substantially selectively remove the at least one metal ion from the leachate, obtain the precipitate and regenerate the at least one acid by obtaining a composition comprising the acid an enriched in the at least one rare earth element.
  • the precipitate can comprise hematite.
  • the hydrolysis can be carried out at a temperature of about 150 to about 170 °C, about 160 to about 168 °C, about 162 to about 165 °C.
  • the hydrolysis of the at least one metal ion contained in the leachate can be carried out as described in WO 2013/037054, which is hereby incorporated by reference in its entirety.
  • the at least one compound can be chosen from NaOH, NaOCI, KOH and KOCI.
  • the composition can be recirculated in the process and used upstream of the hydrolysis so as to be mixed with the leachate, thereby concentrating the at least one rare earth element.
  • the at least one metal comprised in the solid can comprise Al, Fe, Ca, Na, K and/or Si.
  • the at least one metal can comprised in the solid can comprise a member chosen from Al, Fe, Ca, Na, Ti, Mg, No, Pd, Pt, Zn, Cu, Au, Ag, Co, Li, Ni, Mn.Th, K, Si and mixtures thereof.
  • the at least one acid used for leaching the at least one material can be HCI, H 2 S0 4 , HN0 3 or mixtures thereof. More than one acid can be used as a mixture or separately. Solutions made with these acids can be used at various concentration.
  • the at least one rare earth element in the leachate, can be in the form of an ion.
  • the at least one rare earth element can be solubilized into the solution and can be found as a soluble ion, associated to chlorine, a sulfate, a nitrate, or hydrates thereof, etc.
  • various bases can be used for raising up the pH such as KOH, NaOH, Ca(OH) 2 , CaO, MgO, Mg(OH) 2 , CaC0 3 , Na 2 C0 3 , NaHC0 3 , C0 2 , or mixtures thereof.
  • the at least one material can be chosen from aluminum-bearing materials and derivatives, zinc-bearing materials and derivatives thereof, copper-bearing materials and derivatives thereof, nickel- bearing materials and derivatives thereof, and titanium-bearing materials and derivatives thereof.
  • the at least one metal ion can comprise at least one aluminum ion, at least one zinc ion, at least one copper ion, at least one nickel ion, at least one titanium ion and/or at least one iron ion.
  • the at least one metal ion can comprise a first metal ion and a second metal ion.
  • the first metal ion can comprise at least one aluminum ion, at least one zinc ion, at least one copper ion, at least one nickel ion, at least one titanium ion and/or at least one iron ion.
  • the second metal ion can comprise at least one aluminum ion, at least one zinc ion, at least one copper ion, at least one nickel ion, at least one titanium ion and/or at least one iron ion.
  • the first metal ion can be at least one aluminum ion.
  • the second metal ion can be at least one iron ion.
  • the at least one iron ion can be precipitated.
  • it can be precipitated by means of an ionic precipitation and it can precipitate in the form of various salts, hydroxides, chlorides or hydrates thereof.
  • the at least one iron ion can be precipitated as FeCI 2 , FeCI 3 , Fe(OH) 3 , Fe(OH) 2 , hematite, geotite, jarosite or hydrates thereof.
  • the at least one rare earth element can be solubilized into the solution and can be found as a soluble ion, associated as an hydroxide or a salt, or hydrates thereof.
  • the at least aluminum ion can be precipitated.
  • it can be precipitated by means of an ionic precipitation and it can precipitate in the form of various salts, (such as chlorides, sulfates) or hydroxides or hydrates thereof.
  • the at least one aluminum ion can be precipitated as AI(OH)3, AlC , AI 2 (S0 4 )3, or hydrates thereof.
  • the at least one rare earth element can be solubilized into the solution and can be found as a an ion associated to an hydroxide or a salt or hydrates thereof.
  • the residual and substantially purified or refined solution can contain the at least one rare earth element into a mixture of residual soluble ions, such as CI " , SO 4 2 -, Na + .
  • the at least one material can be an aluminum-bearing material
  • the aluminum-bearing material can be an aluminum-bearing ore.
  • clays, argillite, mudstone, beryl, cryolite, garnet, spinel, bauxite, or mixtures thereof can be used as starting material.
  • the aluminum-bearing material can also be a recycled industrial aluminum-bearing material such as slag.
  • the aluminum-bearing material can also be red mud or fly ashes.
  • the processes of the present disclosure can be effective for treating various nickel-bearing ores.
  • niccolite, kamacite, taenite, limonite, garnierite, laterite, pentlandite, or mixtures thereof can be used.
  • the processes of the present disclosure can be effective for treating various zinc-bearing ores.
  • smithsonite, warikahnite, sphalerite, or mixtures thereof can be used.
  • the processes of the present disclosure can be effective for treating various copper-bearing ores.
  • copper-bearing oxide ores can be used.
  • chalcopyrite, chalcocite, covellite, bornite, tetrahedrite, malachite, azurite, cuprite, chrysocolla, or mixtures thereof can also be used.
  • the processes of the present disclosure can be effective for treating various titanium-bearing ores.
  • ecandrewsite, geikielite, pyrophanite, ilmenite, or mixtures thereof can be used.
  • the at least one rare earth element can be chosen from scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium, and from at least one rare metal chosen from indium, zirconium, lithium, and gallium.
  • rare earth elements can sometimes be divided into two categories, light rare earth elements (LRE) and heavy rare earth elements (HRE).
  • the light rare earth elements can comprise lanthanum, cerium, praseodymium, neodymium, and samarium (atomic numbers 57-62), and they are usually more abundant than heavy ones.
  • the at least one rare element can be extracted under the form of various salts, oxides, hydroxides, and hydrates thereof.
  • the at least one rare earth element can be chosen from scandium, gallium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, dysprosium, erbium, ytterbium and mixtures thereof.
  • the at least one rare earth element is chosen from scandium, gallium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, dysprosium and mixtures thereof.
  • the at least one rare earth element is chosen from scandium, gallium, yttrium, cerium and mixtures thereof.
  • the at least one rare earth element can be yttrium.
  • the at least one rare earth element can be scandium.
  • the at least one rare earth element can be gallium.
  • the at least one rare earth element can be cerium.
  • the at least one rare earth element and/ot the at least one rare metal can be substantially selectively precipitated, extracted and/or isolated by means of a liquid-liquid extraction and/or at least one extracting agent and/or an ion exchange resin.
  • the at least one rare earth element can be extracted, purified and/or recovered by means of a technique as described in US 5, 104,544, that is hereby integrated by reference in its entirety. More particularly, US 5,104,544 describes a technique using an ion exchanger that can be subjected to reverse osmosis.
  • the resin can be as described in this document or it can be made of other material such as poly(trimethylene terephthalate) (PTT).
  • the at least one extracting agent can be chosen from di-(2-ethylhexyl) phosphoric acid (HDEHP), mono(2-ethylhexyl)2-ethylhexyl phosphonate (HEH/EHP), bis(2,4,4-trimethylpentyl) monothiophosphinic acid), octyl phenyl phosphate (OPAP), 2-ethylhexylphosphonic acid mono-2- ethylhexyl ester (PC88A) and optionally toluene, tributyl phosphate, di- isoamylmethyl phosphonate, 7-(4-ethyl-1-methyloctyl)-8-hydroxyquinoline, di- (2-ethylhexyl) phosphinic acid, bis(2,4,4-trimethylpentyl) phosphinic acid, 8- hydroxyquinoline, and (2-ethylhexyl
  • the at least one extracting agent can be di-(2- ethylhexyl) phosphoric acid.
  • the at least one extracting agent can be 2- ethylhexylphosphonic acid mono-2-ethylhexyl ester.
  • the at least one extracting agent can be octyl phenyl phosphate.
  • the at least one extracting agent can be tributyl phosphate.
  • the at least one extracting agent can be chosen from diethylenetriamine-penthaacetic acid (DTPA), ethylenediaminetetraacetic (EDTA), 1 ,4,7, 10-tetraazacyclododecane-1 ,4,7,10-tetraacetic acid (DOTA), bis(2,4,4-trimethylpentyl) monothiophosphinic acid and mixtures thereof.
  • DTPA diethylenetriamine-penthaacetic acid
  • EDTA ethylenediaminetetraacetic
  • DOTA 10-tetraazacyclododecane-1 ,4,7,10-tetraacetic acid
  • bis(2,4,4-trimethylpentyl) monothiophosphinic acid and mixtures thereof.
  • the at least one rare earth element and/or the at least one rare metal found as an ion in the leachate can be precipitated.
  • scandium can be precipitated in the form of Sc(OH)3, ScCI 3 , ScF 3 , and/or [ScF 6 ] 3" (cation), wherein the cation can be sodium, potassium, magnesium, calcium etc
  • Scandium can be precipitated at a pH of about 7 to about 9, or about 7 to about 8.
  • the liquor or leachate can comprise the at least one rare earth element under the form of a chloride, and wherein the leachate can be reacted with an extracting agent in order to substantially selectively extract gallium therefrom, thereby obtaining a Ga-free solution and an extracted gallium solution, and separating the solutions from one another.
  • gallium in the leachate can be under the form of GaCI 3 .
  • the extracting agent can be octyl phenyl phosphate, 2- ethylhexylphosphonic acid mono-2-ethylhexyl ester and toluene, tri-butyl phosphate or mixtures thereof.
  • the extracted GaCI 3 can then be precipitated and then converted into Ga 2 0 3 .
  • the Ga-free solution can then be reacted with another an extracting agent in order to substantially selectively extract cerium therefrom, thereby obtaining a Ce-free solution and an extracted cerium solution, and separating the solutions from one another.
  • the cerium in the Ga-free solution can be under the form of CeCI 3 .
  • the another extracting agent can be tri-butyl phosphate, di-isoamylmethyl phosphonate, di-(2-ethylhexyl) phosphoric acid, 7-(4-ethyl-1 -methyloctyl)-8- hydroxyquinoline or mixtures thereof.
  • the process can further comprise converting the extracted cerium into Ce0 2 .
  • the process can further comprise reacting the Ce-free solution with a further extracting agent in order to substantially selectively extract scandium therefrom, thereby obtaining a Sc-free solution and an extracted scandium solution, and separating the solutions from one another.
  • scandium in the Ce-free solution can be under the form of ScCI 3 .
  • the further extracting agent can be di-(2-ethylhexyl) phosphoric acid, di-(2-ethylhexyl) phosphinic acid or a mixture thereof.
  • the process can further comprise converting the extracted scandium into Sc 2 0 3 .
  • the extracted scandium can be converted into Sc 2 0 3 by means of NaOH.
  • the process can further comprise reacting the Sc-free solution with still a further extracting agent in order to substantially selectively extract samarium, europium or a mixture thereof, thereby obtaining a Sm-free solution and/or Eu-free solution and extracted samarium and/or europium solution, and separating the solutions from one another.
  • the still a further extracting agent can be chosen from bis(2,4,4-trimethylpentyl) phosphinic acid, di-(2-ethylhexyl) phosphoric acid and a mixture thereof.
  • the process can further comprise reacting the Sm-free solution and/or Eu-free solution with still another extracting agent in order to substantially selectively extract gadolinium, thereby obtaining a Gd-free solution and an extracted gadolinium solution, and separating the solutions from one another.
  • the still another extracting agent can be 8- hydroxyquinoline.
  • the process can further comprise reacting the Gd-free solution with yet another extracting agent in order to substantially selectively extract yttrium, thereby obtaining a Y-free solution and an extracted yttrium solution, and separating the solutions from one another.
  • the yet another extracting agent can be (2-ethylhexyl) phosphonic acid, di-(2- ethylhexyl) phosphonic acid or a mixture thereof.
  • the process can further comprise reacting the Y-free solution with still yet another extracting agent in order to substantially selectively extract dysprosium and/or erbium, thereby obtaining a Dy-free solution and/or an Er-free solution and an extracted dysprosium and/or erbium solution, and separating the solutions from one another.
  • the liquor can be reacted with a first extracting agent in order to substantially selectively extract gallium therefrom, thereby obtaining a Ga-free solution and an extracted gallium solution, and separating the solutions from one another.
  • gallium in the liquor can be under the form of GaCI 3 .
  • the first extracting agent can be tri-butyl phosphate optionally in kerosene.
  • the Ga-free solution can be reacted with a precipitating agent for precipitating at least one rare earth element present in the Ga-free solution, thereby obtaining a precipitate containing the at least one rare earth element and recovering the precipitate via a solid-liquid separation.
  • the process can further comprise leaching the precipitate with at least one acid so as to obtain a leach solution comprising the at least one rare earth element.
  • the acid can be HCI.
  • the leach solution can be reacted with a second extracting agent so as to substantially selectively extract a first group of rare earth elements, thereby obtaining a solution comprising the extracted rare earth elements of the first group and a raffinate comprising a second group of rare earth elements, and separating the solution from the raffinate.
  • the first group can comprise yttrium and scandium.
  • the second group can comprise cerium, neodynium, europium and praseodymium.
  • the second extracting agent can be chosen from di-(2-ethylhexyl)phosphoric acid and 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester.
  • the process can further comprise reacting the solution comprising the extracted rare earth elements of the first group with HCI at least once so as to remove impurities therefrom.
  • the process can further comprise stripping the solution comprising the extracted rare earth elements of the first group with at least one acid so as to obtain a first group strip liquor.
  • the at least one acid can be HCI.
  • the process can further comprise repeating at least once the extraction with the second extracting agent.
  • the first group strip liquor can be reacted with a third extracting agent so as to substantially selectively extracting at least one of scandium, erbium and dysprosium from the first group strip liquor, thereby obtaining a solution comprising the extracted at least one of scandium, erbium and dysprosium, and an yttrium raffinate, and separating the solution from the raffinate.
  • the third extracting agent can be tri-butyl phosphate.
  • the process can further comprise stripping the solution comprising the extracted at least one of scandium, erbium and dysprosium solution with at least one acid so as to obtain another first group strip liquor.
  • the at least one acid can be HCI.
  • the another first group strip liquor can be reacted with a fourth extracting agent so as to substantially selectively extracting erbium and dysprosium from the another first group strip liquor, thereby obtaining a solution comprising the extracted erbium and dysprosium, and a scandium raffinate, and separating the solution from the raffinate.
  • the at least one rare earth element can be substantially selectively precipitated, extracted and/or isolated by means of an adsorption on activated charcoal optionally modified with tributyl phosphate or on a polyurethane polyether foam (PUF).
  • activated charcoal optionally modified with tributyl phosphate or on a polyurethane polyether foam (PUF).
  • PEF polyurethane polyether foam
  • the at least one rare earth element can be substantially selectively removed by means of a liquid-liquid extraction.
  • the liquid-liquid extraction can be carried out by using an extracting agent.
  • scandium can be precipitated from a by-product generated during the process.
  • scandium can be precipitated from a solution generated during the process.
  • scandium can be precipitated using HNO 3 .
  • the at least one rare earth element can be substantially selectively precipitated, extracted and/or isolated by at least one technique chosen from ion exchange resin, extraction by means of solvent(s) and adsorption.
  • the at least one rare earth element can be substantially selectively precipitated, extracted and/or isolated by means of an ion exchange resin.
  • the at least one rare earth element can be substantially selectively precipitated, extracted and/or isolated by means of a liquid-liquid extraction.
  • the at least one rare earth element can be substantially selectively precipitated, extracted and/or isolated by means of an electrowinning process.
  • the at least one iron ion can be precipitated under the form of Fe 2 0 3 by means, for example, of an hydrolysis.
  • the substantially selectively removing of the at least one rare earth element and/or the at least one rare metal and the removing of the at least one metal from the leachate can be made in various manners.
  • the at least one metal ion can be removed and then, the at least one rare earth element and/or the at least one rare metal can be removed.
  • the at least one rare earth element and/or the at least one rare metal can be removed and then, the at least one metal ion can be removed.
  • a first metal ion can be removed, then a second metal ion can be removed and finally, the at least one rare earth element and/or the at least one rare metal can be removed.
  • the at least one rare earth element and/or the at least one rare metal can be removed, then, a first metal ion can be removed, and (optionally) finally a second metal ion can be removed.
  • the at least one rare earth element and/or the at least one rare metal can be removed, then, a second metal ion can be removed, and finally the first metal ion can be removed.
  • Various other possible combinations can also be envisaged.
  • the at least one metal ion can be removed by using an ion exchange resin or ion exchange system.
  • an ion exchange resin or system can be effective for allowing only chlorides of rare earth elements and chlorides rare metals to pass therethrough, while capturing the at least one metal ion.
  • the at least one iron ion can be precipitated.
  • it can be precipitated by means of an ionic precipitation and it can precipitate in the form of various salts, hydroxides, chlorides or hydrates thereof.
  • the at least one iron ion can be precipitated as FeCI 2 , FeCI 3 , Fe(OH) 3 , Fe(OH) 2 , hematite, geotite, jarosite or hydrates thereof.
  • various methods, processes and strategies can be used for extracting the at least one rare earth element and/or the at least one rare metal from the leachate.
  • the methods and processes described in WO/2012/126092, WO/2012/149642 and PCT/CA2013/000226 can be used in combination with the methods and processes of the present disclosure. These document are hereby incorporated by reference in their entirety.
  • the processes of the present disclosure can comprise at least substantially selectively removing the at least one metal ion from the leachate comprises treating the leachate with an extracting agent, an ion exchange resin and/or a reducing agent, thereby obtaining a composition having a reduced content in the at least one metal ion; and reacting the composition having the reduced content in the at least one metal ion with a precipitating agent so as to substantially selectively precipitate a first rare earth element and/or a first rare metal.
  • the leachate comprises (i) the first rare earth element and optionally the first rare metal and (ii) FeC .
  • the extracting agent can be chosen from tri-butyl phosphate, di-2-ethylhexyl phosphoric acid (HDEHP), bis(2,4,4- trimethylpentyl) phosphinic acid and 2-ethylhexyl phosphonic acid mono-2- ethylhexyl ester).
  • HDEHP di-2-ethylhexyl phosphoric acid
  • bis(2,4,4- trimethylpentyl) phosphinic acid 2-ethylhexyl phosphonic acid mono-2- ethylhexyl ester
  • the extracting agent can be tri-butyl phosphate.
  • the extracting agent can be tri-butyl phosphate in kerosene.
  • the acidic composition can be reacted with Fe(0), thereby obtaining a composition having a reduced content in Fe 3+ .
  • the first rare earth element can be scandium.
  • the acidic composition can comprise at least one rare metal.
  • the processes can comprise reacting the composition having the reduced content in the at least one iron ion with the precipitating agent so as to substantially selectively precipitate the first rare earth element and the first rare metal.
  • the first rare metal can be gallium.
  • the precipitating agent can be chosen from oxalic acid, NaOH, MgO, CaC0 3 and mixtures thereof.
  • the precipitating agent can be CaC0 3 .
  • the first rare earth element and optionally the first rare metal is/are substantially selectively precipitated by maintaining a pH value below 2, or a pH at a value of about 1 to about 2.
  • the first rare earth element and optionally the first rare metal is/are substantially selectively precipitated by maintaining Redox potential of about +380 mV.
  • the processes can comprise reacting the composition having reduced content in the at least one iron ion with the precipitating agent so as to substantially selectively precipitate a first rare earth element and first rare metal that are comprised in a so-formed precipitate, and recovering the precipitate.
  • the processes can further compriseg leaching the precipitate and obtaining a leaching solution.
  • the precipitate can be leached with HCI.
  • HCI can have a concentration of about 5 to about 15 mol/L.
  • the leaching solution can be further extracted with an extracting agent so as to substantially selectively extract the first rare earth element and the first rare metal and obtain a loaded organic phase.
  • the extracting agent can be tri-butyl phosphate, tri- butyl phosphate in kerosene or tri-butyl phosphate in kerosene and in the presence of isodecanol.
  • the processes can further comprising scrubbing the loaded organic phase with a scrubbing solution so as to recover the first rare earth element and obtained a scrubbed organic phase.
  • the scrubbing solution can be an acidic aqueous solution comprising HCI at a concentration of about 2 to about 12 mol/L.
  • the scrubbing solution can be used in a ratio scrubbing solution : loaded organic phase of about 1 : 1.
  • the processes can further comprise stripping the scrubbed organic phase with a stripping solution so as to recover the first rare metal.
  • the stripping solution can be water.
  • the stripping solution can be used in a ratio stripping solution : loaded organic phase of about 1 : 2.
  • the composition having a reduced content in the at least one iron ion can be reacted with the precipitating agent so as to obtain a liquid comprising at least one further rare earth element and the precipitate comprising the first rare earth element and the first rare metal, the process further comprising separating the liquid from the precipitate.
  • the process can further comprise reacting the liquid with another precipitating agent so as to obtain another precipitate, and recovering the another precipitate.
  • the liquid can be reacted with the another precipitating agent at a pH of about 7.8 to about 8.2 or about 7.9 to about 8.1.
  • the liquid can be reacted with the another precipitating agent by maintaining Redox potential at about +340 mV or at about +380 mV.
  • the liquid can be reacted with the another precipitating agent by maintaining a temperature of about 50 to about 70 °C.
  • the another precipitating agent can be chosen from oxalic acid, NaOH, MgO, CaC0 3 and mixtures thereof.
  • the another precipitating agent can be CaC0 3 .
  • the processes can further comprise leaching the another precipitate and obtaining a leaching solution comprising a second rare earth element.
  • the another precipitate can be leached with HCI.
  • the leaching solution comprising the second rare earth element can be extracted with an extracting agent so as to substantially selectively extract the second rare earth element and obtain a loaded organic phase comprising the second rare earth element and an aqueous phase comprising at least one light rare earth element.
  • the extracting agent di(ethylhexyl)phosphonic acid or di(ethylhexyl)phosphonic acid in kerosene.
  • the processes can further comprise at least partially removing a third rare earth element from the loaded organic phase comprising the second rare earth element.
  • the processes can further comprise at least partially removing a third rare earth element from the loaded organic phase comprising the second rare earth element by treating the loaded organic phase with an acidic scrubbing solution.
  • the scrubbing solution can comprise 1 N HCI.
  • the third rare earth element can cerium.
  • the processes can further comprise treating the loaded organic phase comprising the second rare earth element with an acidic stripping solution so as to obtain a strip liquor comprising the second rare earth element and recovering the strip liquor.
  • the strip liquor can comprise 3.5 N HCI.
  • the processes can comprise treating the strip liquor comprising the second rare earth element with an extracting agent so as to substantially selectively extract a fourth rare earth element and optionally a fifth rare earth element from the strip liquor and obtaining a raffinate comprising the second rare earth element.
  • the extracting agent can be tri-butyl phosphate or tri-butyl phosphate in kerosene.
  • the fourth rare earth element can be dysprosium.
  • the fifth rare earth element is erbium.
  • the processes can further comprise reacting an organic phase comprising the fourth rare earth element and optionally the fifth rare earth element with a strip solution so as to obtain a strip liquor comprising the fifth rare earth element and optionally the fifth rare earth element.
  • a strip solution can be water.
  • the second rare earth element is yttrium.
  • the leaching solution comprising the second rare earth element can be extracted with an extracting agent so as to substantially selectively extract the second rare earth element and obtain a loaded organic phase comprising the second rare earth element and a raffinate comprising at least one light rare earth element.
  • the extracting agent can be di(ethylhexyl)phosphonic acid or di-(2-ethylhexyl) phosphoric acid.
  • the processes can further comprise at least partially removing a third rare earth element from the loaded organic phase comprising the second rare earth element.
  • the processes can further comprise at least partially removing a third rare earth element from the loaded organic phase comprising the second rare earth element by treating the loaded organic phase with an acidic scrubbing solution.
  • the scrubbing solution comprises about 1 N to about 2 N HCI.
  • the processes can further comprise treating the loaded organic phase comprising the second rare earth element with a stripping solution so as to obtain a strip liquor comprising the second rare earth element.
  • the stripping solution can comprise about 3 M to about 4M HCI.
  • the strip liquor comprising the second rare earth element can be extracted with an extracting agent so as to remove a fourth rare earth element and optionally a fifth rare earth element, thereby obtaining a raffinate comprising the second rare earth element and a loaded organic phase comprising the fourth rare earth element and optionally the fifth rare earth element.
  • the extracting agent is tri-butyl phosphate or tri- butyl phosphate in kerosene.
  • the processes can comprise recovering the raffinate comprising the second rare earth element.
  • the second rare earth element can be yttrium.
  • the fourth rare earth element can be dysprosium.
  • the fifth rare earth element can be erbium.
  • the processes can further comprise reacting the loaded organic phase comprising the fourth rare earth element and the fifth rare earth element with a stripping solution so as to obtain strip liquor comprising the fourth rare earth element and the fifth rare earth element.
  • a stripping solution can be water.
  • the processes can further comprise reacting the strip liquor with an extracting agent so as to substantially selectively extract the fifth rare earth element from the strop liquor, thereby obtaining a raffinate comprising the fourth rare earth element and a loaded organic phase comprising the fifth rare earth element.
  • the extracting agent can be di(ethylhexyl)phosphonic acid or di-(2-ethylhexyl) phosphoric acid.
  • the proceses can further comprise separating the raffinate from the loaded organic phase comprising the fifth rare earth element, treating the loaded organic phase with a scrubbing solution so as to remove impurities therefrom and then treating the loaded organic phase with a stripping solution so as to obtain a strip liquor comprising the fifth rare earth element.
  • the scrubbing solution can comprise about 2 M to about 4 M HCI.
  • the raffinate can be reacted with an oxidation agent so as to oxidize the third rare earth element.
  • the oxidation agent can comprise sodium hypochlorite.
  • the raffinate can be reacted with an oxidation agent at a pH of about 0.5 to about 1.5.
  • the processes can further comprise removing, from the raffinate, the oxidized third rare earth element that is under the form of a precipitate, thereby obtaining a filtrate comprising a sixth rare earth element.
  • the processes can further comprise reacting the filtrate with an extracting agent so as to substantially selectively extracting the sixth rare earth element from the filtrate, thereby obtaining a loaded organic phase comprising the sixth rare earth element and another raffinate comprising a seventh rare earth element and an eight rare earth element, and separating the loaded organic phase comprising the sixth rare earth element from the raffinate.
  • the extracting agent can be di(ethylhexyl)phosphonic acid or di-(2-ethylhexyl) phosphoric acid.
  • the processes can further comprise treating the loaded organic phase with a scrubbing solution so as to remove impurities therefrom and then treating the loaded organic phase with a stripping solution so as to obtain a strip liquor comprising the sixth rare earth element.
  • a scrubbing solution can comprise about 0.5 M to about 1.5 M HCI.
  • the stripping solution can comprise about 2 M to about 3 M HCI.
  • the sixth rare earth element can europium.
  • the seventh rare earth element can be praseodymium.
  • the eigth rare earth element can be neodymium.
  • the processes can further comprise reducing the sixth rare earth element by means of a reducing agent.
  • the reducing agent can be zinc (0).
  • the processes can further comprise reacting the sixth rare earth element with sodium sulphate so as to obtain a sulphate derivative thereof under the form of a precipitate and recovering the precipitate.
  • the processes can further comprise reacting the raffinate comprising the seventh rare earth element and the eight rare earth element with an extracting agent so as to substantially selectively extracting the eight rare earth element from the raffinate, thereby obtaining a loaded organic phase comprising the eight rare earth element a raffinate comprising the seventh rare earth element, and separating the loaded organic phase comprising the eight rare earth element from the raffinate.
  • the extracting agent can be di(ethylhexyl)phosphonic acid or di-(2-ethylhexyl) phosphoric acid.
  • the processes can further comprise treating the loaded organic phase with a scrubbing solution so as to remove impurities therefrom and then treating the loaded organic phase with a stripping solution so as to obtain a strip liquor comprising the eight rare earth element.
  • a scrubbing solution can comprise about 2 M to about 3 M HCI.
  • the stripping solution can comprise about 3 M to about 4 M HCI.
  • the processes can further comprise, pre-treating or treating the acidic composition with an ion exchange resin so as to remove impurities.
  • the processes can further comprise, before extracting at least one rare earth element and optionally at least one rare metal from the acidic composition, treating the acidic composition with an ion exchange resin so as to at least partially remove impurities therefrom.
  • the processes can further comprise treating the at least one rare earth element and optionally the at least one rare metal extracted by the process by means of a plasma torch so as to further purify the at least one rare earth element and optionally the at least one rare metal.
  • the process can comprise the preparation of the starting material (for example clay in the example shown in Fig.1 ).
  • CPP stands for Clay Preparation Plant.
  • Such a treatment can be a physical treatment such as those described in WO2008141423, WO/2012/126092 or WO/2012/149642, hereby incorporated by reference in their entirety at least one leaching step for leaching the material that comprises at least one rare earth element.
  • the material can comprise at least one other element chosen from Al, Fe, Ca, Na, Ti, Mg, No, Pd, Pt, Zn, Cu, Au, Ag, Co, Li, Ni, Mn,Th, K, Si and mixtures thereof.
  • the leaching in ALP can be carried out, for example, by using an acid having a low concentration (for example about 1 to about 10 weight %, about 1 to about 5 weight %, or about 2 to about 4 weight %).
  • the acid can be HCI, H 2 S0 4 or HNO3.
  • the leaching can be carried out at a temperature of about 80 to about 140 °C, about 90 to about 130 °C or about 100 to about 120 °C.
  • the leaching can be carried out at a pressure of about 5 to about 100 psig or about 15 to about 50 psig.
  • Such a low acid concentration can be carried out in order to substantially selectively leach the at least one rare earth element, and/or the at least one rare metal and optionally at least one other component such as at least one other alkali metal.
  • the at least one other component leached can be, for example, a metal oxide such as an alkali metal oxide.
  • the at least one other component leached can comprise Na 2 0, K 2 0, CaO, and mixtures thereof.
  • the at least one other component leached can comprise Fe, Al and various other metals, for example, in the form of a chloride. More than one leaching step can be done (for example see ALP Leaching # 1 and ALP Leaching # 2).
  • Leaching step can be performed semi- continuous or continuous Both steps can be made using the same acid or a different acid.
  • the acid concentration in a first and optional subsequent leaching can be the same or different.
  • the at least one rare earth element and/or the at least one rare metal is at least substantially leached and solubilized (in a liquid portion) while the at least one other element is still substantially in a solid form (solid portion).
  • the liquid is then separated from the solid.
  • the starting material is a clay (for example argillite)
  • the solid form can comprise Si, Al, Fe, and optionally Ti but it can be substantially free of the at least one rare earth element. It can also be substantially free of alkali metals and/or alkaline earth metals.
  • Such a solid can be used, for example, in cement industry (cement manufacturing) since substantially free of alkali (for example Na and K).
  • the leachate (or liquid portion) can comprise, in addition of the at least one rare earth element (for example in the form of a chloride (if the acid is HCI)) and/or the at least one rare metal, various metal chlorides for example in low quantity.
  • the metal chlorides MeCI and the at least one rare earth element and/or the at least one rare metal in the form of a chloride can then be pre-concentrated and hydrolyzed at low temperature for example about 150 to about 170 °C, about 160 to about 168 °C or about 162 °C to about 165 °C.
  • Fe is found as a chloride
  • Fe 2 C>3 hematite form
  • acid recovery for example
  • argillite when argillite is used as a starting material, components such as REO (Rare Earth Oxides), RMO (Rare Metal Oxides), Na 2 0, K 2 0 and CaO will be leached as well as trace of metals such as Fe and Al.
  • REO Rotary Earth Oxides
  • RMO Rotary Metal Oxides
  • Na 2 0, K 2 0 and CaO will be leached as well as trace of metals such as Fe and Al.
  • the recycled acid can be used before pre-concentration and/or for leaching.
  • the obtained hematite can optionally be treated with a base (for example NaOH) so as to at least partially neutralize it.
  • a base for example NaOH
  • a liquid portion obtained from the pre-concentrator can comprise the at least one rare earth element (for example in the form of a chloride) as well as other non-hydrolyzable metal chlorides (MeCI).
  • a liquid portion can be treated as described in WO/2012/126092 or WO/2012/1 9642 in order to extract the at least one rare earth element therefrom.
  • the at least one rare earth element can be extracted by means of an ion exchange resin.

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Abstract

L'invention concerne des procédés de récupération d'au moins un élément de terre rare et/ou d'au moins un métal rare provenant d'au moins un matériau. Le procédé peut comprendre : la lixiviation dudit au moins un matériau par au moins un acide à faible concentration, ce qui permet d'obtenir un lixiviat comprenant ledit au moins un élément de terre rare et/ou ledit au moins un métal rare et au moins un ion métallique, et un solide comprenant au moins un métal, et la séparation du lixiviat du solide ; au moins l'élimination notable, sélective dudit au moins un ion métallique du lixiviat ; et l'élimination notable, sélective dudit au moins un élément de terre rare et/ou dudit au moins un métal rare du lixiviat, ce qui permet d'obtenir ledit au moins un élément de terre rare et/ou ledit au moins un métal rare.
PCT/CA2013/000492 2012-05-16 2013-05-16 Procédés de récupération d'éléments de terre rare provenant de divers matériaux WO2013170370A1 (fr)

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RU2581327C1 (ru) * 2015-01-19 2016-04-20 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" Способ извлечения скандия из красного шлама производства глинозема
CN105779762A (zh) * 2016-05-17 2016-07-20 南昌航空大学 一种萃取分离制备5n铒的工艺
CN107099666A (zh) * 2017-05-16 2017-08-29 广东富远稀土新材料股份有限公司 一种萃取分离铥、镱、镥的方法

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AU2008286599A1 (en) * 2007-08-10 2009-02-19 Grirem Advanced Materials Co., Ltd. A metallurgical process for iron-rich monazite rare earth ore or concentrate
US8216532B1 (en) * 2011-06-17 2012-07-10 Vierheilig Albert A Methods of recovering rare earth elements

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US2024026A (en) * 1933-11-17 1935-12-10 Warner Chemical Company Recovering lithium compounds
JPH05287405A (ja) * 1991-05-17 1993-11-02 Sumitomo Metal Mining Co Ltd 希土類元素の回収方法
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RU2581327C1 (ru) * 2015-01-19 2016-04-20 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" Способ извлечения скандия из красного шлама производства глинозема
CN105779762A (zh) * 2016-05-17 2016-07-20 南昌航空大学 一种萃取分离制备5n铒的工艺
CN107099666A (zh) * 2017-05-16 2017-08-29 广东富远稀土新材料股份有限公司 一种萃取分离铥、镱、镥的方法

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