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WO2018195642A1 - Précipitation directe d'oxalate pour la récupération d'éléments de terres rares - Google Patents

Précipitation directe d'oxalate pour la récupération d'éléments de terres rares Download PDF

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Publication number
WO2018195642A1
WO2018195642A1 PCT/CA2017/050508 CA2017050508W WO2018195642A1 WO 2018195642 A1 WO2018195642 A1 WO 2018195642A1 CA 2017050508 W CA2017050508 W CA 2017050508W WO 2018195642 A1 WO2018195642 A1 WO 2018195642A1
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WO
WIPO (PCT)
Prior art keywords
solution
rare earth
recovery
salt
oxalate
Prior art date
Application number
PCT/CA2017/050508
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English (en)
Inventor
Chen Xia
Wesley GRIFFITH
Original Assignee
Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources Canada
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources Canada filed Critical Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources Canada
Priority to PCT/CA2017/050508 priority Critical patent/WO2018195642A1/fr
Publication of WO2018195642A1 publication Critical patent/WO2018195642A1/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
    • C22B59/00—Obtaining rare earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
    • B01D9/0054—Use of anti-solvent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • 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
    • C22B3/08—Sulfuric acid, other sulfurated 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D2009/0086—Processes or apparatus therefor
    • B01D2009/009—Separation of organic compounds by selective or extractive crystallisation with the aid of auxiliary substances forming complex or molecular compounds, e.g. with ureum, thioureum or metal salts
    • B01D2009/0095—Separation of organic compounds by selective or extractive crystallisation with the aid of auxiliary substances forming complex or molecular compounds, e.g. with ureum, thioureum or metal salts with the aid of other complex forming substances than ureum, thioureum or metal salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0077—Screening for crystallisation conditions or for crystal forms
    • 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 specification relates to the field of extractive metallurgy, in particular to the field of mineral or ore processing. More particularly, the present specification relates to the recovery of rare earth elements in ore processing.
  • REEs Rare earth elements
  • These elements are typically highly dispersed in ore deposits, and therefore are not found as rare earth minerals for extraction.
  • REEs are rather present as side products in the processing of ores.
  • Various methods for ore processing are known and often involve a series of dissolution, leaching, extraction, separation steps and the like. It has proven beneficial to recover valuable REEs during ore processing, both for improving the efficiency of the ore processing itself, as well as for the recovery of REEs for further uses.
  • REEs Based on the high selectivity of oxalate to REEs, a common method for the recovery of REEs is oxalic acid precipitation.
  • the REEs are most likely found dissolved in solutions from ore refining processes.
  • REEs are precipitated as REE salts and can be recovered.
  • Chinese patent applications 1043768 and 1044499 provide other examples of methods for the recovery of RREs comprising oxalic acid precipitation on acid leaching solution from the leaching of clay.
  • Another example of oxalic acid precipitation for the recovery of REEs can be found in US patent publication 2015/0354026.
  • Certain exemplary embodiments provide A method for recovering at least one rare earth element from an aqueous acid solution, the method comprising the steps of: a) treating the aqueous acid solution with oxalic acid or at least one oxalate salt, in the presence of at least one additive salt to precipitate the at least one rare earth element as at least one rare earth salt; and b) recovering the at least one rare earth salt from the treated aqueous acid solution as a solid product.
  • Figure 1 represents a conceptual flow chart of a direct oxalate precipitation
  • Figure 2 is a graph of REE recovery at various oxalic dosage conditions.
  • Figure 3 is a graph of REE recovery at various pH.
  • Figure 4 is a graph of REE recovery at various temperatures
  • Figure 5 is a graph of REE recovery for different alkalis for adjusting pH.
  • Figure 6 is a graph of REE recovery when NaCI is used as an additive salt.
  • Figure 7 is a graph of REE recovery for the study of the effect of NaCI.
  • Figure 8 is a graph of REE recovery with reduced oxalic addition.
  • Figure 9 is a graph of REE recovery for different additive salts.
  • Rare earth element or “REE” as used herein defines one of a set of seventeen chemical elements in the periodic table, specifically the fifteen lanthanides, and scandium and yttrium which are considered rare earth elements because they tend to occur in the same ore deposits as the lanthanides and exhibit similar chemical properties. Therefore, rare earth elements are cerium (Ce), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), holmium (Ho), lanthanum (La), lutetium (Lu), neodymium (Nd), praseodymium (Pr), promethium (Pm),
  • samarium Sm
  • scandium Sc
  • terbium Tb
  • thulium Tm
  • ytterbium Yb
  • yttrium Y
  • Oxalate refers to the dianion derived from oxalic acid, having the formula C 2 0 4 2 ⁇ , also written as (COO) 2 2 ⁇ .
  • Oil processing refers to a term used in the field of extractive metallurgy. Also known as mineral processing, ore dressing, or ore refining, it is the process of separating commercially valuable minerals from their ores. Those terms may be used interchangeably herein.
  • Leaching refers to an extractive metallurgy process where ore is soluble and impurities are insoluble, and therefore which converts metals into soluble salts in aqueous media.
  • Dissolution is generally the process by which a solid, gas, or liquid is dispersed homogeneously in a gas, solid, or, especially, a liquid. In metallurgy, it most often refers to the dispersion of valuable metals found in ores into an aqueous solution and /or a suitable solvent.
  • Pre-purification as used herein typically refers to a purification step to potentially remove some undesired impurities, carried out before undergoing a further treatment of an ore processing process.
  • Hydrolysis is usually the cleavage of chemical bonds by the addition of water. In many cases of metal ions such as iron and aluminum, hydrolysis tends to proceed as pH rises leading to the precipitation of a hydroxide.
  • low grade refers to a materiel or solution of inferior quality, potentially containing lesser amounts of valuable materials and/or higher amounts of impurities.
  • Pregnant solution as used herein defines a metal-bearing aqueous solution obtained after treatment such as leaching in an ore refining process, and before concentration and recovery of the metal.
  • the expression "stoichiometric amount" of a reagent of a reaction is the optimum amount or ratio where, assuming that the reaction proceeds to completion: all of the reagent is consumed; there is no deficiency of the reagent; there is no excess of the reagent.
  • the stoichiometry is used to find the right amount of one reactant to "completely" react with the other reactant in a chemical reaction - that is, the stoichiometric amounts that would result in no leftover reactants when the reaction takes place.
  • the present specification provides a direct oxalate precipitation for REEs recovery from a low-grade REE pregnant solution, without the need for pre-purification.
  • the REEs may typically be found in aqueous pregnant acid solutions derived from various steps of an ore refining process, such as dissolution, leaching, or the like.
  • the pregnant acid solution therefore comprises at least one dissolved REE.
  • the solution comprises multiple dissolved REEs.
  • the aqueous pregnant solution may be obtained, for example, from a dissolution or leaching process with an acid solution, such as sulfuric acid, hydrochloric acid, or the like, or mixtures thereof.
  • the direct oxalate precipitation of the present specification may be conducted directly on aqueous pregnant acid solution without pre-purification such as iron hydrolysis, iron precipitation, double sulfate precipitation, solvent extraction or the like, and combinations thereof. Proceeding with direct oxalate precipitation would generally increase the oxalic acid consumption and provide low yield and low purity REEs. However, the present specification provides for the direct oxalate
  • precipitation comprising treatment of the aqueous pregnant acid solution with oxalic acid or an oxalate salt, or mixtures thereof, in the presence of at least one additive salt, to cause precipitation of at least one REE as at least one REE salt.
  • the reaction conditions which will be described below may be adjusted to selectively precipitate only one specific REE. In other embodiments some selected RREs may precipitate and others may remain in the solution. In yet other embodiments, all of the REEs dissolved in the solution are reacted to precipitate.
  • the amount of oxalic acid added to the pregnant solution may be around 5 times the stoichiometric amount.
  • the amount of oxalic acid is around 4 times and more preferably the amount of oxalic acid is less then 2 times the stoichiometric amount.
  • the additive salt may be a chloride, a sulfate or a combination thereof.
  • the additive salt is selected from NaCI, Na 2 S0 4 , KCI, K 2 S0 4 , NH 4 CI, (N H 4 ) 2 S0 4j and combination thereof.
  • the additive salt may be added as a solid or as an aqueous solution in an amount of at least 0.5 mol/L of total volume of the aqueous acid solution, preferably at least 1 mol/L. Also preferably, the additive salt is a chloride salt.
  • the treatment of the aqueous pregnant acid solution with oxalic acid and the additive salt may be carried out around 15°C or ambient temperature (25°C), or the solution may be heated up to 100°C.
  • the solution is heated to a temperature from 50°C to 100°C, and more preferably between 75°C and 100°C
  • the treatment step may also comprise adjustment of the pH of the solution.
  • the pH may be adjusted with a base, preferably a hydroxide, an oxide or a carbonate, or any combination thereof of potassium, ammonium, magnesium, or any combination of these bases.
  • the pH may be adjusted to a range between 0.5 and 3.5.
  • the pH may be adjusted between 1 and 3, and more preferably around 1.5.
  • the pH may be adjusted at any time during the process when necessary, for example before the addition of oxalic acid, simultaneously with the addition of oxalic acid, after the addition of oxalic acid, or a combination thereof.
  • the solution may be left to react for a certain period of time to allow the REE salts to form.
  • the reaction temperature may be maintained during this aging time.
  • the solution may then be left for the REE salts to settle for a period of time.
  • the temperature may also be maintained during the settling time.
  • the precipitated REE salts may then be recovered from the treated solution as a solid product. This step may be achieved by filtration or any suitable conventional methods.
  • the recovered REE salts may be submitted to additional treatments to further purify, separate, recover specific REEs, or the like.
  • the recovered precipitate may be calcinated, dissolved in an acid solution for further treatment, converted to hydroxides for acid dissolution, or any suitable recovery process commonly known in the art.
  • the solution obtained after the recovery of REEs precipitated salts may be further treated for recycling in any appropriate ore processing step.
  • the solution may be treated to raise the pH and therefore precipitate impu rities that may remain.
  • the pH can be raised from 1 to less than 3, or from 3 to 3.5.
  • the precipitated impurities may then be recovered, for example by filtration to provide a cleaned or partially cleaned solution.
  • This cleaned or partially cleaned solution may be subjected to further refining to recover possible remaining valuables metals or other valuable materials, for example, in a second leaching of dissolution step.
  • the oxalic acid was freshly prepared as 0.5 mol/L solution before each test.
  • the solution pH was measured with Orion 8102 BNUWP Ross UltraTM Combination pH probe.
  • ATC automatic temperature compensation
  • the pH was controlled manually whenever required using NaOH (50% solution) and H 2 S0 4 (10% solution).
  • 14% ammonium hydroxide was used to adjust pH instead of NaOH.
  • the reaction vessel was placed in a water bath sitting in a heating kettle (GLAS-COL), and the temperature was measured with a J-type thermal couple. Temperature control was realized through a GLAS-COL DigitrolTM II temperature controller.
  • the temperature could be controlled within a range of ⁇ 2°C. Ice pellets were used in the water bath to cool down the PLS temperature quickly, when required.
  • the reaction vessel containing 100 mL of PLS was first heated to the designated temperature and the pH was adjusted to the target level. Once the temperature of the solution was stabilized, the oxalic acid solution was slowly added through a micro pump at a constant rate, or through a glass pipette. The oxalic acid was delivered over a 30 minute period and agitation was provided by overhead stirrers. Unless otherwise stated, all experiments were executed in open vessels with a 30 minute reaction time (oxalic acid addition period). Following that, a 90 minute aging time was applied using the same agitation method and strength. During the aging period, the pH was monitored but not adjusted and the temperature was maintained. The solution was then allowed to settle for 20 hours. The settling temperature was maintained at the reaction temperature.
  • the PLS vessel was capped loosely during the aging and settling stages. At the end of the settling stage, the product was filtered through a microfilter set using a MilliporeTM filter paper. The solid was collected and oven-dried at 90°C to 100°C. The barren leaching solution (BLS) was measured for its volume and then samples were taken for chemical analysis by Can met MINING'S Analytical Service Group using both Inductively coupled plasma atomic emission spectroscopy (ICP AES) and Inductively coupled plasma mass spectrometry (ICP MS) methods.
  • ICP AES Inductively coupled plasma atomic emission spectroscopy
  • ICP MS Inductively coupled plasma mass spectrometry
  • REE recovery yield and oxalic stoichiometric consumption data were calculated from the analytical results.
  • the recoveries of metallic elements were calculated using the metal concentration in the BLS and PLS.
  • Metal balance calculations were practiced for REEs to locate significant errors in experimental or analytical procedures.
  • the oxalic acid consumption was defined as the addition amount of this reagent.
  • the reagent regenerated from the barren solutions or oxalate products was not counted in the calculation of reagent consumptions.
  • the oxalic acid consumption was counted as the times of stoichiometric amounts of oxalic acid required for all the REEs to precipitate as oxalate (times of stoichiometric demand - TSD).
  • the solution pH is an important factor for oxalate precipitation to properly proceed, since the pH is directly influencing the activity of the dissociated oxalate anion which is the direct precipitation reactant. It is known in the art that between pH 0 and pH 7, the higher the pH the higher the concentration of ionized oxalate. As a result, the increase of pH from 1 to 4 could theoretically reduce the demand of total oxalic acid addition.
  • Temperature has an impact on oxalate anion activity, oxalic acid solubility and oxalate metal complex stability. More importantly, an elevated temperature (e.g. 70°C-80°C) is recommended for producing strong and fully formed crystals that are easy to filter. Between 75 and 100°C, TREE recovery increased with increasing temperature, but all REE recoveries observed at high temperature were lower than that at 25°C ( Figure 4). Such an observation indicates that the room temperature and the high temperature oxalate precipitates have different chemistries. The response of oxalate precipitation at elevated temperature (i.e.
  • the temperature conditions that favour the formation of double salt may also increase the REE recovery in oxalate precipitation process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne un procédé de récupération d'éléments de terres rares dans une solution aqueuse. En particulier, l'invention concerne une précipitation directe d'oxalate d'éléments de terres rares à partir d'une solution d'acide aqueuse, comprenant le traitement avec une solution d'oxalate ou d'acide oxalique en présence d'un sel d'additif.
PCT/CA2017/050508 2017-04-26 2017-04-26 Précipitation directe d'oxalate pour la récupération d'éléments de terres rares WO2018195642A1 (fr)

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PCT/CA2017/050508 WO2018195642A1 (fr) 2017-04-26 2017-04-26 Précipitation directe d'oxalate pour la récupération d'éléments de terres rares

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PCT/CA2017/050508 WO2018195642A1 (fr) 2017-04-26 2017-04-26 Précipitation directe d'oxalate pour la récupération d'éléments de terres rares

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020181381A1 (fr) * 2019-03-12 2020-09-17 Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources Canada Procédé et système de récupération d'éléments des terres rares
WO2021011926A1 (fr) * 2019-07-17 2021-01-21 West Virginia University Systèmes et processus de récupération de concentré de terres rares de qualité élevée présentes dans un drainage minier acide
CN115369242A (zh) * 2022-09-06 2022-11-22 李星岚 一种浸出离子吸附型稀土过程的沉淀工艺
US11827954B2 (en) 2019-07-17 2023-11-28 West Virginia University Rare earth enrichment process by contacting raw material with a base at specific pH values
EP4107298A4 (fr) * 2020-02-21 2024-04-03 The Saskatchewan Research Council Procédé de récupération de terre rare à partir de minerais contenant de la bastnaesite
LU103142B1 (de) 2023-06-06 2024-12-06 thyssenkrupp Polysius GmbH Klimaschonende Puzzolanerzeugung
WO2024251709A1 (fr) 2023-06-06 2024-12-12 thyssenkrupp Polysius GmbH Production de puzzolana respectueuse du climat
DE102023114757A1 (de) 2023-06-06 2024-12-12 Thyssenkrupp Ag Klimaschonende Puzzolanerzeugung

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US4980141A (en) * 1987-05-26 1990-12-25 Mitsubishi Kinzoku Kabushiki Kaisha Hexagonal-bipyramid crystalline scandium oxide powder and a process for preparing the same
US5116560A (en) * 1991-03-22 1992-05-26 General Electric Company Method of forming rare earth oxide ceramic scintillator with ammonium dispersion of oxalate precipitates
US20130091989A1 (en) * 2011-10-13 2013-04-18 Yu-Lung Sun Method for recovering rare earth, vanadium and nickel
WO2014094037A1 (fr) * 2012-12-17 2014-06-26 Scandium Pty Ltd Procédé pour la production d'un matériau solide contenant du scandium de teneur en scandium augmentée
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US5116560A (en) * 1991-03-22 1992-05-26 General Electric Company Method of forming rare earth oxide ceramic scintillator with ammonium dispersion of oxalate precipitates
US20130091989A1 (en) * 2011-10-13 2013-04-18 Yu-Lung Sun Method for recovering rare earth, vanadium and nickel
WO2014094037A1 (fr) * 2012-12-17 2014-06-26 Scandium Pty Ltd Procédé pour la production d'un matériau solide contenant du scandium de teneur en scandium augmentée
US20160068929A1 (en) * 2014-09-08 2016-03-10 Patrick R. Taylor EXTRACTION OF RARE EARTH METALS FROM NdFeB USING SELECTIVE SULFATION ROASTING
CN106636689A (zh) * 2017-01-04 2017-05-10 江西理工大学 一种从稀土废水池沉淀渣中提取稀土的方法

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020181381A1 (fr) * 2019-03-12 2020-09-17 Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources Canada Procédé et système de récupération d'éléments des terres rares
WO2021011926A1 (fr) * 2019-07-17 2021-01-21 West Virginia University Systèmes et processus de récupération de concentré de terres rares de qualité élevée présentes dans un drainage minier acide
US11827954B2 (en) 2019-07-17 2023-11-28 West Virginia University Rare earth enrichment process by contacting raw material with a base at specific pH values
EP4107298A4 (fr) * 2020-02-21 2024-04-03 The Saskatchewan Research Council Procédé de récupération de terre rare à partir de minerais contenant de la bastnaesite
CN115369242A (zh) * 2022-09-06 2022-11-22 李星岚 一种浸出离子吸附型稀土过程的沉淀工艺
LU103142B1 (de) 2023-06-06 2024-12-06 thyssenkrupp Polysius GmbH Klimaschonende Puzzolanerzeugung
WO2024251709A1 (fr) 2023-06-06 2024-12-12 thyssenkrupp Polysius GmbH Production de puzzolana respectueuse du climat
DE102023114757A1 (de) 2023-06-06 2024-12-12 Thyssenkrupp Ag Klimaschonende Puzzolanerzeugung

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