WO2014066727A1 - Procédé permettant de récupérer du scandium à partir d'une boue contenant des métaux - Google Patents

Procédé permettant de récupérer du scandium à partir d'une boue contenant des métaux Download PDF

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Publication number
WO2014066727A1
WO2014066727A1 PCT/US2013/066751 US2013066751W WO2014066727A1 WO 2014066727 A1 WO2014066727 A1 WO 2014066727A1 US 2013066751 W US2013066751 W US 2013066751W WO 2014066727 A1 WO2014066727 A1 WO 2014066727A1
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WO
WIPO (PCT)
Prior art keywords
scandium
liquor
solids
thorium
metal
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Application number
PCT/US2013/066751
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English (en)
Inventor
Larry J WESTRUM
Colin P ECKERLING
Caleb R OWEN
John M BIRMINGHAM
Original Assignee
Boulder Scientific Mining Company
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Filing date
Publication date
Application filed by Boulder Scientific Mining Company filed Critical Boulder Scientific Mining Company
Publication of WO2014066727A1 publication Critical patent/WO2014066727A1/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
    • 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
    • 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
    • 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 disclosed process relates generally to a method for extracting and concentrating scandium values from an aqueous slurry of metal-bearing residues, and more specifically to a process comprising nucleating thorium values from a metal-bearing slurry, returning said thorium values in situ by precipitation to said process and producing a solution that is substantially free from thorium from which scandium salts may be isolated.
  • Scandium is commonly grouped as a member of the rare earth elements including yttrium and the lanthanide metals in the Periodic Table of the Elements. It is modestly abundant in the earth's crust with a Clarke value of 25 ppm (Pohl, W.L. Economic Geology: Principle and Practice, Wiley-Blackwell, 2011, p 261). With few exceptions, scandium is found as a minor constituent of other economically important metalliferous minerals rather than as an enriched scandium mineral in its own right. High grade scandium ore is quite scarce and is found in only a few locations around the globe.
  • scandium and other rare earth elements are found dispersed at low levels in ores that are mined and processed for their primary value in tungsten, tantalum, aluminum, nickel, niobium, zirconium, titanium or uranium.
  • scandium is often associated with other secondary metals such as iron, manganese, vanadium, and thorium.
  • Waste streams in the form of liquors, slag, slimes, sludge, slurries or solid discharge from the primary metal process may be suitable for processing to recover secondary metal values, such as scandium.
  • the partitioning and ultimate isolation of purified scandium value from a mineral or a process waste stream containing many metallic constituents will generally rely on differential chemical or physical properties.
  • One technique involves treating a scandium-bearing pulp or slurry with a strong mineral acid to extract said scandium and other metals from the solids and provide for a first stage of separation.
  • Selective affinity of dissolved metal ions for a solvent or for a coordinating chemical functionality like a halide, sulfate, carbonate, or carboxylate ion, etc. will lead to a partitioning of the metal ion between phases.
  • Dissolved aqueous metal ions may undergo characteristic ligand ion-exchange in solution to produce insoluble salts which may be separated by precipitation and filtration.
  • a solid phase resin bearing a monodentate or bidentate ligand with a high relative affinity for dissolved scandium may be used to scavenge scandium directly from a pregnant liquor.
  • thorium is often present in ores containing scandium. Because thorium will readily accompany scandium through a purification scheme, it is therefore desirable to reject thorium from a scandium process stream in the early stages in order to avoid its concentration. Thorium may be partitioned away from scandium using ion selective resins (US Patent No. 4,765,909) or by liquid-liquid extraction (US Patent No. 2,990,244).
  • An input slurry stream may also contain significant levels of iron as mentioned above.
  • the oxidation state of said iron is nominally Fe(II) but Fe(III) may be present. Because Fe(III) interferes with chelating resin extraction performance, it is desirable to reduce Fe(III) to the Fe(II) state in solution. This may be conducted by contacting the solution to any of a variety of reducing agents including the elemental forms of magnesium, calcium, iron, tin, or zinc. Following the reduction of Fe(III) the resulting solution is filtered of solids.
  • the disclosed process provides for a method to economically recover available scandium from metal-bearing residues such as those originating from a bed effluent of a fluidized bed chlorination process comprising titanium-bearing ores. Unlike prior techniques, the disclosed process avoids the use of hydrocarbon solvents and hydrophobic extractants. In addition, the disclosed process allows for the rejection of metals such as thorium from a scandium solution in an early phase of the process in order to avoid the subsequent concentration thereof. The disclosed process also minimizes potential interferences with chelating resin extractions.
  • the disclosed process provides for a method of recovering scandium values in a metal-bearing effluent.
  • the disclosed process rejects thorium from a pregnant liquor which thereby minimizes later removal efforts.
  • a reduction step can be implemented to minimize potential interferences during chelating resin extractions.
  • the disclosed method provides for the recovery of available scandium from a metal- bearing stream without having to use hydrocarbon solvents and hydrophobic extractants.
  • the disclosed process provides a method of substantially rejecting thorium from a scandium-bearing solution in an early phase of the process in order to avoid a subsequent concentration of thorium.
  • the disclosed process provides a method of adjusting a pH of an acidulated metal- bearing slurry to cause a nucleation of thorium solids to occur.
  • the disclosed process provides a method of producing a liquor from a metal-bearing stream that is substantially free of thorium which may be used as an input stream for a scandium isolation phase.
  • the disclosed process provides a method of producing a liquor from a metal-bearing stream that is substantially free of Fe(III) which may be used as an input stream for a scandium isolation phase.
  • the disclosed process provides for a method of using a conventional scandium isolation process to receive a stream substantially free of thorium for scandium concentration purposes.
  • the disclosed process provides for a method of using a conventional scandium isolation process to receive a stream substantially free of Fe(III) for scandium concentration purposes.
  • the disclosed process provides for a method of recovering scandium values from a titanium carbothermal chlorination waste stream.
  • FIG. 1 depicts a general flow diagram for a process capable of recovering scandium values from an effluent slurry.
  • FIG. 2 shows the transition in solubility of thorium and scandium in a pH range of interest.
  • FIG. 3 shows a general comparison of metal concentrations at a beginning and an end of the disclosed process.
  • FIG. 1 depicts a process for recovering scandium values from a fluidized bed effluent. Although a fluidized bed effluent was used, it will be evident that the disclosed process may be used to recover scandium values from other metal-bearing slurries.
  • the process from which the bed effluent originates comprises the carbothermal chlorination of ilmenite and optionally other titanium containing ores.
  • Solid residues from the chlorination process are disengaged from the titanium tetrachloride stream and combined with water to produce an acidic slurry 1 containing scandium values found in the solution phase, in the suspended solids, and in the sediment.
  • Overall scandium levels in the slurry are low with a nominal concentration of about 25 ppm spread across the solid and solution phases.
  • Acidic slurry 1 serves as the input stream for the disclosed process. It is
  • the disclosed process may comprise unit operations conducted as a continuous process, batch process, semi-batch process, or a combination thereof.
  • Scandium is prepared for isolation from the input slurry by acidification of said slurry with an acid 2 which may comprise hydrochloric acid, hydrofluoric acid, sulfuric acid, sulfurous acid, or a combination thereof.
  • Acidulation 3 allows scandium from suspended solids and sediment to be released into the solution phase thereby forming a first liquor LIQi. It is contemplated that acidulation of the slurry may be performed within a range of temperatures from about 15 °C to about 85 °C and for a residence time of about thirty (30) seconds to about three (3) hours. Acid concentration comprises a range corresponding to a pH of about 0.00 to about 1.70.
  • nucleating agent 4 may comprise an alkali metal hydroxide or an alkaline earth metal hydroxide, however other agents may be used.
  • nucleating agent 4 may comprise an alkali metal hydroxide or an alkaline earth metal hydroxide, however other agents may be used.
  • ammonium hydroxide or an alkali metal carbonate could be suitable.
  • First liquor LIQi is dewatered 7 whereby a second liquor LIQ 2 (about 0 °C to about 50 °C) is carried forward. Spent solids from the dewatering step are directed from the process stream to solid waste 8.
  • Second liquor LIQ 2 is contacted with a reducing substance to reduce interfering cation Fe(III) to Fe(II).
  • a reducing element or ion produces a third liquor LIQ3.
  • Reduction 9 minimizes unproductive Fe(III) complexation with the ion exchange resin used in subsequent stages of the disclosed process.
  • Third liquor LIQ 3 which comprises a diminished level of interfering Fe(III) ions is carried forward to an ion exchange resin bed (not shown) in which a stripping of scandium takes place.
  • ion exchange resin bed not shown
  • it is contemplated that some or all of second liquor LIQ 2 may optionally be sent through a reduction bypass circuit 10 whereby the bypass liquor may be introduced directly to the ion exchange resin bed (not shown).
  • the reducing substances used herein comprise non- interfering metals which upon oxidation by Fe(III) may be rejected from the process stream.
  • non-interfering metals may comprise iron, tin, zinc, calcium or magnesium.
  • Third liquor LIQ 3 and/or the bypass liquor may optionally be adjusted with a strong mineral acid to ensure a pH range of about 1.70 to about 2.10 prior to contact with the chelating cation exchange resin.
  • third liquor LIQ 3 is contacted with an ion exchange resin 12 in the resin bed (not shown) at such a rate so as to avoid losses by channeling or inadequate equilibration and in a temperature range of about 0 °C to about 50 °C.
  • resin 12 comprises a chelating iminodiacetic acid such as commercially available Amberlite 748i.
  • stripping solution 11 comprising a strong mineral acid or salt or a chelating carboxylic acid. Stripping solution 11 is used to strip scandium and other metals from resin 12 thereby producing a fourth liquor LIQ 4 enriched in scandium (pregnant influent liquor). It is contemplated that stripping solution 11 can comprise hydrochloric acid, hydrofluoric acid, sulfuric acid, sulfurous acid, nitric acid or a combination of said acids at a strength of about 3.0 to about 9.0 moles of acid equivalent per liter.
  • An aqueous chelating acid solution comprising citric acid, tartaric acid, lactic acid, malic acid, diglycolic acid, o-phthalic acid, salicylic acid or a combination of a chelating acid and a mineral acid may be used.
  • a pH additive 14 such as alkali metal hydroxide is used to adjust the pH of fourth liquor LIQ 4 to a pH range of about 1.80 to about 2.10 whereby a fifth liquor LIQ 5 is formed.
  • Fifth liquor LIQ 5 is passed through a resin bed comprised of chelating ion exchange resin 17 such as Amberlite 748i at a temperature range of about 0 °C to about 35 °C.
  • the scandium values are adsorbed on resin 17 while barren effluent 18 is directed to waste or for use as process water.
  • stripping solution 16 comprising a strong mineral acid.
  • One or more bed volumes of stripping solution 16 may be used to strip resin 17 of scandium and other metals thereby producing a sixth liquor LIQ6 enriched in scandium.
  • stripping solution 16 can comprise hydrochloric acid, hydrofluoric acid, sulfuric acid, sulfurous acid, nitric acid or a combination of said acids at a strength of about 3.0 to about 9.0 moles of acid equivalent per liter.
  • Additives 19 comprise ammonium carbonate, ammonium hydroxide or oxalic acid. It is contemplated that monocarboxylic acid, dicarboxylic acid or tricarboxylic acid, non-metallic hydroxides, non-metallic carbonates, or non-metallic organic carboxylates could also be used.
  • the precipitate is dewatered to produce a compact cake of scandium enriched solids 22. The remaining solution or mother liquor 21 will be returned to the disclosed process.
  • the scandium stripping step comprises contacting one or more resultant liquors with an ion exchange resin in a resin bed.
  • an ion exchange resin in a resin bed.
  • FIG. 3 shows a comparison of metal concentrations at the beginning and end of the disclosed process.
  • the solid line represents the metal values detected in the input slurry.
  • the dotted line represents the metal values detected in the second resin strip solution (sixth liquor LIQ 6 ) EXAMPLE 1
  • a 513.6 g sample of titanium dioxide sump slurry was treated with 18 mL of 12 M hydrochloric acid. This pH adjustment, from 2.18 to 0.13, causes the lixiviation of scandium. To induce thorium nucleation the pH was adjusted using 30 mL of 6 M sodium hydroxide to a pH of 1.66. The slurry was filtered and 34.3 g of residue was isolated. The residue was analyzed and found to contain 4.16 mg of scandium, and 19.04 mg of thorium. 504.1 g of filtrate was isolated and determined to contain 10.31 mg of scandium and 4.31 mg of thorium by ICPMS.
  • the filtrate contained 947.8 mg of Fe, 162.7 mg of Mn, 26.40 mg of V, and 94.78 mg of Al, per mg of Sc.
  • the filtrate underwent a reduction using 20.167 g of iron powder.
  • the slurry was agitated for approximately 15 seconds before any residual iron powder was recovered via magnetic separation affording the reduction liquor. Unreduced ferric iron was not detectable with potassium thiocyanate as an indicator.
  • the reduction liquor was passed through 13 mL of Amberlite-748i ion exchange resin.
  • the column was pre conditioned using 200 mL of 6 M hydrochloric acid followed by 100 mL of pH 2.04 hydrochloric acid solution. Through the resin bed was passed 38.78 bed volumes of ferrous filtrate at a flow rate of 0.37 bed volume/min or 4.85 mL/min.
  • the effluent solution was collected and analyzed.
  • the effluent solution contained 2.44 mg of scandium, a 16.88 % Sc loss.
  • the column was washed with 4.85 bed volumes of pH 2.04 hydrochloric acid solution resulting in a 1.37 % Sc loss.
  • the wash and effluent contained 99.9 % Fe, 99.9 % Mn, 89.17 %, V and 99.0 % of the respective influent metal mass.
  • the resin was quantitatively stripped using 22.9 g of 3 M hydrochloric acid.
  • For the second pass through the resin bed 28.35 g of influent resulted in 27.233 g of effluent containing 0.00 % of the initial scandium.
  • the column was washed with 43.85 g of pH 2.04 hydrochloric solution. 0.74 % of the initial scandium was lost in the wash solution.
  • the second resin bed effluent contained 100.00 % Fe, 99.99 % Mn, 47.19 % V, and 99.54 % Al by comparison to the influent metal mass.
  • the column was stripped and regenerated using 25.05 g of 3 M hydrochloric acid.
  • the final solution was analyzed and found to contain 7.56 mg of scandium for a final scandium recovery of 52.65
  • the disclosed process can be used in conjunction with a scandium isolation phase capable of stripping a scandium value from a metal-bearing stream.
  • the disclosed process comprises a method of providing a stream substantially free of thorium, and optionally Fe(III), for input into a scandium isolation phase which can comprise ion exchange and/or liquid- liquid extraction methodologies.
  • the disclosed process comprises the steps of:
  • the disclosed process can also be used in conjunction with a scandium isolation phase capable of stripping a scandium value from a titanium carbothermal chlorination waste stream.
  • the disclosed process comprises a method of providing a stream substantially free of thorium, and optionally Fe(III), for input into a scandium isolation phase which can comprise ion exchange and/or liquid-liquid extraction.
  • the disclosed process comprises the steps of: a) Treating an aqueous carbothermal chlorination waste slurry comprising metal- bearing solids with a strong mineral acid thereby producing a first liquor;
  • Also disclosed is process for isolating scandium values from a metal-bearing waste stream comprising the steps of: treating a slurry comprising metal-bearing solids with a strong mineral acid thereby producing a first liquor; maintaining the first liquor at a temperature and for a period of time sufficient to dissolve scandium values from the metal- bearing slurry solids; adjusting a pH of the first liquor to cause a nucleation of thorium solids to occur; dewatering precipitated solids from the first liquor thereby separating the nucleated thorium solids and producing a second liquor substantially free of thorium; treating the second liquor with a reducing agent to reduce Fe(III) to Fe(II) and to thereby produce a third liquor substantially free of Fe(III) to be used as an input stream for a scandium isolation phase; and introducing the third liquor into a scandium isolation process whereby scandium values are stripped therefrom.
  • the second liquor can be introduced directly into a scandium isolation phase as an input stream.
  • the scandium isolation process of the disclosed method further comprises the steps of: treating the third (or second) liquor with a chelating cation exchange resin in protonated form to strip Sc(III) therefrom and thereby produce a barren effluent substantially free of scandium values; and contacting the cation exchange resin with a stripping agent to release scandium values bound thereto to a fourth liquor.
  • the scandium isolation process further comprises the steps of: adjusting a pH of the fourth liquor to form a fifth liquor; treating the fifth liquor with a second chelating cation exchange resin in protonated form to strip Sc(III) therefrom and thereby produce a barren effluent substantially free of scandium values; and contacting the second cation exchange resin with a stripping agent to release scandium values bound thereto to a sixth liquor.
  • the fourth liquor and/or the sixth liquor may be treated with a precipitation agent to produce scandium-enriched solids which are subsequently dewatered to produce a scandium enriched cake.
  • an apparatus capable of housing a slurry comprising metal-bearing solids for treatment with a strong mineral acid whereby a first liquor is produced, the apparatus capable of maintaining the first liquor at a temperature and for a period of time sufficient to dissolve scandium values from the metal-bearing slurry solids and wherein a pH of the first liquor can be adjusted to cause a nucleation of thorium solids to occur; the apparatus capable of separating the nucleated thorium solids whereby a second liquor substantially free of thorium is produced.
  • the disclosed apparatus further being capable of reducing Fe(III) to Fe(II) whereby a liquor substantially free of Fe(III) is produced.

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  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

La présente invention se rapporte à un procédé et à un appareil permettant de récupérer des valeurs de scandium dans un effluent contenant des métaux, par exemple à partir d'un procédé de chloration en lit fluidisé, sans utiliser des solvants d'extraction et des solvants organiques qui ne sont pas biodégradables. Le procédé de la présente invention rejette le thorium d'une liqueur mère, ce qui permet de réduire plus tard à un minimum les efforts d'élimination. Le procédé consiste à aciduler une boue de déchets afin d'obtenir une première liqueur qui contient du scandium dissous et d'autres métaux, y compris du thorium. L'ajustement du pH de la première liqueur provoque la nucléation du thorium dissous et son renvoi in situ par précipitation. La déshydratation du précipité entraîne la formation de matières solides appauvries en scandium et une seconde liqueur qui contient du scandium qui est sensiblement dépourvue de thorium et qui est sélectivement divisée lors d'une phase de support de matières solides et, par la suite, éliminée de la résine au cours d'une série d'étapes d'échange d'ions pour produire une liqueur de scandium de laquelle peuvent être isolées des matières solides contenant du scandium. Une étape de réduction aide à réduire à un minimum les interférences potentielles pendant les extractions de la résine de chélation.
PCT/US2013/066751 2012-10-26 2013-10-25 Procédé permettant de récupérer du scandium à partir d'une boue contenant des métaux WO2014066727A1 (fr)

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US201261718946P 2012-10-26 2012-10-26
US61/718,946 2012-10-26

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9102999B2 (en) 2013-01-10 2015-08-11 Bloom Energy Corporation Methods of recovering scandium from titanium residue streams
EP3710607A4 (fr) * 2017-11-17 2021-08-25 II-VI Delaware, Inc. Récupération sélective de métaux des terres rares à partir d'une suspension acide ou d'une solution acide
CN114599439A (zh) * 2019-10-28 2022-06-07 力拓铁钛加拿大公司 钪浓缩物的纯化

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4765909A (en) * 1987-04-23 1988-08-23 Gte Laboratories Incorporated Ion exchange method for separation of scandium and thorium
US4988487A (en) * 1989-10-24 1991-01-29 Gte Laboratories Incorporated Process for recovering metal values such as scandium, iron and manganese from an industrial waste sludge
JPH08232026A (ja) * 1995-02-24 1996-09-10 Mitsubishi Materials Corp スカンジウムの精製方法
JP2000313928A (ja) * 1999-04-26 2000-11-14 Taiheiyo Kinzoku Kk 酸化鉱石からニッケルとスカンジウムを回収する方法
JP2007231382A (ja) * 2006-03-01 2007-09-13 Mitsui Mining & Smelting Co Ltd 希土類元素の回収方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4765909A (en) * 1987-04-23 1988-08-23 Gte Laboratories Incorporated Ion exchange method for separation of scandium and thorium
US4988487A (en) * 1989-10-24 1991-01-29 Gte Laboratories Incorporated Process for recovering metal values such as scandium, iron and manganese from an industrial waste sludge
JPH08232026A (ja) * 1995-02-24 1996-09-10 Mitsubishi Materials Corp スカンジウムの精製方法
JP2000313928A (ja) * 1999-04-26 2000-11-14 Taiheiyo Kinzoku Kk 酸化鉱石からニッケルとスカンジウムを回収する方法
JP2007231382A (ja) * 2006-03-01 2007-09-13 Mitsui Mining & Smelting Co Ltd 希土類元素の回収方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9102999B2 (en) 2013-01-10 2015-08-11 Bloom Energy Corporation Methods of recovering scandium from titanium residue streams
EP3710607A4 (fr) * 2017-11-17 2021-08-25 II-VI Delaware, Inc. Récupération sélective de métaux des terres rares à partir d'une suspension acide ou d'une solution acide
CN114599439A (zh) * 2019-10-28 2022-06-07 力拓铁钛加拿大公司 钪浓缩物的纯化

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