JP6275138B2 - Treatment of lithium-containing materials - Google Patents

Treatment of lithium-containing materials Download PDF

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JP6275138B2
JP6275138B2 JP2015526829A JP2015526829A JP6275138B2 JP 6275138 B2 JP6275138 B2 JP 6275138B2 JP 2015526829 A JP2015526829 A JP 2015526829A JP 2015526829 A JP2015526829 A JP 2015526829A JP 6275138 B2 JP6275138 B2 JP 6275138B2
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lithium
leaching
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JP2015531826A (en
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シャルマ,ヤテンドラ
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リード アドバンスド マテリアルズ プロプライエタリー リミテッド
リード アドバンスド マテリアルズ プロプライエタリー リミテッド
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • C22B26/12Obtaining lithium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/04Halides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/08Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction 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
    • C22B3/10Hydrochloric acid, other halogenated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/02Light metals
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/14Electrolytic production of inorganic compounds or non-metals of alkali metal compounds
    • C25B1/16Hydroxides
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Process efficiency
    • Y02P10/21Process efficiency by recovering materials
    • Y02P10/212Recovering metals from waste
    • Y02P10/234Recovering metals from waste by hydro metallurgy

Description

  The present application relates to processing of lithium-containing materials.

  In particular, the invention relates to the treatment of lithium-containing materials and processes for the production of lithium hydroxide and lithium carbonate. This process utilizes the electrolysis of an aqueous lithium chloride solution obtained from lithiasite or concentrate, or brine. In certain aspects, the process of the present invention is provided to provide high purity or battery grade lithium hydroxide and lithium carbonate products.

  The process of the present invention can also provide a hydrochloric acid product. Further, in certain embodiments, the process of the present invention can utilize a noble metal-containing mixed metal oxide (MMO) electrode to increase the efficiency of the electrochemical portion of the process.

  Typically, known processes for producing lithium carbonate from lithium-containing ores or concentrates utilize heat treatment of α-lysian pyroxene or concentrates. This heat treatment is called “calcination” and converts α-lysian pyroxene into β-lysian pyroxene that can be dissolved by acid. The step in which the β-lysianite is dissolved in the acid occurs in a kiln furnace to produce a soluble lithium salt. The lithium salt passes through one or more tanks where the lithium salt is purified. The leached raw lithium salt then passes through a step where the pH of the slurry is adjusted, which facilitates precipitation of certain impurities including iron and magnesium. Therefore, the purified lithium salt is treated with soda ash to produce lithium carbonate. The lithium carbonate is further treated with slaked lime to produce lithium hydroxide.

  Typically, processes for the production of lithium carbonate and lithium hydroxide from brine use an evaporator to increase the concentration of salts contained therein before going through a series of steps to reduce the impurities present Has steps.

  The conventional processes described above are relatively inefficient in removing impurities remaining in the impregnated leach solution, resulting in the production of relatively low purity lithium hydroxide and lithium carbonate. This is particularly problematic when it is desired to produce high quality or battery grade lithium hydroxide and lithium carbonate products.

  The process of the present invention aims to substantially solve one or more of the aforementioned problems associated with conventional processes, or at least provide a beneficial alternative to this.

  The above description of the background art is only to help understanding of the present invention. This description is not an admission or admission that any material mentioned is (or was) part of the common general knowledge at the priority date stage of the application.

  Throughout the specification and claims, unless the text requires otherwise, the word “having”, or variations thereof, such as “having” are It is understood that any other number or group of numbers is not meant to be excluded, although it is meant to include groups.

  The term “battery grade lithium carbonate” means a product having a purity of about 99.5% or greater. Similarly, the term “battery grade lithium hydroxide” means a product having a purity of about 99% or greater.

In the present invention, a process for the treatment of a lithium-containing material comprising:
(I) preparing a process solution from the lithium-containing material;
(Ii) passing the process solution from step (i) through a series of impurity removal steps, thereby providing a substantially purified lithium chloride solution;
(Iii) passing the purified lithium chloride solution of step (ii) through an electrolysis step, thereby producing a lithium hydroxide solution;
(Iv) a step of carbonating the solution by passing pressurized carbon dioxide through the lithium hydroxide solution produced in the step (iii), whereby a lithium carbonate precipitate is produced. Steps,
I have a,
The lithium-containing material is α-lysian pyroxene or ore concentrate,
The process further comprises a first step, wherein a process is provided in which the α-lycia pyroxene ore concentrate is calcined to produce β-lysian pyroxene .

  In one aspect of the invention, the process solution of step (i) is prepared in the form of an impregnated leach solution. Preferably, the impregnated leaching solution is formed by passing a lithium-containing material through a leaching step, and the material is leached with hydrochloric acid.

  Preferably, the impurity removal step (ii) further includes a concentration step of concentrating the impregnated leach solution until the lithium chloride is substantially saturated.

  The lithium hydroxide solution generated in step (iii) may be thickened by evaporation of water to provide lithium hydroxide monohydrate crystals.

In yet another aspect of the present invention, the first portion of the lithium hydroxide solution produced in step (iii) is thickened by evaporation / crystallization to provide lithium hydroxide monohydrate crystals,
The second part is carbonated by passing pressurized carbon dioxide through the solution, thereby producing a lithium carbonate precipitate.

Preferably, the impurity removal step of step (ii) includes
Hydropyrolysis of Al and Fe chloride,
PH increase for precipitation of Al, Fe, Mg, and Mn hydroxide,
Lithium carbonate precipitation for removal of Ca, and
Has one or more of separate crystallization for Na and K removal.

  Preferably, the separation and crystallization for removing Na and K is performed immediately after the concentration step.

  The impurity removal step preferably further includes an ion exchange step. Preferably, the ion exchange step substantially removes all of calcium, magnesium, and other multivalent cations remaining in the process solution. Also preferably, the multivalent cation is removed to a level of less than about 10 ppm.

  Also preferably, during evaporation / crystallization, water evaporated from the solution is recompressed and combined with make-up vapor and utilized for evaporation / crystallization. In the evaporation / crystallization step, a vacuum evaporation crystallization apparatus is preferably used.

Preferably, the β-lysianite is cooled and milled prior to the leaching step. The β-lysianite is preferably milled to less than about 300 μm. Also, the β-lysian pyroxene is preferably milled to P 80 of about 75 μm.

  Preferably, the leaching step is performed at the heating temperature.

  The hydrochloric acid solution used in the leaching step is preferably about 20 wt% HCl.

  Preferably, the heating temperature in the leaching step is approximately the boiling point of the hydrochloric acid solution used in the leaching step.

  The leaching step is preferably performed at atmospheric pressure.

  In one form of the invention, the leaching step is performed in a chlorination furnace at about 108 ° C. for a residence time of about 6 to 10 hours. Preferably, the residence time is about 8 hours.

  The process of the present invention will now be described by way of example with reference to certain examples and the accompanying drawings.

2 is a schematic flowchart showing a process for processing a lithium-containing material according to the first embodiment of the present invention; The lithium-containing material is an α-lysian pyroxene concentrate.

  FIG. 1 shows a process 10 for the treatment of a lithium-containing material according to a first embodiment of the present invention. In this example, the lithium-containing material is provided in the form of an α-lysian pyroxene concentrate.

  All unit operations performed in process 10 are configured to operate continuously with full process equipment and control.

The α-lysian pyroxene concentrate 12 passes through the firing step and is fired in a firing furnace 14 at a temperature between about 1050 ° C. and 1100 ° C. to convert the α-lysian pyroxene into leaching β-lysian pyroxene. Off-gas from the calciner is directed through a cyclone (not shown) and an electrostatic sedimentation separator (not shown) configured to meet existing environmental emission limits. The resulting high-temperature fired product passes through the cooler 16 and is indirectly cooled to about 80 ° C. This is then dry milled in a mill, such as a closed circuit ball mill 18, to less than 300 μm, for example P 80 of about 75 μm.

  After storage in a surge bin (not shown), the milled β-lysianite is mixed in a slurry step in an excess of at least 40-300% from the stoichiometric ratio of 20 wt% hydrochloric acid. The slurry step is fed to a leaching step, for example a brewing circuit 22, which has a first leaching stage 24 and a second leaching stage 26.

  The leaching step is carried out in a continuous leaching tank for about 6 to 12 hours, for example about 8 hours, at about 108 ° C., which is the boiling point of the hydrochloric acid leaching solution added in the slurry step. The leaching circuit 22 uses a pulp density of about 40%, which maximizes the leaching concentration and does not exceed the lithium chloride solubility limit during leaching. The off gas is cleaned with a wet scrubber (not shown). The leaching step 22 produces a residual slurry and a process solution such as an impregnated leaching solution. Lithium and aluminosilicate in β-lysianite are leached into the solution together with other impurities, and a sub-saturated concentration of lithium chloride is obtained in the impregnated leach liquid.

  The impregnated leach solution from the leach circuit 22 passes through the thickening circuit 28. The thickening circuit 28 has preferably two stages 28a and 28b aligned with the stages 24 and 26 of the brewing circuit 22. Overflow from the thickening circuit 28 is directed to a hydrolysis step 30 that operates at about 300 ° C. Here, the chlorides of Al and Fe present in the impregnation and leaching solution are converted into insoluble oxides 32, respectively. Any residual HCl is recovered in the HCl removal step 34.

  In addition to the aforementioned Al and Fe recovered using hydropyrolysis step 30, most of the remaining soluble iron, aluminum, and magnesium is removed from the leachate liquid through a series of impurity removal steps. . This is shown in a broad sense by the impurity removal step 36 of FIG. The impurity removal step 36 further comprises a pH adjustment step 38, LiOH is added and the pH is raised to about 9. The product of step 38 passes through the belt filter 42, from which Al, Fe, Mn, and Mg containing precipitates are recovered. The impurity removal step 36 further includes a calcium precipitation step 44, with the addition of sodium carbonate (soda ash) or lithium carbonate 46 to produce a calcium-containing precipitate 48 from another belt filter 50.

  The thickener underflow product 52 of the second thickening step 28b passes through the drying step 54 before passing through the waste 56 and subsequent disposal 58.

  The liquid product of the belt filter 50 is mostly a LiCl solution, which passes through the fractionation crystallization step 62 after passing through the concentration step 60. In the concentration step 60, the LiCl solution is concentrated to near the saturation point, for example from 35 to 40 wt% LiCl and cooled to a sub-zero temperature. In the subsequent fractional crystallization step 62, the Na and K impurities 64 are largely removed as NaCl and KCl crystals by filtering, respectively.

  When substantially all of the aforementioned impurities have been removed, the lithium chloride solution passes through an ion exchange step 66. This step has an ion exchange (IX) column 68 that removes substantially all residual calcium, magnesium, and other multivalent cations to a level below about 10 ppm, for example a level of 1 ppm. .

  Next, another purified lithium chloride solution is heat treated at 90 ° C. and supplied to the electrolysis step 70. This has a large number of electrolysers, for example 6 to 20 electrolysers. Here, lithium chloride and water are consumed to produce lithium hydroxide, chlorine, and hydrogen.

  After passing through the electrolyzer, the thin or depleted lithium chloride solution contains dissolved chlorine gas. The dissolved chlorine is removed in two stages, just before the leaching circuit 22, before this thin lithium chloride solution is recycled to the slurry step. In the first stage, hydrochloric acid is added to the lithium chloride solution, the pH drops below 5, and a certain amount of chlorine gas is generated from the solution. The remaining dissolved chlorine gas is then removed with an air strip solution (not shown).

  Chlorine and hydrogen produced as by-products are combined to produce HCl, which is used in the slurry step and leaching circuit 22.

  The lithium hydroxide solution obtained in the electrolysis step 70 first passes through a holding tank 72, from which, as shown in FIG. 1, (i) volatilized and crystallized, monohydrate crystals of lithium hydroxide Or (ii) sent to a carbonation step to convert to lithium carbonate.

  In the first case of these options, lithium hydroxide in solution is crystallized, for example, in a vacuum evaporation crystallizer 80 (Oslo type) operating at a temperature of about 80 ° C. and a pressure of about 45 kPa. The residence time is about 60 minutes, which gives a coarse crystalline product. The resulting water vapor is recompressed and combined with makeup steam and used as a heating medium for the crystallizer 80.

The lithium hydroxide crystals are washed with cold water (not shown), and a washing efficiency of 99% is obtained. The resulting cleaning solution is recycled to the brewing circuit 22 as described above. The solids from the centrifuge are fed to an indirect furnace or dryer 82 operating at about 120 ° C. to dry the crystals. The crystalline product is battery grade LiOH.H 2 O, which is pneumatically transported to the product bottle 84 and is coated when it is finally transported to the packing station (not shown) It is cooled to 50 ° C. by a screw conveyor 86.

  In the second option described above, lithium carbonate is produced by carbonation of a lithium chloride solution. Here, in the carbonation vessel 90, the compressed carbon dioxide gas 88 passes through the lithium hydroxide solution, and lithium carbonate is precipitated. This slurry is supplied by a filter 94 to a washer / centrifuge 92, after which the wash water is recycled to the electrolyzer 70 with residual lithium hydroxide solution or with mother liquor. Undried lithium carbonate crystals are supplied to the dryer 96. Here, hot air is used and the crystals are dried. Medium pressurized air is used to heat the air. After drying, the battery grade lithium carbonate is refined to the particle size required by the customer and then packaged (not shown) before passing through storage bin 98.

  Condensate is used throughout the process as high temperature process water, cooling process water, and makeup water for cooling water. If the process does not return to condensate, an overall positive water balance occurs and about 1/10 of the process water is discharged into a sewage system (not shown).

It is envisioned that tantalite and alumina can also be recovered using the process of the present invention. The filter cake from the thickening step is discharged to a tantalite recovery plant (not shown). The discharge from the tantalite recovery plant is fed to a belt filter to remove moisture and this water returns to the tantalite recovery plant. The filter does not use a washing process and has a filtration area of 19 m 2 . The filter cake from the belt filter is dried in a direct furnace. The dried alumina silicate is cooled to 50 ° C. with a covered screw conveyor and then conveyed pneumatically to storage bins prior to shipping.

  In a second embodiment of the present invention, the lithium-containing material is provided in the form of a lithium-containing brine. Brine does not require a firing step, a cooling step, a milling step, and a leaching step as shown in the first embodiment of the present invention, but the process residue is the same as in the first embodiment described above. It is assumed that they are substantially equivalent.

  As mentioned above, the process of the present invention provides a process whereby high purity or battery grade lithium hydroxide and lithium carbonate products are obtained from alpha-lysian pyroxene or concentrate or from lithium-containing brine, Production of a hydrogen chloride gas product is also possible.

  Changes and modifications apparent to those skilled in the art are within the scope of the invention. For example, it is envisioned that brewing circuit 22 may have only a single brewing stage / operation without departing from the scope of the present invention.

Claims (20)

  1. A process for the treatment of lithium-containing materials,
    (I) passing the lithium-containing material through a leaching step, the leaching step having a first leaching stage and a second leaching stage, wherein the lithium-containing material is leached with hydrochloric acid and impregnated leaching A solution is produced,
    The first leaching stage is combined with a subsequent first thickening stage, and the second leaching stage is combined with a subsequent second thickening stage; and
    (Ii) hydrothermally decomposing the impregnated leach solution, whereby Al and Fe chlorides are converted to insoluble oxides and removed, the remaining hydrochloric acid is recovered, and the leach step (i) To be reused, steps,
    (Iii) passing the impregnated leach solution from step (ii) through an impurity removal step, thereby providing a lithium chloride solution ;
    (Iv) passing the lithium chloride solution of step (iii) through an electrolysis step, where only lithium chloride and added water are consumed, thereby producing only lithium hydroxide solution, chlorine, and hydrogen , Steps and
    (V) combining the chlorine and hydrogen produced in the electrolysis step (iv) to produce hydrochloric acid, wherein the hydrochloric acid is utilized in the leaching step (i) ;
    (Vi) a step of carbonating the lithium hydroxide solution produced in step (iv) by passing pressurized carbon dioxide, whereby a lithium carbonate precipitate is produced;
    Have
    The lithium-containing material is α-lysian pyroxene or ore concentrate,
    The process further comprises a first step, wherein the α-lysian pyroxene ore concentrate is calcined to produce β-lysian pyroxene.
  2. The process of claim 1 , wherein the impurity removal step ( iii ) comprises a concentration step of concentrating the impregnated leach solution until lithium chloride is saturated.
  3. The process according to claim 1 or 2 , wherein a part of the lithium hydroxide solution produced in the step ( iv ) is converted into lithium hydroxide monohydrate crystals by evaporation of moisture.
  4. The impurity removal step of the step ( iii ) includes:
    PH increase for precipitation of Al, Fe, Mg, and Mn hydroxide,
    Lithium carbonate precipitation for removal of Ca, and
    Having one or more separate crystallization for the removal of Na and K, The process according to claim 1.
  5. The process according to claim 4 , wherein the separation and crystallization for the removal of Na and K is performed immediately after the concentration step.
  6. The impurity removal step further comprises an ion exchange step, the process according to claim 4 or 5.
  7. 7. The process of claim 6 , wherein the ion exchange step substantially removes all of calcium, magnesium, and other multivalent cations remaining in the impregnated leach solution.
  8. 8. The process of claim 7 , wherein the multivalent cation is removed to a level of less than 10 ppm.
  9. 9. A process according to claim 7 or 8 , wherein the multivalent cation is removed to a level of less than 1 ppm.
  10. During evaporation / crystallization, water is evaporated from the lithium hydroxide solution is re-compressed, combined with makeup steam, is utilized for evaporation / crystallization, any one of claims 3 to 9 The process described in
  11. 11. The process according to any one of claims 3 to 10 , wherein a vacuum evaporation crystallization apparatus is used in the evaporation / crystallization step.
  12. The β- spodumene, before the step (i), is cooled is milling process according to any one of claims 1 to 11.
  13. 13. The process of claim 12 , wherein the [beta] -lysianite is milled to less than 300 [mu] m.
  14. The β- spodumene is milled to P 80 of 75 [mu] m, the process according to claim 12 or 13.
  15. 15. The process according to any one of claims 1 to 14 , wherein step ( iii ) is performed at a heating temperature.
  16. Wherein said hydrochloric acid solution used in the leaching step is 20 wt% of HCl, according to any one of claims 1 to 15 process.
  17. The process according to claim 16 , wherein the heating temperature of the leaching step is the boiling point of the hydrochloric acid solution used in the leaching step.
  18. The leaching step is carried out at atmospheric pressure A process according to any one of claims 1 to 17.
  19. The leaching step, in a chlorination furnace is carried out over a residence time of 6 to 10 hours at 108 ° C., the process according to any one of claims 1 to 18.
  20. 20. The process of claim 19 , wherein the leaching step is performed over a 8 hour residence time.
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Priority Applications (3)

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AU2012903483 2012-08-13
AU2012903483A AU2012903483A0 (en) 2012-08-13 Processing of Lithium Containing Ore
PCT/AU2013/000857 WO2014026217A1 (en) 2012-08-13 2013-08-01 Processing of lithium containing material

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KR (1) KR101857458B1 (en)
CN (1) CN104271781A (en)
AU (1) AU2013201833B2 (en)
CA (1) CA2851786C (en)
CL (1) CL2014001656A1 (en)
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CN102947225A (en) * 2010-02-17 2013-02-27 辛博尔股份有限公司 Processes for preparing highly pure lithium carbonate and other highly pure lithium containing compounds
CA2796849A1 (en) * 2010-04-23 2011-10-27 Simbol Mining Corp. A process for making lithium carbonate from lithium chloride

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KR101857458B1 (en) 2018-05-14
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