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WO2023275346A2 - Extraction de lithium mica - Google Patents

Extraction de lithium mica Download PDF

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Publication number
WO2023275346A2
WO2023275346A2 PCT/EP2022/068230 EP2022068230W WO2023275346A2 WO 2023275346 A2 WO2023275346 A2 WO 2023275346A2 EP 2022068230 W EP2022068230 W EP 2022068230W WO 2023275346 A2 WO2023275346 A2 WO 2023275346A2
Authority
WO
WIPO (PCT)
Prior art keywords
lithium
mica
calcium carbonate
gypsum
mixture
Prior art date
Application number
PCT/EP2022/068230
Other languages
English (en)
Other versions
WO2023275346A3 (fr
Inventor
Roderick SMITH
Original Assignee
British Lithium Limited
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 British Lithium Limited filed Critical British Lithium Limited
Publication of WO2023275346A2 publication Critical patent/WO2023275346A2/fr
Publication of WO2023275346A3 publication Critical patent/WO2023275346A3/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/06—Sulfates; Sulfites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/06—Sulfating roasting
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/42—Micas ; Interstratified clay-mica products
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • 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
    • 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 invention relates to a process for the mobilisation of lithium from lithium micas by calcination and neutral pH aqueous leaching to form a leach solution enriched in lithium.
  • Lithium micas present an important source of lithium that is likely to grow in significance as the demand for lithium is expected to increase considerably in light of a worldwide effort to reduce carbon emissions.
  • Lithium from salar brines requires pumping and evaporation of vast quantities of water to extract and concentrate brines before impurity removal to produce a final lithium salt product.
  • Spodumene a lithium-bearing pyroxene mineral, is mined from hard rock deposits and typically requires high temperature roasting at approximately 1,000°C and acid leaching to produce a lithium-enriched brine or pregnant leach solution that is then purified to obtain a final lithium salt product.
  • Lithium micas could be an alternative hard rock source of lithium, but these have never been exploited commercially. These lithium micas occur within granites in Europe and elsewhere, and contain gangue minerals, principally quartz and feldspar. Exploiting these deposits commercially requires formulation of economic and environmentally sustainable methods for extraction of lithium salts of acceptable quality from these micas.
  • Lithium micas are structurally classed as tri-octahedral micas and can exist in a solution series whose end members are polylithionite (KLi 2 AISi40io(F,OH) 2 ; potassium lithium aluminium silicate fluorite hydroxide) and siderophyllite (KFe 2 AI(Al 2 Si 2 )Oio(F,OH) 2 ; potassium iron aluminium silicate hydroxide fluoride) .
  • Zinnwaldite KLiFeAI(AISi 3 )Oio(OH,F) 2 ; potassium lithium iron aluminium silicate hydroxide fluoride
  • Zinnwaldite is one such example of a mica that forms part of this solid solution series.
  • lithium micas contain a wider range of elements than spodumene, the conventional hard rock source of lithium, which is LiA ShOe) (lithium aluminium inosilicate) and they are consequently less rich in lithium than spodumene.
  • LiA ShOe lithium aluminium inosilicate
  • the lower Li content and more complex mineralogy of lithium micas compared to spodumene gives rise to the need for an extraction process to generate brine from lithium-mica minerals that affords improved recovery of lithium at a lower cost and environmental impact through reduced and more targeted use of reagents and more optimised roasting conditions, bringing fewer contaminants into solution.
  • One known method for the extraction of Li from micas relies on elevated temperature leaching of micas in sulphuric acid, either at atmospheric pressure or in an autoclave or other device to increase pressure. This method does not rely on calcining in the presence of a sulphate salt, instead relying on the sulphuric acid, heated to a temperature in excess of 90 °C, to act as the lixiviant which results in a significant environmental burden in the form of acidified waste streams.
  • the present invention provides a process for recovering lithium from lithium mica, the process comprising: mixing lithium mica with gypsum and calcium carbonate (CaCC ) to provide a lithium mica concentrate-salt mixture; and calcining the lithium mica salt mixture at a predetermined temperature for a predetermined time to provide a calcined lithium sulphate containing product.
  • CaCC calcium carbonate
  • the lithium mica may, in one or more embodiments, be a product of beneficiation.
  • the process is preferably free from hydrated lime.
  • the predetermined temperature of the calcining step is preferably in the range of between 750°C and about 1100°C, preferably between 800°C and 1100°C, preferably between 800°C and lOOCrC.
  • the predetermined time for the calcining step is preferably between 15 and 120 minutes.
  • the process of the present invention eliminates a step within the conventional lithium extraction process.
  • the process of the present invention is therefore free of milling, grinding or crushing of the mica prior to calcining.
  • the increased surface area of the calcined lithium sulphate containing product increases the leaching recovery rate of the product.
  • the present invention provides a process for the extraction of lithium from mica with a reduced number of associated steps, reduced energy requirements, reduced associated labour and cost implications, and reduced carbon footprint whilst providing improved lithium recovery compared to conventional processes.
  • the sulphate salt(s) present within the gypsum is preferably present within the mixture such that the total sulphate salt(s) concentration is in a stoichiometric excess compared to the concentration of lithium within the lithium mica.
  • the calcium carbonate is preferably provided in the form of limestone.
  • the ratio of lithium mica to calcium carbonate within the mixture is preferably within the range of 6: 1 and 3: 1.
  • the ratio of mica to gypsum to calcium carbonate is within the range of between 6: x: 1 and 6: x: 2.
  • the ratio of lithium mica to sulfate salt(s) present within the gypsum is within the range of 6: 1 and 2:1.
  • the ratio of mica to gypsum to calcium carbonate is within the range of between 6: 1: x and 6: 3: x.
  • the calcining step occurs within a rotary kiln.
  • the process may comprise pelletising of the lithium mica, gypsum and calcium carbonate mixture prior to the calcining step.
  • the lithium mica is calcined without the use of prior milling or grinding steps to reduce particle size of the lithium mica.
  • the particle size distribution for Pso of the calcined lithium sulphate containing product is less than 1 mm, preferably less than 350 pm, preferably less than 250 pm, preferably about 75 pm or less.
  • the process preferably further comprises leaching of the calcined lithium sulphate containing product in a leach liquor comprising waterto provide a lithium enriched pregnant leach liquor.
  • the calcined lithium sulphate containing product may be introduced to water having a neutral pH.
  • the leach liquor such as for example water, is preferably free of pH modifiers.
  • the calcined lithium sulphate containing product is discharged directly, without additional cooling prior to discharge, into water.
  • the process of the present invention can be used to achieve >80% recovery of lithium into the pregnant leach solution.
  • the pregnant leach solution can be purified to produce the final lithium salts.
  • the pulp density of the lithium enriched pregnant leach liquor is between 7% and 40%, preferably between 10% and 35%, for example between 10% and 30%.
  • the process of the present invention has also been found to reduce fluorine gas evolution. Due to the fluorine content of mica, the evolution of fluorine gas is a concern which could pose a significant health risk.
  • Table 1 illustrates the pH of leach liquor resulting from the calcination of different ratios of mica: sulphate salt: calcium salt:
  • Table 1 shows that the resultant pregnant leach formed after the calcining step was always alkaline with a pH ranging from 7.8 to 10.8.
  • the fluorine content in the feed forthe calcining step, in the leach residue and in the pregnant leach liquor was assayed. It was found that 100% of the fluorine content in the feed mixture was present within the leach residue and the pregnant leach liquor. As a result, it is considered that any fluorine gas liberated from the mica during calcining, and on exposure to water, is converted to hydrofluoric acid (HF) which is subsequently neutralised by the presence of alkaline calcium carbonate forming insoluble compounds that remain in the leach residue.
  • HF hydrofluoric acid
  • the calcium carbonate is the feed mixture is preferably present at a level in excess of stoichiometric requirements to neutralise the generated hydrofluoric acid.
  • the present invention therefore provides a process for extracting lithium from lithium mica with reduced generation of fluorine gas.
  • Figure 1 is a graph illustrating the relationship between lithium recovery (%) and the ratio of calcium carbonate or the ratio of hydrated lime;
  • Figure 2 is a flow chart of one embodiment of the process of the present invention for extracting lithium from lithium-mica minerals;
  • Figure 3 is a further schematic illustration of the calcinating and leaching process according to one embodiment of the present invention for extracting lithium from lithium-mica minerals;
  • Figures 4A and 4B are graphs illustrating the relationship between lithium recovery (%) from ground feed mixture and unground feed mixture at differing temperatures
  • Figure 5 is a graph illustrating the relationship between pulp density and lithium recovery (%).
  • Figure 6 is a graph illustrating the relationship between leaching time and lithium recovery (%) post-calcination of 6:3.8:2
  • Mica gypsum: limestone at 1000°C for 50 minutes.
  • the graph shows that as the ratio of calcium carbonate increases within the feed mixture (i.e. within the feed mixture of lithium mica, gypsum and calcium carbonate), the lithium recovery (%) achieved by the process of the present invention increases. This is in contrast to a conventional process for extraction lithium from lithium mica using a feed mixture of lithium mica, gypsum and hydrated lime.
  • Figure 1 shows that as the ratio of hydrated lime increases within the feed mixture (i.e. within the feed mixture of lithium mica, gypsum and hydrated lime), the lithium recovery (%) achieved by the process of the present invention decreases.
  • the increased lithium recovery obtained using calcium carbonate, rather than hydrated lime may result from the significantly lower moisture content within calcium carbonate.
  • the hydrated lime (calcium hydroxide) decomposes to calcium oxide and water:
  • the moisture created during decomposition of hydrated lime has been found to increase adherence of the feed mixture to the apparatus and is therefore considered to reduce limestone recovery further.
  • the process for extracting lithium material from lithium mica material comprises mixing lithium mica with gypsum and calcium carbonate (CaCC>3) to provide a lithium mica concentrate-salt mixture; and calcining the lithium mica salt mixture at a predetermined temperature for a predetermined time to provide a calcined lithium sulphate containing product (101).
  • the sulphate salt(s) within the gypsum may be present within the mixture such that the total sulphate salt(s) concentration is at least stoichiometrically equal to the concentration of lithium within the lithium mica material.
  • the sulphate salt(s) present within the mixture such that the total sulphate salt(s) concentration is in a stoichiometric excess compared to the concentration of lithium within the lithium mica material.
  • Calcium carbonate may be provided in the form of limestone.
  • Mixture 1 the ratio of lithium mica to sulfate salt (within gypsum) to carbonate salt (within limestone) is 6: 3: 2;
  • Mixture 2 the ratio of lithium mica to sulfate salt (within gypsum) to carbonate salt (within limestone) is 3: 3: 1.
  • the ratio of lithium mica to carbonate salt(s) within the mixture is preferably within the range of 6: 1 and 3: 1.
  • the ratio of lithium mica to sulfate salt(s) is preferably within the range of 6: 1 and 2:1.
  • the ratio of lithium mica to sulfate salt to carbonate salt(s) is preferably within the range of between 6: x: 1 and 6: x: 2.
  • the ratio of lithium mica to sulfate salt(s) to carbonate salt(s) is preferably within the range of between 6: 1: x and 6: 3: x.
  • the mixture is calcined within a rotary calciner (102). It is however to be understood that the mixture may be calcined in any suitable calcining vessel as is not to be limited to a rotary calciner.
  • the angle of inclination of the calciner tube, rotation speed of the calciner tube, and rotation speed of the screw feeder of the rotary calciner can each be varied.
  • the dynamics of the mixture within the calcining vessel, for example within the rotary calciner, is of importance to ensure sufficient mixing and blending of the material, to improve calcination, and to reduce sintering of the mixture by preventing material from contacting inner walls of the vessel for prolonged periods of time.
  • the rotary parameters of the rotary calciner are each selected to provide a cascading mixing motion of the mixture within the vessel.
  • the rotary parameters of the calcining vessel are optimised to maximise residence time inside the tube.
  • the speed of rotation is approximately 1 rpm.
  • the feed mixture is heated to any suitable temperature within the calcining vessel within the range of about 750 °C to 1100 °C. It is to be understood that the mixture may be heated to any suitable temperature within the calcining vessel, for example within the range of 800 °C to 1100 °C, preferably within the range of 800 °C to 1000 °C, preferably within the range 900 °C to 1000 °C.
  • the calcining step is carried out for a period of between 30 and 50 minutes, however it is to be understood that the calcining step may be performed for any suitable duration, such as for example between 15 minutes and 120 minutes.
  • the calcium is present to aid the conversion process by raising the sintering temperature of the mixture as well as capture any gases that may evolve during the calcining process such as fluorine gas.
  • the calcining process i.e. the addition of the sulphate salt(s) and calcium carbonate
  • the furnace may provide a controlled residence time of between 15 and 120 minutes in the hot zone.
  • the calcined lithium sulphate containing product is subsequently exposed to leaching by introducing the product to a leaching vessel comprising an aqueous leach liquor.
  • the leach process preferably uses water with a natural pH, ie no requirement for any pH adjustment.
  • the aqueous leach liquor leaches the calcined lithium sulphate containing product.
  • the leaching step may be carried out at a temperatures between 20°C and 90°C to produce a lithium-enriched pregnant leach liquor.
  • Heating of the stirred leach vessel may be achieved by baffled coils, immersion heaters, a jacketed tank system or from residual heat from the calcination step.
  • the leach vessel may be agitated and the reaction may be left running for between 0.1 and 24hrs to reach the desired recovery of Li into the leach solution.
  • the leach reaction may be carried out continuously or batch-wise.
  • the leaching step is preferably done over a period of time between lh and 4h, at temperatures of up to 90°C and at less than 20% solids m/m. It is however to be understood that the leaching step may be carried out over any suitable time period, such as for example over a time period as short as 10 minutes, or over a time period as long as 24 hours.
  • the resultant lithium enriched pregnant leach liquor may contain between 0.1 and 45 g/litre, preferably between 5g/litre and 45g/litre of Li.
  • the leached, calcined mixture is filtered. Filtration may occur using any suitable means, including for example pressure filtration and vacuum filtration.
  • the filtrate is a lithium enriched pregnant leach liquor which is collected and used for further processing.
  • the solid leach residue can be disposed of or used for further processing.
  • lithium recovery using the feed mixture of the present invention without any additional milling or grinding, at temperatures of above 900 °C provide for comparable lithium recovery rates (with residence times of between 30 minutes and 50 minutes) to results achieved using milled or ground feed mixture.
  • Pulp density can be an important consideration of hydrometallurgical separation. Water evaporation has the highest associated operational costs of the extraction and purification process.
  • Figure 5 shows a clear reduction in lithium recovery across the pulp densities of 10% to 30%. It is considered that as the residence time increases, the mica has continued to breakdown and release more potassium in the form of potassium sulphate. This increase in potassium sulphate may increase the saturation of the pregnant leach liquor, thereby reducing the solubility of lithium sulphate, maintaining a higher level of lithium in the residue and reducing the recovery.
  • lithium recovery was found to be similar to the lithium recovery achieved at a temperature of 1000 °C at 30 minutes.
  • Leaching time can influence the lithium recovery rate.
  • the results of leaching time on lithium recovery are shown in Figure 6. It can be seen that in general the longer the leaching time, the higher the lithium recovery. With an increased leaching time, the conglomerates of calcined material have longer to break apart, increasing the surface area and allowing a greater degree of dissolution of lithium sulphate.
  • the use of calcium sulphate (gypsum) in the calcining step was found to significantly reduce binding of the mica material/calcined mica material to the sides of the equipment. Furthermore, when using calcium sulphate, it was found that the feed mixture had greater mobility within the apparatus.
  • the use of calcium sulphate has also been found to promote conglomeration and pellitisation of the feed material. Conglomeration and pellitisation of the feed material helps to reduce loss of lithium material during extraction. For example, without conglomeration and pellitisation lithium material may be lost as dust during extraction. The conglomeration and pellitisation is thought to occur as a result of calcium sulphate absorbing moisture.
  • the process of the present may be carried out without requiring additional milling circuits whilst achieving high lithium recovery rates.
  • the process of the present invention reduces the number of process steps, in particular milling steps, and therefore reduces the risk of loss of lithium during extraction.
  • the number of steps of the process have been reduced therefore requiring less apparatus.
  • the associated process and operating costs, labour and energy consumption of the apparatus and the process of the present invention are therefore reduced whilst the lithium recovery has been improved compared to conventional lithium mica extraction processes.
  • the process and apparatus of the present invention provide for improved lithium recovery from lithium mica material, whilst also providing for significant associated energy, carbon, time and cost savings.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

La présente invention concerne un procédé de récupération de lithium à partir de lithium mica, le procédé consistant à : mélanger le lithium mica avec du gypse et du carbonate de calcium (CaCO3) pour fournir un mélange de sel concentré de lithium mica ; et calciner du mélange de sel de lithium mica à une température prédéterminée pendant un temps prédéterminé pour fournir un produit contenant du sulfate de lithium calciné.
PCT/EP2022/068230 2021-07-02 2022-07-01 Extraction de lithium mica WO2023275346A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB2109646.6A GB2608461A (en) 2021-07-02 2021-07-02 Process for extraction of lithium from lithium-micas by calcination without pH adjustment
GB2109646.6 2021-07-02

Publications (2)

Publication Number Publication Date
WO2023275346A2 true WO2023275346A2 (fr) 2023-01-05
WO2023275346A3 WO2023275346A3 (fr) 2023-02-09

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2022/068230 WO2023275346A2 (fr) 2021-07-02 2022-07-01 Extraction de lithium mica

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GB (1) GB2608461A (fr)
WO (1) WO2023275346A2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116986836A (zh) * 2023-08-04 2023-11-03 江西永兴特钢新能源科技有限公司 一种锂云母渣除杂改性的方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB409636A (en) * 1932-12-29 1934-05-03 Metallgesellschaft Ag Process for recovering the lithium contained in siliceous lithiumbearing minerals
GB530028A (en) * 1938-06-22 1940-12-03 Bolidens Gruv Ab Method of recovering lithium from minerals
CN108330298B (zh) * 2018-02-14 2020-08-25 中南大学 一种从多金属云母矿石中提取铷、铯、锂、钾的方法
CN110395751B (zh) * 2019-04-15 2022-01-28 江西南氏锂电新材料有限公司 一种从锂云母提取硫酸锂的方法
CN110396592B (zh) * 2019-06-28 2020-07-10 江西南氏锂电新材料有限公司 以锂矿石自燃为热源焙烧制锂盐的方法及焙烧装置
CN111778391A (zh) * 2020-07-10 2020-10-16 江西省丙戊天成环保科技有限公司 一种焙烧锂云母提锂的隧道窑制备工艺及其装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116986836A (zh) * 2023-08-04 2023-11-03 江西永兴特钢新能源科技有限公司 一种锂云母渣除杂改性的方法

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GB202109646D0 (en) 2021-08-18
GB2608461A (en) 2023-01-04
WO2023275346A3 (fr) 2023-02-09

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