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WO2025117493A1 - Récupération de sulfate intégrée et génération de sous-produit à valeur ajoutée dans des procédés hydrométallurgiques - Google Patents

Récupération de sulfate intégrée et génération de sous-produit à valeur ajoutée dans des procédés hydrométallurgiques Download PDF

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Publication number
WO2025117493A1
WO2025117493A1 PCT/US2024/057378 US2024057378W WO2025117493A1 WO 2025117493 A1 WO2025117493 A1 WO 2025117493A1 US 2024057378 W US2024057378 W US 2024057378W WO 2025117493 A1 WO2025117493 A1 WO 2025117493A1
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WO
WIPO (PCT)
Prior art keywords
sulfate
calcium
chelating agent
alkali metal
solution
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
PCT/US2024/057378
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English (en)
Inventor
Ghazaleh Nazari
Gomer ABRENICA
Jolina Pagulayan
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II VI Delaware Inc
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II VI Delaware Inc
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Filing date
Publication date
Application filed by II VI Delaware Inc filed Critical II VI Delaware Inc
Publication of WO2025117493A1 publication Critical patent/WO2025117493A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G53/84—Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Complex oxides containing nickel and at least one other metal element
    • C01G53/42—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
    • C01G53/44—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G53/82—Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
    • 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
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present disclosure relates to the recovery of sulfate as a value-added product from hydrometallurgical processes.
  • the methods described herein may be used in, for example, mining and metallurgy, precursor cathode active material (pCAM) production, and battery recycling processes.
  • pCAM precursor cathode active material
  • Na2SO4 IOH2O, Glauber’s salt is a by-product of many hydrometallurgical processes. While useful in certain applications, Na2SO4 has limited market value. Worldwide, Na2SO4 resources are expected to be sufficient to last hundreds of years at the present rate of world consumption. Consequently, the production of this salt leads to an excess supply, resulting in significant waste disposal challenges.
  • Gypsum calcium sulfate dihydrate
  • the process involves reacting a sulfate, such as lithium sulfate (Li2SO4) or Na2SC>4 with a calcium (Ca) source, such as calcium hydroxide (Ca(OH)2) or calcium oxide (CaO) in the presence of a chelating agent (also referred to herein interchangeably as a complexing agent).
  • a sulfate such as lithium sulfate (Li2SO4) or Na2SC>4
  • a calcium (Ca) source such as calcium hydroxide (Ca(OH)2) or calcium oxide (CaO)
  • a chelating agent also referred to herein interchangeably as a complexing agent
  • the processes described herein not only address environmental concerns associated with traditional by-products but also opens new avenues for revenue generation through the production of gypsum, positioning it as a valuable asset in the materials landscape.
  • Sodium hydroxide (NaOH) and/or lithium hydroxide (LiOH) may be regenerated and reused in the process.
  • the processes described herein may be employed in various hydrometallurgical processes such as, for example, mining and metallurgy, pCAM production, and battery recycling, and provide one or more of the following advantages.
  • calcium exists primarily as an ionic species (Ca 2+ ) in aqueous solution, thereby enhancing its reactivity with sulfate ions (SCO 2 ’).
  • the present inventors have achieved this by use of chelation/complexation.
  • chelation/complexation By forming stable complexes, the availability of Ca ions in solution is enhanced, thereby allowing for more effective interaction with sulfate ions and promoting the formation of gypsum.
  • Chelating agents also help maintain calcium in a soluble form, thereby increasing the overall efficiency of the reaction and ensuring optimal conditions for gypsum precipitation.
  • the present disclosure relates to a method of converting an alkali metal sulfate to calcium sulfate, the method including: reacting an aqueous solution of the alkali metal sulfate with an aqueous solution of a Ca source in the presence of a chelating agent.
  • the present disclosure relates to a method of converting an alkali metal sulfate generated during a hydrometallurgical process (such as, but not limited to, pCAM production) to calcium sulfate, the method including:
  • the method further includes:
  • the present disclosure relates to a method of recovering sulfate produced in a hydrometallurgical process (such as, but not limited to, pCAM production) in the form of calcium sulfate, the process including:
  • the Ca source is calcium hydroxide (Ca(OH)2), calcium oxide (CaO), or a combination thereof.
  • the alkali metal hydroxide and/or the residual chelating agent is recovered by gravity separation, centrifugation, electrodialysis, nanofiltration, and/or reverse osmosis.
  • the method is conducted at a temperature of between about 20° C and about 90° C, such as between about 30° C and about 70° C, or between about 40° C and about 60° C.
  • the chelating agent is selected from the group consisting of diols, triols, polyols, monosaccharides, disaccharides, metaphosphates, and any combination of any of the foregoing.
  • Suitable diols include, but are not limited to, glycols, such as, e.g., ethylene glycol, propylene glycol, 1,3 -butanediol, 1,4- butanediol, and any combination thereof.
  • Suitable triols include, but are not limited to, glycerol.
  • Suitable polyols include, but are not limited to, sorbitol (e.g., D-sorbitol), mannitol (e.g., D-mannitol), galactitol (e.g., D-galactitol), glucitol, xylitol, and any combination thereof.
  • Suitable monosaccharides include, but are not limited to, glucose, fructose, galactose, and any combination thereof.
  • Suitable disaccharides include, but are not limited to, sucrose, lactose, maltose, and trehalose, and any combination thereof.
  • Suitable metaphosphates include, but are not limited to, sodium trimetaphosphate, sodium hexametaphosphate, sodium-potassium hexametaphosphate, potassium metaphosphate, and any combination thereof.
  • the concentration (aqueous concentration) of the chelating agent is between about 10 wt.% and about 90 wt.%, such as between about 20 wt.% and about 80 wt.%, between about 30 wt.% and about 70 wt.%, or between about 40 wt.% and about 60 wt.% by weight.
  • the concentration (aqueous concentration) of the chelating agent is about 10 wt.%, about 15 wt.%, about 20 wt.%, about 25 wt.%, about 30 wt.%, about 35 wt.%, about 40 wt.%, about 45 wt.%, about 50 wt.%, about 55 wt.% or about 60 wt.%.
  • the chelating agent forms a complex with the calcium ions (Ca 2+ ) in the solution, (ii) enhances solubility of calcium ions (Ca 21 ) in the solution, and/or (iii) enhances interaction of calcium ions (Ca 21 ) in the solution with sulfate (SC>4 2 ') ions in the solution.
  • FIG. 1 is an exemplary process flow diagram showing a process for recovering sulfate from an effluent containing an alkali metal sulfate as anhydrous sodium sulfate, performed in accordance with current industry practice.
  • FIG. 2 is an exemplary process flow diagram showing a process for recovering sulfate from an effluent containing an alkali metal sulfate as calcium sulfate (gypsum), according to one aspect as described herein. It will be understood that the process shown in FIG. 2 is only illustrative and is non-limiting. Additional process steps to those shown may be added (or removed) as required.
  • the conversion of Na SO4 (or I 2SO4) to gypsum can be accomplished by reacting it with, for example, calcium chloride (CaCh) (Eq. 1) or calcium nitrate (Ca(NOa)2) (Eq. 2). Owing to their high solubility of about 74.5 g and 121 g in 100 mL water at 20° C, respectively, these reagents can easily react with Na2SO4 to produce calcium sulfate.
  • CaCh calcium chloride
  • Ca(NOa)2 calcium nitrate
  • U.S. Patent No. 8,273,181 describes a process of removing calcium and obtaining sulfate salts from an aqueous sugar solution.
  • Bouzouaid et.al., Cement and Concrete Research, 149(2-3), 106563, 2021 describes the solubility of portlandite in the presence of gluconate, D- sorbitol, D-mannitol and D-galactitol.
  • the term “about” means an acceptable error for a particular value as determined by one of ordinary skill in the art, which depends in part on how the value is measured or determined. In certain aspects, the term “about” means within 1, 2, 3, or 4 standard deviations. In certain aspects, the term “about” means within 15%, 10%, 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2%, 1%, 0.5%, or 0.05% of a given value or range.
  • the term “comprising” includes, but is not limited to, those embodiments, for example, an embodiment of any composition of matter, composition, method, or process, or the like, that “consist of’ or “consist essentially of’ the described features.
  • the approximating language may correspond to the precision of an instrument for measuring the value.
  • the modifier “about” should also be considered as disclosing the range defined by the absolute values of the two endpoints.
  • the expression “from about 2 to about 4” also discloses the range “from 2 to 4.”
  • the term “about” may refer to plus or minus 10% of the indicated number.
  • “about 10%” may indicate a range of “9 to 11,” and “about 1” may mean from “0.9-1.1.”
  • Other meanings of “about” may be apparent from the context, such as rounding off, so, for example “about 1” may also mean from “0.5 to 1.4.”
  • FIG. 1 is an exemplary process flow diagram showing a process for recovering sulfate from an effluent containing an alkali metal sulfate as anhydrous sodium sulfate, performed in accordance with current industry practice.
  • the current industry practice process of FIG.1 involves providing effluent containing alkali metal sulfates (10). The effluent then undergoes cooling crystallization (S100). The resulting product is then isolated by filtration and washed (S200) to produce Glauber’s salt (NazSCfi- IOH2O) (20). For a process directed to lithium battery (LiB) recycling, a Li recovery process may be performed (S300). The Glauber’s salt (20) is then dissolved (S400) in water and the solution is then subjected to evaporative crystallization (S500). The resulting solid is isolated by filtration (S600) and the sodium sulfate is dried (S700) to product anhydrous sodium sulfate (30).
  • FIG. 2 is an exemplary process flow diagram showing a process for recovering sulfate from an effluent containing an alkali metal sulfate as calcium sulfate (gypsum), according to one non-limiting aspect as described herein.
  • the non-limiting process of FIG. 2 involves providing effluent containing alkali metal sulfates (11).
  • a solution containing a Ca source (such as Ca(OH)2) or CaO) and a chelating agent (21) is added and a solid is formed by precipitation (S101).
  • the solid is isolated by filtration and washed (S201) to form wet gypsum (31).
  • the filtrate which is a basic solution containing alkali metal hydroxide and/or the residual chelating agent may be recovered and reused (S301).
  • the wet gypsum (31) is dried (S401) to afford dry gypsum (41).
  • Example 2 a substantial amount of Ca remains unprecipitated. Owing to the alkalinity of the system and knowing that Ca(OH)2 has very poor solubility in water, it was theorized that the residual Ca was still in sucrate form. To test this theory, additional Na2SO4 was added to the solution. After 1 hour of reaction time at 25 0 C, the slurry was filtered using a Whatman 41 filter paper fitted in a Buchner funnel via vacuum filtration. The filtrate was analyzed for Ca, Na and S using ICP-OES. The results are shown in Table 3.
  • the resulting filtrate after filtering off the gypsum may be processed via known and suitable methods such as, but not limited to, gravity separation, centrifugation, electrodialysis, nanofiltration, or reverse osmosis to preferentially recover the sucrose solution and alkali hydroxide solution separately for reuse and recycling.
  • the slurry is then filtered, washed, and dried to produce the gypsum by-product.
  • Ca is then removed from the solution containing residual Ca, NaOH or LiOH, and chelating agent using a process such as, but not limited to, ion exchange and chemical precipitation, prior to separation and recovery of the chelating agent and alkali hydroxides for reuse and recycling.
  • the chelating agent and/or alkali hydroxides are recovered by, for example, gravity separation, centrifugation, electrodialysis, nanofiltration, or reverse osmosis.

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

Abstract

La présente invention concerne un procédé amélioré pour la récupération de sulfate dans des procédés hydrométallurgiques. Selon un aspect, le procédé consiste à faire réagir un sulfate, tel que du sulfate de lithium (Li2SO4) ou du Na2SO4 avec une source de calcium (Ca), telle que l'hydroxyde de calcium (Ca(OH)2) ou l'oxyde de calcium (CaO) en présence d'un agent chélatant. Les procédés décrits ici peuvent être utilisés par exemple dans l'exploitation minière et la métallurgie, la production de matériau actif de cathode précurseur (pCAM) et le recyclage de batterie.
PCT/US2024/057378 2023-11-28 2024-11-26 Récupération de sulfate intégrée et génération de sous-produit à valeur ajoutée dans des procédés hydrométallurgiques Pending WO2025117493A1 (fr)

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PCT/US2024/057378 Pending WO2025117493A1 (fr) 2023-11-28 2024-11-26 Récupération de sulfate intégrée et génération de sous-produit à valeur ajoutée dans des procédés hydrométallurgiques

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111807414A (zh) * 2020-06-18 2020-10-23 贵州金瑞新材料有限责任公司 一种利用碱式盐法生产无氟超纯一水硫酸锰的方法
CN115537551A (zh) * 2022-10-13 2022-12-30 四川长虹格润环保科技股份有限公司 一种从废旧锂电池正极材料中优先提锂、锰的方法
US20230383377A1 (en) * 2022-05-27 2023-11-30 Ii-Vi Delaware, Inc. Hydrometallurgical process for lithium-ion battery waste recycling

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KR101913906B1 (ko) * 2015-06-17 2018-10-31 주식회사 엘지화학 이차전지용 양극활물질, 이의 제조방법 및 이를 포함하는 이차전지
JP7194185B2 (ja) * 2017-11-22 2022-12-21 ネマスカ リチウム インコーポレーテッド 様々な金属の水酸化物および酸化物ならびにそれらの誘導体の調製プロセス
CN109980219B (zh) * 2019-04-19 2020-12-04 中南大学 全梯度镍钴锰正极材料、氧化钌包覆材料及其制备方法

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CN111807414A (zh) * 2020-06-18 2020-10-23 贵州金瑞新材料有限责任公司 一种利用碱式盐法生产无氟超纯一水硫酸锰的方法
US20230383377A1 (en) * 2022-05-27 2023-11-30 Ii-Vi Delaware, Inc. Hydrometallurgical process for lithium-ion battery waste recycling
CN115537551A (zh) * 2022-10-13 2022-12-30 四川长虹格润环保科技股份有限公司 一种从废旧锂电池正极材料中优先提锂、锰的方法

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ZIEGENHEIM SZILVESZTER, SZTEGURA ALEX, SZABADOS MáRTON, KóNYA ZOLTáN, KUKOVECZ ÁKOS, PáLINKó ISTVáN, SIPOS PáL: "EDTA analogues – unconventional inhibitors of gypsum precipitation", JOURNAL OF MOLECULAR STRUCTURE, ELSEVIER AMSTERDAM, NL, vol. 1256, 1 May 2022 (2022-05-01), NL , pages 132491, XP093333738, ISSN: 0022-2860, DOI: 10.1016/j.molstruc.2022.132491 *

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