PL448069A1 - Method for obtaining high-purity lithium rhenate(VII) from solutions obtained from the processing of Li-ion batteries - Google Patents

Method for obtaining high-purity lithium rhenate(VII) from solutions obtained from the processing of Li-ion batteries

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Publication number
PL448069A1
PL448069A1 PL448069A PL44806924A PL448069A1 PL 448069 A1 PL448069 A1 PL 448069A1 PL 448069 A PL448069 A PL 448069A PL 44806924 A PL44806924 A PL 44806924A PL 448069 A1 PL448069 A1 PL 448069A1
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PL
Poland
Prior art keywords
lithium carbonate
solution
lithium
vii
precipitate
Prior art date
Application number
PL448069A
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Polish (pl)
Other versions
PL249110B1 (en
Inventor
Katarzyna Leszczyńska-Sejda
Arkadiusz Palmowski
Grzegorz Benke
Michał Ochmański
Dorota Kopyto
Alicja Grzybek
Original Assignee
Sieć Badawcza Łukasiewicz - Instytut Metali Nieżelaznych
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.)
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Publication date
Application filed by Sieć Badawcza Łukasiewicz - Instytut Metali Nieżelaznych filed Critical Sieć Badawcza Łukasiewicz - Instytut Metali Nieżelaznych
Priority to PL448069A priority Critical patent/PL249110B1/en
Publication of PL448069A1 publication Critical patent/PL448069A1/en
Publication of PL249110B1 publication Critical patent/PL249110B1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G47/00—Compounds of rhenium
    • 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
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Przedmiotem zgłoszenia jest sposób wytwarzania wysokiej czystości renianu(VII) litu poprzez reakcję węglanu litu i kwasu renowego(VII), w wyniku której uzyskuje się roztwór, który kolejno odparowuje się, a wydzielony osad suszy dla uzyskania renianu(VII) litu, który charakteryzuje się tym, że węglan litu strąca się z wodnych wieloskładnikowych roztworów powstających przy przerobie złomu baterii Li-ion, o pH 1 - 6, które powstają z hydrometalurgicznego przerobu masy bateryjnej Li-ion, a zawierają minimum 2,0 g/dm3 Li, poprzez dodanie wodnego roztworu węglanu sodu, o stężeniu powyżej 200 g/dm3, stosując 5% - 20% nadmiar węglanu sodu liczony na ilość stechiometryczną Li w roztworze, a strącanie prowadzi się w temperaturze powyżej 90°C, ciągle mieszając ze stałą prędkością dozowania roztworu Na2CO3, mieszczącą się w zakresie 2 - 20 cm3/min, po procesie dozowania uzyskany osad surowego węglanu litu oddziela się w temperaturze >90°C przez filtrację i przemywa na filtrze wodą, w temperaturze >90°C, w ilości 200 - 500 cm3 na każde 100 g wytrąconego osadu węglanu litu, a powstałe popłuczyny wodne zawraca się do etapu strącania węglanu litu, tak aby stężenie litu w roztworze wynosiło ≥2,0 g/dm3 i kolejno wytrącony osad węglanu litu przemywa obiegową mieszaniną etanolowo-izopropanolową w ilości 100-500 cm3 na każde 100 g wytrąconego osadu węglanu litu i kolejno węglan litu kieruje się do cyklicznego oczyszczania, gdzie węglan litu rozpuszcza się w wodzie stosując na każde 100 g tego związku 0,5 - 1,5 dm3 wody, dodając w sposób ciągły gazowe CO2, ze stałą prędkością wynoszącą minimum 1,0 dm3/minutę, minimum przez 30 minut, tak powstały roztwór oddziela się przez filtrację od nierozpuszczalnej pozostałości zanieczyszczeń, którą kieruje się do etapu strącania węglanu litu, a następnie odfiltrowany roztwór podgrzewa się do temperatury 90°C - 95°C i miesza przez minimum 1 h, po czym powstały osad węglanu litu oddziela się od roztworu z zastosowaniem filtracji w temperaturze >90°C i zawraca do kolejnego cyklu oczyszczania węglanu litu, które to oczyszczanie prowadzi się w sposób cykliczny z zawrotem oczyszczanego węglanu litu, stosując od 1 do 4 cykli, a powstały po cyklicznym oczyszczaniu węglan litu przemywa się bezwodną mieszaniną etanolowo-izopropanolową w stosunku od 1:1 do 1:3, w ilości minimum 150 cm3 na każde 100 g wytrąconego osadu węglanu litu, po czym roztwory powstałe z oczyszczania węglanu litu łączy się, a powstały osad oczyszczonego węglanu litu dodaje się porcjami, z szybkością ≤30 g/min, do wodnego roztworu kwasu renowego(VII) zawierającego do 900 g/dm3 Re, do momentu neutralizacji kwasu, czyli osiągnięcia pH na poziomie 7,0 - 9,5, dozowanie prowadzi się w temperaturze pokojowej, a zneutralizowany roztwór filtruje się i odparowuje się do sucha w temperaturze nieprzekraczającej 60°C, z dodatkiem 0 - 15 cm3 30% wodnego roztworu H2O2 na każde 200 g Re, uzyskując mieszaninę hydratów renianu(VII) litu, którą przemywa się wodą, w temperaturze pokojowej, w ilości minimum 50 cm3 i kolejno bezwodnym etanolem, w ilości minimum 50 cm3, na każde 100 g oczyszczanej mieszaniny hydratów renianu(VII) litu, po czym przemytą mieszaninę suszy się w zakresie temperatury 110°C - 180°C, przez 2 - 8 h, uzyskując w ten sposób renian(VII) litu, który zawiera od 2,35% do 2,68% Li i zarazem od 63,53% do 72,42% oraz do 1000 ppm sumy zanieczyszczeń metalicznych.The subject of the application is a method for producing high-purity lithium rhenate (VII) by reacting lithium carbonate and rhenic acid (VII), as a result of which a solution is obtained, which is subsequently evaporated and the separated precipitate is dried to obtain lithium rhenate (VII), which is characterized in that lithium carbonate is precipitated from aqueous multi-component solutions formed during the processing of Li-ion battery scrap, with a pH of 1 - 6, which are formed during the hydrometallurgical processing of Li-ion battery mass and contain a minimum of 2.0 g/dm3 of Li, by adding an aqueous sodium carbonate solution with a concentration above 200 g/dm3, using a 5% - 20% excess of sodium carbonate calculated on the stoichiometric amount of Li in the solution, and the precipitation is carried out at a temperature above 90°C, with continuous stirring at a constant rate of dosing the Na2CO3 solution, in the range of 2 - 20 cm3/min, after the dosing process the obtained precipitate of crude lithium carbonate is separated at a temperature of >90°C by filtration and washed on the filter with water at a temperature of >90°C, in the amount of 200 - 500 cm3 for every 100 g of precipitated lithium carbonate precipitate, and the resulting water washings are returned to the stage of precipitation of lithium carbonate, so that the concentration of lithium in the solution is ≥2.0 g/dm3 and then the precipitated lithium carbonate precipitate is washed with a circulating ethanol-isopropanol mixture in the amount of 100-500 cm3 for every 100 g of precipitated lithium carbonate precipitate and then the lithium carbonate is sent to cyclic purification, where lithium carbonate is dissolved in water using 0.5 - 1.5 dm3 of water for every 100 g of this compound, continuously adding gaseous CO2, at a constant rate of at least 1.0 dm3/minute, for at least 30 minutes minutes, the solution thus obtained is separated by filtration from the insoluble residue of impurities, which is directed to the stage of precipitation of lithium carbonate, and then the filtered solution is heated to a temperature of 90°C - 95°C and stirred for a minimum of 1 h, after which the resulting lithium carbonate precipitate is separated from the solution by filtration at a temperature of >90°C and returned to the next cycle of lithium carbonate purification, which is carried out in a cyclic manner with the return of the purified lithium carbonate, using from 1 to 4 cycles, and the lithium carbonate formed after the cyclic purification is washed with an anhydrous ethanol-isopropanol mixture in a ratio of 1:1 to 1:3, in the amount of at least 150 cm3 for every 100 g of the precipitated lithium carbonate precipitate, after which the solutions resulting from the purification of lithium carbonate are combined, and the resulting precipitate of purified lithium carbonate is added in portions, at a rate of ≤30 g/min, to the aqueous solution of lithium carbonate rhenium(VII) containing up to 900 g/dm3 of Re, until the acid is neutralized, i.e. pH is reached at 7.0 - 9.5, dosing is carried out at room temperature, and the neutralized solution is filtered and evaporated to dryness at a temperature not exceeding 60°C, with the addition of 0 - 15 cm3 of 30% aqueous H2O2 solution for each 200 g of Re, obtaining a mixture of lithium rhenate(VII) hydrates, which is washed with water at room temperature, in the amount of at least 50 cm3 and subsequently with anhydrous ethanol, in the amount of at least 50 cm3, for each 100 g of purified mixture of lithium rhenate(VII) hydrates, after which the washed mixture is dried in the temperature range of 110°C - 180°C, for 2 - 8 h, thus obtaining lithium rhenate(VII), which contains from 2.35% to 2.68% Li and at the same time from 63.53% to 72.42% and up to 1000 ppm of total metallic impurities.

PL448069A 2024-03-21 2024-03-21 Method for obtaining high-purity lithium rhenate(VII) from solutions obtained from the processing of Li-ion batteries PL249110B1 (en)

Priority Applications (1)

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PL448069A1 true PL448069A1 (en) 2025-09-22
PL249110B1 PL249110B1 (en) 2026-03-02

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Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
ABAKUMOV A.M. ET AL.: "Solid State Sci. 2001, 3(5), 581–586 doi: 10.1016/S1293-2558(01)01168-2", "SYNTHESIS AND CRYSTAL STRUCTURE OF THE LITHIUM PERRHENATE MONOHYDRATE LIREO4·H2O." *
BURKERT P.K. ET AL.: "Z. Naturforsch. B 1976, 31(2), 145–148 doi: 10.1515/znb-1976-0201", "SPECTROSCOPIC INVESTIGATIONS IN THE SOLID STATE CHEMISTRY, X RE-NQR INVESTIGATIONS ON TLREO4 AND LIREO4*2H2O." *
ULBRICHT K. ET AL.: "Z. Anorg. Und Allg. Chem. 1968, 358(5-6), 193–304 doi: 10.1002/zaac.19683580502", "SPEKTROSKOPISCHE UNTERSUCHUNGEN AN EINIGEN WASSERFREIEN PERRHENATEN." *

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