RU2019101553A - METHOD FOR PRODUCING HIGH PURITY LITHIUM HYDROXIDE MONOHYDRATE FROM MATERIALS CONTAINING LITHIUM CARBONATE OR LITHIUM CHLORIDE - Google Patents

METHOD FOR PRODUCING HIGH PURITY LITHIUM HYDROXIDE MONOHYDRATE FROM MATERIALS CONTAINING LITHIUM CARBONATE OR LITHIUM CHLORIDE Download PDF

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RU2019101553A
RU2019101553A RU2019101553A RU2019101553A RU2019101553A RU 2019101553 A RU2019101553 A RU 2019101553A RU 2019101553 A RU2019101553 A RU 2019101553A RU 2019101553 A RU2019101553 A RU 2019101553A RU 2019101553 A RU2019101553 A RU 2019101553A
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solution
lithium
lithium chloride
chloride
membrane electrolysis
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RU2019101553A
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Russian (ru)
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RU2019101553A3 (en
RU2751710C2 (en
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Александр Дмитриевич Рябцев
Михаил Александрович Дудин
Денис Александрович Петров
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Акционерное общество "Ангарский электролизный химический комбинат"
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Priority to RU2019101553A priority Critical patent/RU2751710C2/en
Priority to PCT/RU2020/000145 priority patent/WO2020162796A2/en
Publication of RU2019101553A publication Critical patent/RU2019101553A/en
Publication of RU2019101553A3 publication Critical patent/RU2019101553A3/ru
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    • 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
    • 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
    • C25B1/01Products
    • C25B1/34Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Claims (5)

1. Способ получения моногидрата гидроксида лития высокой степени чистоты из материалов, содержащих карбонат лития либо хлорид лития, включающий приготовление раствора хлорида лития, очистку раствора хлорида лития от примесей кальция и магния, электрохимическую конверсию раствора хлорида лития в раствор гидроксида лития мембранным электролизом, упаривание раствора гидроксида лития и кристаллизацию моногидрата гидроксида лития, карбонизацию части раствора гидроксида лития (маточника) с получением карбоната лития и использованием его в технологическом процессе, улавливание и утилизацию анодного хлора, отличающийся тем, что раствор хлорида лития перед подачей на операцию электрохимической конверсии хлорида лития мембранным электролизом сначала очищают от сульфат-иона путем взаимодействия раствора хлорида лития с хлоридом бария и отделением образующейся твердой фазы от раствора хлорида лития фильтрацией, затем раствор хлорида лития очищают от кальция и магния переводом их в нерастворимые соединения с использованием в качестве реагента раствора гидроксида лития концентрацией 2,0-6,0 моль/л и отделением образующейся твердой фазы от раствора хлорида лития фильтрацией, затем раствор хлорида лития глубоко очищают от остаточного количества кальция и магния на ионообменной хелатообразующей смоле, содержащей группы иминодиуксуной кислоты, с последующей двух стадийной регенерацией отработанной смолы вначале обработкой раствором соляной кислоты концентрацией 1,0-4,0 моль/л затем обработкой раствором гидроксида лития концентрацией 1,0-3,0 моль/л, мембранный электролиз проводят при плотности тока 2-5 кА/м2, анолит, циркулирующий в анодном контуре мембранной электролизной установки, подкисляют соляной кислотой до значений рН=1-3, концентрацию хлорида лития в анолите поддерживают на уровне 50-300 г/л, концентрацию гидроксида лития в получаемом на операции электрохимической конверсии растворе поддерживают в пределах 40-80 г/л.1. A method of obtaining high purity lithium hydroxide monohydrate from materials containing lithium carbonate or lithium chloride, including the preparation of a solution of lithium chloride, purification of a solution of lithium chloride from impurities of calcium and magnesium, electrochemical conversion of a solution of lithium chloride into a solution of lithium hydroxide by membrane electrolysis, evaporation of the solution lithium hydroxide and crystallization of lithium hydroxide monohydrate, carbonization of a part of lithium hydroxide solution (mother liquor) to obtain lithium carbonate and use it in the technological process, capture and utilization of anodic chlorine, characterized in that the lithium chloride solution before feeding to the operation of electrochemical conversion of lithium chloride by membrane electrolysis first, it is purified from sulfate ion by interaction of a solution of lithium chloride with barium chloride and separation of the resulting solid phase from a solution of lithium chloride by filtration, then the solution of lithium chloride is purified from calcium and magnesium by converting them into insoluble unification using a lithium hydroxide solution with a concentration of 2.0-6.0 mol / l as a reagent and separating the resulting solid phase from the lithium chloride solution by filtration, then the lithium chloride solution is deeply purified from the residual amount of calcium and magnesium on an ion-exchange chelating resin containing groups iminodiaxic acid, followed by two-stage regeneration of the spent resin, first by treatment with a solution of hydrochloric acid with a concentration of 1.0-4.0 mol / l, then by treatment with a solution of lithium hydroxide with a concentration of 1.0-3.0 mol / l, membrane electrolysis is carried out at a current density of 2 -5 kA / m 2 , the anolyte circulating in the anode circuit of the membrane electrolysis unit is acidified with hydrochloric acid to pH = 1-3, the concentration of lithium chloride in the anolyte is maintained at 50-300 g / l, the concentration of lithium hydroxide in the resulting operation the electrochemical conversion of the solution is maintained in the range of 40-80 g / l. 2. Способ по п. 1, отличающийся тем, что приготовление раствора хлорида лития осуществляют путем прямого контакта материала, содержащего карбонат лития с соляной кислотой, получаемой путем улавливания хлора, образуемого на аноде в процессе электрохимической конверсии хлорида лития мембранным электролизом, раствором карбамида аммония.2. A method according to claim 1, characterized in that the preparation of a lithium chloride solution is carried out by direct contact of a material containing lithium carbonate with hydrochloric acid obtained by trapping chlorine formed at the anode in the process of electrochemical conversion of lithium chloride by membrane electrolysis, an ammonium carbamide solution. 3. Способ по п. 1, отличающийся тем, что приготовление раствора хлорида лития осуществляют путем прямого контакта материала, содержащего карбонат лития, с соляной кислотой, получаемой путем прямого взаимодействия водорода и хлора, образуемых в процессе электрохимической конверсии хлорида лития мембранным электролизом.3. A method according to claim 1, characterized in that the preparation of a lithium chloride solution is carried out by direct contact of a material containing lithium carbonate with hydrochloric acid obtained by direct interaction of hydrogen and chlorine formed during the electrochemical conversion of lithium chloride by membrane electrolysis. 4. Способ по п. 1, отличающийся тем, что приготовление раствора хлорида лития осуществляют путем прямого контакта материала, содержащего карбонат лития, с соляной кислотой, при этом хлор, образуемый на аноде в процессе электрохимической конверсии хлорида лития мембранным электролизом, улавливают гидродсидом натрия с получением раствора гипохлорита натрия.4. The method according to claim 1, characterized in that the preparation of the lithium chloride solution is carried out by direct contact of the material containing lithium carbonate with hydrochloric acid, while the chlorine formed at the anode during the electrochemical conversion of lithium chloride by membrane electrolysis is captured with sodium hydroxide with obtaining a sodium hypochlorite solution. 5. Способ по п. 1, отличающийся тем, что в качестве ионообменной хелатообразующей смолы, содержащей группы иминодиуксуной кислоты, используют смолу Lewatit ТР-208.5. The method according to claim 1, characterized in that Lewatit TP-208 resin is used as the ion-exchange chelating resin containing iminodiaxic acid groups.
RU2019101553A 2019-01-21 2019-01-21 Method for producing high-purity lithium hydroxide monohydrate from materials containing lithium carbonate or lithium chloride RU2751710C2 (en)

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RU2019101553A RU2751710C2 (en) 2019-01-21 2019-01-21 Method for producing high-purity lithium hydroxide monohydrate from materials containing lithium carbonate or lithium chloride
PCT/RU2020/000145 WO2020162796A2 (en) 2019-01-21 2020-03-18 Method for producing high-purity lithium hydroxide monohydrate

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112279279A (en) * 2020-10-26 2021-01-29 荆门市格林美新材料有限公司 Preparation method of battery-grade lithium hydroxide monohydrate
CN112881589A (en) * 2021-03-12 2021-06-01 江西云威新材料有限公司 Method for detecting carbonate ion content in lithium hydroxide monohydrate
CN114590826A (en) * 2022-04-18 2022-06-07 四川兴晟锂业有限责任公司 Treatment process and equipment for potassium-rich mother liquor of lithium hydroxide production system

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2021417988A1 (en) * 2021-01-05 2023-07-27 Sociedad Quimica Y Minera De Chile S.A. Method for the production of lithium hydroxide (lioh) directly from lithium chloride (lici), without the need for an intermediate production of lithium carbonate or similar

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US4036713A (en) * 1976-03-04 1977-07-19 Foote Mineral Company Process for the production of high purity lithium hydroxide
RU2186729C2 (en) * 2000-05-30 2002-08-10 Открытое акционерное общество "Новосибирский завод химконцентратов" Method of production of lithium chloride
RU2196735C1 (en) * 2001-07-20 2003-01-20 Закрытое акционерное общество "Экостар-Наутех" Process of extracting monohydrate of high-purity lithium hydroxide from materials containing lithium carbonate
US9049886B2 (en) * 2007-01-26 2015-06-09 Philip Morris Usa Inc. Methods and apparatus for the selective removal of constituents from aqueous tobacco extracts
EP2268851A4 (en) * 2008-04-22 2011-05-25 Chemetall Foote Corp Method of making high purity lithium hydroxide and hydrochloric acid
CA3172956A1 (en) * 2010-02-17 2011-08-25 Terralithium Llc Method of producing high purity lithium carbonate
RU2516538C2 (en) * 2012-02-17 2014-05-20 Закрытое акционерное общество (ЗАО) "Экостра-Наутех" Method of obtaining lithium concentrate from lithium-bearing natural brines and its processing
RU2656452C2 (en) * 2016-02-04 2018-06-05 Общество с ограниченной ответственностью "Экостар-Наутех" (ООО) "Экостар-Наутех" Method for obtaining lithium hydroxide monohydrate from alcohols and the plant for its implementation

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112279279A (en) * 2020-10-26 2021-01-29 荆门市格林美新材料有限公司 Preparation method of battery-grade lithium hydroxide monohydrate
CN112279279B (en) * 2020-10-26 2023-05-12 荆门市格林美新材料有限公司 Preparation method of battery grade lithium hydroxide monohydrate
CN112881589A (en) * 2021-03-12 2021-06-01 江西云威新材料有限公司 Method for detecting carbonate ion content in lithium hydroxide monohydrate
CN112881589B (en) * 2021-03-12 2023-04-07 江西云威新材料有限公司 Method for detecting carbonate ion content in lithium hydroxide monohydrate
CN114590826A (en) * 2022-04-18 2022-06-07 四川兴晟锂业有限责任公司 Treatment process and equipment for potassium-rich mother liquor of lithium hydroxide production system
CN114590826B (en) * 2022-04-18 2023-07-18 四川兴晟锂业有限责任公司 Treatment process and equipment for potassium-rich mother liquor of lithium hydroxide production system

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WO2020162796A9 (en) 2020-12-24
RU2019101553A3 (en) 2020-07-21
WO2020162796A2 (en) 2020-08-13
RU2751710C2 (en) 2021-07-16
WO2020162796A3 (en) 2020-10-22

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