HRP20211184T1 - Postupci za tretiranje vodenih sastava koji sadrže litij sulfat i sumpornu kiselinu - Google Patents

Postupci za tretiranje vodenih sastava koji sadrže litij sulfat i sumpornu kiselinu Download PDF

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Publication number
HRP20211184T1
HRP20211184T1 HRP20211184TT HRP20211184T HRP20211184T1 HR P20211184 T1 HRP20211184 T1 HR P20211184T1 HR P20211184T T HRP20211184T T HR P20211184TT HR P20211184 T HRP20211184 T HR P20211184T HR P20211184 T1 HRP20211184 T1 HR P20211184T1
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HR
Croatia
Prior art keywords
lithium sulfate
sulfuric acid
solution
kpa
process according
Prior art date
Application number
HRP20211184TT
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English (en)
Inventor
Jean-François Magnan
Guy BOURASSA
Nicolas Laroche
Bertin OUELLET
Clive Richmond Brereton
Steven BUCHI
Tsuki NAKA
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Nemaska Lithium Inc.
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Application filed by Nemaska Lithium Inc. filed Critical Nemaska Lithium Inc.
Publication of HRP20211184T1 publication Critical patent/HRP20211184T1/hr

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0022Evaporation of components of the mixture to be separated by reducing pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00Lithium compounds
    • C01D15/06Sulfates; Sulfites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • B01D9/0013Crystallisation cooling by heat exchange by indirect heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0059General arrangements of crystallisation plant, e.g. flow sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0077Screening for crystallisation conditions or for crystal forms
    • 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
    • C25B1/14Alkali metal compounds
    • C25B1/16Hydroxides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/46Sulfur-, selenium- or tellurium-containing compounds
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/02Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
    • C30B7/04Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Metallurgy (AREA)
  • Electrochemistry (AREA)
  • Secondary Cells (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
  • Removal Of Specific Substances (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Claims (13)

1. Postupak za tretiranje vodenih sastava koji sadrže litij sulfat i sumpornu kiselinu, pri čemu navedeni postupak sadrži: kristalizaciju uparavanjem vodenih sastava koji sadrže litij sulfat i sumpornu kiselinu, pod uvjetima za dobivanje kristala litij sulfat monohidrata i otopine reduciranog sadržaja litij sulfata, i za inhibiranje razlaganja navedenih kristala litij sulfat monohidrata u bezvodni litij sulfat, po izboru, razdvajanje kristala litij sulfat monohidrata od otopine reduciranog sadržaja litij sulfata, naznačen time, što se kristalizacija uparavanjem provodi na temperaturi od 40°C do 95 °C i pod tlakom od 1 kPa do 75 kPa.
2. Postupak sukladno patentnom zahtjevu 1, pri čemu vodeni sastav koja sadrži litij sulfat i sumpornu kiselinu sadrži od 1 tež.% do 35 tež.% litij sulfata u odnosu na ukupnu težinu vodenog sastava.
3. Postupak sukladno patentnom zahtjevu 1 ili 2, pri čemu vodeni sastav koji sadrži litij sulfat i sumpornu kiselinu sadrži od 7 tež.% do 15 tež.% sumporne kiseline u odnosu na ukupnu težinu vodenog sastava.
4. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 3, pri čemu vodeni sastav koji sadrži litij sulfat i sumpornu kiselinu nadalje sadrži natrij sulfat i/ili kalij sulfat u količini do 10 tež.% u odnosu na ukupnu težinu vodenog sastava.
5. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 4, gdje se kristalizacija uparavanjem provodi na temperaturi od 75°C do 85°C.
6. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 5, gdje se kristalizacija uparavanjem provodi pod tlakom od 15 kPa do 20 kPa.
7. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 5, gdje se kristalizacija uparavanjem provodi pod tlakom od 5 kPa do 15 kPa.
8. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 7, gdje uvjeti za dobivanje kristala litij sulfat monohidrata i otopine reduciranog sadržaja litij sulfata nadalje sadrže kristalizaciju uparavanjem vodenog sastava koji sadrži litij sulfat i sumpornu kiselinu tokom vremena u kojem otopina reduciranog sadržaja litij sulfata sadrži koncentraciju sumporne kiseline koja je manja od 65 tež.% u odnosu na ukupnu težinu otopine reduciranog sadržaja litij sulfata.
9. Postupak sukladno patentnom zahtjevu 8, gdje se kristalizacija uparavanjem provodi dok otopina reduciranog sadržaja litij sulfata sadrži koncentraciju sumporne kiseline od 40 tež.% do 50 tež.% u odnosu na ukupnu težinu otopine reduciranog sadržaja litij sulfata.
10. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 9, pri čemu postupak sadrži: odvajanje kristala litij sulfat monohidrata od otopine reduciranog sadržaja litij sulfata, hlađenje otopine reduciranog sadržaja litij sulfata pod uvjetima za dobivanje dodatnog dijela kristala litij sulfat monohidrata i otopine dodatno reduciranog sadržaja litij sulfata koji sadrži sumpornu kiselinu; i razdvajanje kristala litij sulfat monohidrata od otopine dodatno reduciranog sadržaja litij sulfata koji sadrži sumpornu kiselinu, pri čemu se hlađenje provodi na temperaturi od 15°C do 80°C, pod tlakom od 1 kPa do 100 kPa.
11. Postupak sukladno bilo kojem od patentnih zahtjeva od 1 do 10, pri čemu postupak nadalje sadrži koncentriranje otopine reduciranog sadržaja litij sulfata pod uvjetima za dobivanje kiselog kondenzata i koncentrata koji sadrži sumpornu kiselinu, pri čemu navedeni koncentrat sadrži ukupnu koncentraciju sumporne kiseline, litij sulfata i po izboru natrij sulfata koja je veća od 65 tež.% u odnosu na ukupnu težinu koncentrata.
12. Postupak sukladno patentnom zahtjevu 11, gdje se koncentriranje provodi na temperaturi od 170°C do 200°C.
13. Postupak sukladno patentnom zahtjevu 11 ili 12, pri čemu postupak nadalje sadrži: hlađenje koncentrata koji sadrži sumpornu kiselinu pod uvjetima pri čemu navedeni uvjeti sadrže hlađenje koncentrata do temperature od 5°C do 170°C pod tlakom koji je od 1 kPa do 100 kPa ili od 95 do 105 kPa, da bi se dobila dodatni dio kristala litij sulfat monohidrata i koncentrata reduciranog sadržaja litij sulfata koji sadrži sumpornu kiselinu; i razdvajanje kristala od dodatnog dijela litij sulfat monohidrata od koncentrata reduciranog sadržaja litij sulfata koji sadrži sumpornu kiselinu.
HRP20211184TT 2016-08-26 2021-07-22 Postupci za tretiranje vodenih sastava koji sadrže litij sulfat i sumpornu kiselinu HRP20211184T1 (hr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US201662380056P 2016-08-26 2016-08-26
CA2940509A CA2940509A1 (en) 2016-08-26 2016-08-26 Processes for treating aqueous compositions comprising lithium sulfate and sulfuric acid
PCT/CA2017/051007 WO2018035618A1 (en) 2016-08-26 2017-08-28 Processes for treating aqueous compositions comprising lithium sulfate and sulfuric acid
EP17842498.2A EP3504360B1 (en) 2016-08-26 2017-08-28 Processes for treating aqueous compositions comprising lithium sulfate and sulfuric acid

Publications (1)

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HRP20211184T1 true HRP20211184T1 (hr) 2021-10-15

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Country Link
US (2) US11083978B2 (hr)
EP (1) EP3504360B1 (hr)
JP (1) JP6825082B2 (hr)
KR (1) KR102266697B1 (hr)
CN (2) CN113149040A (hr)
AU (2) AU2017315337B2 (hr)
CA (4) CA2940509A1 (hr)
CL (1) CL2019000483A1 (hr)
DK (1) DK3504360T3 (hr)
ES (1) ES2882337T3 (hr)
HR (1) HRP20211184T1 (hr)
PL (1) PL3504360T3 (hr)
PT (1) PT3504360T (hr)
RS (1) RS62169B1 (hr)
WO (1) WO2018035618A1 (hr)

Families Citing this family (8)

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JP6335316B2 (ja) 2013-10-23 2018-05-30 ネマスカ リチウム インコーポレイテッド 炭酸リチウムの調製のためのプロセス
KR102153976B1 (ko) 2014-02-24 2020-09-10 네마스카 리튬 인코포레이션 리튬 함유 물질을 처리하기 위한 방법
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