JP6889115B2 - HClスパージを行うことを含むリチウム含有材料の処理 - Google Patents
HClスパージを行うことを含むリチウム含有材料の処理 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims description 17
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 95
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 76
- 239000000243 solution Substances 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 68
- 230000008569 process Effects 0.000 claims description 64
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 60
- 238000002386 leaching Methods 0.000 claims description 44
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims description 29
- 239000012535 impurity Substances 0.000 claims description 24
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 23
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 23
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 22
- 229910052744 lithium Inorganic materials 0.000 claims description 21
- 229910052643 α-spodumene Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052644 β-spodumene Inorganic materials 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 11
- 239000012141 concentrate Substances 0.000 claims description 11
- 239000011591 potassium Substances 0.000 claims description 11
- 229910052700 potassium Inorganic materials 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 10
- 241001618883 Euphorbia uralensis Species 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- 238000005342 ion exchange Methods 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 8
- 238000005868 electrolysis reaction Methods 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 4
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 4
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 30
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 30
- 239000000047 product Substances 0.000 description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 10
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000001103 potassium chloride Substances 0.000 description 5
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 159000000002 lithium salts Chemical class 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000009283 thermal hydrolysis Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/04—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- 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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- 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
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
- C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
-
- 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
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- Manufacturing & Machinery (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Battery Electrode And Active Subsutance (AREA)
Description
(i)リチウム含有材料から処理溶液を調製するステップと、
(ii)ステップ(i)からの処理溶液を、HClスパージステップを含む一連の不純物除去ステップに通し、これにより実質的に精製された塩化リチウム溶液を供するステップと、
(iii)ステップ(ii)の精製された塩化リチウム溶液を電気分解ステップに通し、これにより水酸化リチウム溶液を得るステップとを備え、
処理溶液は、ステップ(ii)での一連の不純物除去ステップより前に、濃縮ステップで処理されないことを特徴とするプロセスを提供する。
Claims (25)
- α−リチア輝石鉱石又はα−リチア輝石鉱石濃縮物をか焼して得られるβ−リチア輝石と、リチウム含有鹹水とのいずれかであるリチウム含有材料を処理するプロセスにおいて、
(i)前記リチウム含有材料と塩酸とを用いて処理溶液を得るステップと、
(ii)ステップ(i)からの前記処理溶液に対して不純物除去を行って、実質的に精製された塩化リチウム溶液を供する不純物除去のためのマルチステップの工程であって、(A)多価カチオン不純物除去ステップと、(B)前記多価カチオン不純物除去ステップより後であってHClスパージステップを有する1価カチオン不純物除去ステップとを含むマルチステップの工程と、
(iii)ステップ(ii)の前記精製された塩化リチウム溶液を電気分解ステップに通し、これにより水酸化リチウム溶液を得るステップと、
(iv)前記HClスパージステップでの前記処理溶液から、HClを回収し、回収されたHClをステップ(i)にリサイクルするステップとを備え、
前記処理溶液は、ステップ(ii)での前記マルチステップの工程より前に、濃縮ステップで処理されないことを特徴とするプロセス。 - 請求項1記載のプロセスにおいて、さらに、前記電気分解ステップでの前記塩化リチウム溶液から、HClを回収し、回収されたHClをステップ(i)にリサイクルするステップを備えていることを特徴とするプロセス。
- 請求項1記載のプロセスにおいて、ステップ(iii)で得られた前記水酸化リチウム溶液は、圧縮された二酸化炭素を前記水酸化リチウム溶液に通すことで炭酸化され、これにより炭酸リチウム沈殿を製造することを特徴とするプロセス。
- 請求項1ないし3のいずれか1項に記載のプロセスにおいて、ステップ(i)の前記処理溶液は含浸浸出溶液であることを特徴とするプロセス。
- 請求項4記載のプロセスにおいて、リチウム含有材料を塩酸で浸出させる浸出ステップに前記リチウム含有材料を導入することにより、前記含浸浸出溶液が得られることを特徴とするプロセス。
- 請求項1ないし4のいずれか1項に記載のプロセスにおいて、さらに、前記α−リチア輝石鉱石、又は前記α−リチア輝石鉱石濃縮物をか焼して前記β−リチア輝石を得る第1ステップを備えていることを特徴とするプロセス。
- 請求項1ないし6のいずれか1項に記載のプロセスにおいて、前記HClスパージステップにより、存在するナトリウム及びカリウムが沈殿するようにHCl濃度が高まることを特徴とするプロセス。
- 請求項7記載のプロセスにおいて、前記処理溶液の前記HCl濃度は、少なくとも30重量%まで上昇されることを特徴とするプロセス。
- 請求項8記載のプロセスにおいて、前記処理溶液の前記HCl濃度は、少なくとも36重量%まで上昇されることを特徴とするプロセス。
- 請求項7ないし9のいずれか1項に記載のプロセスにおいて、前記HClスパージステップの後であって前記HClスパージステップからの回収する前記ステップの前に、沈殿した前記ナトリウム及びカリウムを除去するろ過ステップが行われることを特徴とするプロセス。
- 請求項10記載のプロセスにおいて、ナトリウム及びカリウムは、沈殿した塩の形態で沈殿されることを特徴とするプロセス。
- 請求項10又は11記載のプロセスにおいて、前記HClスパージステップからの回収する前記ステップは、蒸留の形態で行われることを特徴とするプロセス。
- 請求項1ないし12のいずれか1項に記載のプロセスにおいて、ステップ(iii)で得られた前記水酸化リチウム溶液は、水の蒸発によって高濃度化され、水酸化リチウム一水和物結晶が得られることを特徴とするプロセス。
- 請求項1ないし13のいずれか1項に記載のプロセスにおいて、ステップ(iii)で得られた前記水酸化リチウム溶液の第1部分は、蒸発/結晶化によって高濃度化され、水酸化リチウム一水和物結晶が得られ、前記水酸化リチウム溶液の第2部分は、圧縮された二酸化炭素を前記水酸化リチウム溶液に通すことで炭酸化され、これにより炭酸リチウム沈殿を製造することを特徴とするプロセス。
- 請求項1ないし14のいずれか1項に記載のプロセスにおいて、前記多価カチオン不純物除去ステップは、塩化アルミニウム及び塩化鉄の加水熱分解と、アルミニウム、鉄、マグネシウム及びマンガンの水酸化物を沈殿させるためにpHを上げることと、カルシウムの除去のための炭酸リチウムの沈殿とのうち、二つ以上を含むことを特徴とするプロセス。
- 請求項15記載のプロセスにおいて、前記マルチステップの工程は、さらに、前記HClスパージステップの後にイオン交換ステップを含むことを特徴とするプロセス。
- 請求項16記載のプロセスにおいて、前記イオン交換ステップでは、含浸浸出溶液中に残ったカルシウム、マグネシウムの多価カチオンを除去することを特徴とするプロセス。
- 請求項17記載のプロセスにおいて、前記多価カチオンが10ppm未満のレベルになるまで除去されることを特徴とするプロセス。
- 請求項6記載のプロセスにおいて、前記β−リチア輝石が、浸出ステップより前に冷却されて粉砕されることを特徴とするプロセス。
- 請求項19記載のプロセスにおいて、前記β−リチア輝石が、300μmより小さく粉砕されることを特徴とするプロセス。
- 請求項5,19及び20のいずれか1項に記載のプロセスにおいて、前記浸出ステップは、前記浸出ステップで用いられる塩酸溶液の沸点である温度で行われることを特徴とするプロセス。
- 請求項5及び19ないし21のいずれか1項に記載のプロセスにおいて、前記浸出ステップで用いられる塩酸溶液は、20重量%の塩酸であることを特徴とするプロセス。
- 請求項5及び19ないし22のいずれか1項に記載のプロセスにおいて、前記浸出ステップは大気圧のもとで行われることを特徴とするプロセス。
- 請求項5及び19ないし23のいずれか1項に記載のプロセスにおいて、前記浸出ステップは、6〜10時間の滞留時間の間、108°Cで連続的浸出タンク内で行われることを特徴とするプロセス。
- 請求項24記載のプロセスにおいて、前記滞留時間は8時間であることを特徴とするプロセス。
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AU2015900222A AU2015900222A0 (en) | 2015-01-27 | Processing of Lithium Containing Material including HCl Sparge | |
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PCT/AU2015/000650 WO2016119003A1 (en) | 2015-01-27 | 2015-10-30 | Processing of lithium containing material including hcl sparge |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023239095A1 (ko) * | 2022-06-09 | 2023-12-14 | 한국선별기 주식회사 | 폐내화갑으로부터 음이온교환을 이용하여 고순도의 탄산리튬을 제조하는 방법 |
Families Citing this family (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AR100672A1 (es) * | 2015-01-27 | 2016-10-26 | Reed Advanced Mat Pty Ltd | PROCESAMIENTO DE MATERIAL QUE CONTIENE LITIO INCLUYENDO INYECCIÓN DE HCl |
KR20190072667A (ko) | 2016-11-14 | 2019-06-25 | 리락 솔루션즈, 인크. | 코팅된 이온 교환 입자를 이용한 리튬 추출 |
EP3661619A4 (en) | 2017-08-02 | 2021-05-05 | Lilac Solutions, Inc. | LITHIUM EXTRACTION WITH POROUS ION EXCHANGE BEADS |
JP7379351B2 (ja) * | 2018-02-17 | 2023-11-14 | ライラック ソリューションズ,インク. | リチウムの抽出と変換のための統合システム |
EP3759257A4 (en) | 2018-02-28 | 2021-11-24 | Lilac Solutions, Inc. | ION EXCHANGE REACTOR WITH PARTICLE TRAPS FOR LITHIUM EXTRACTION |
KR102063810B1 (ko) * | 2018-06-07 | 2020-01-08 | 재단법인 포항산업과학연구원 | 염화 리튬 제조방법 및 그 장치 |
CN108946772A (zh) * | 2018-09-27 | 2018-12-07 | 山东泰和水处理科技股份有限公司 | 一种由锂矿石制备高纯碳酸锂的方法 |
AU2019352457A1 (en) * | 2018-10-01 | 2021-04-29 | Reed Advanced Materials Pty Ltd | Processing of lithium containing brines |
KR102164661B1 (ko) * | 2018-12-06 | 2020-10-12 | 주식회사 에코프로이노베이션 | 리튬 정광으로부터 황산나트튬 혼합 배소에 의한 수산화리튬 제조방법 |
CN109437264A (zh) * | 2018-12-06 | 2019-03-08 | 山东泰和水处理科技股份有限公司 | 一种从提锂废渣中制备氧化铝的方法 |
CN109650414B (zh) * | 2019-01-18 | 2020-01-14 | 成都开飞高能化学工业有限公司 | 高杂质锂源制备电池级、高纯级的氢氧化锂和碳酸锂的方法及*** |
EP4087825A4 (en) | 2020-01-09 | 2024-01-24 | Lilac Solutions, Inc. | PROCESS FOR SEPARATING UNWANTED METALS |
WO2021146768A1 (en) * | 2020-01-20 | 2021-07-29 | Tianqi Lithium Kwinana Pty Ltd | A process for producing alumina and a lithium salt |
KR20230023714A (ko) | 2020-06-09 | 2023-02-17 | 리락 솔루션즈, 인크. | 스케일런트의 존재 하에서의 리튬 추출 |
CA3199218A1 (en) | 2020-11-20 | 2022-05-27 | David Henry SNYDACKER | Lithium production with volatile acid |
KR102253829B1 (ko) * | 2020-11-27 | 2021-05-21 | 대진대학교 산학협력단 | 탄산 리튬 내의 황산 이온 제거 방법 |
KR20240014047A (ko) | 2021-04-23 | 2024-01-31 | 리락 솔루션즈, 인크. | 리튬 추출을 위한 이온 교환 장치 |
WO2023009887A1 (en) * | 2021-07-30 | 2023-02-02 | Schlumberger Technology Corporation | Lithium recovery thermal management |
EP4375387A1 (en) * | 2021-09-30 | 2024-05-29 | Asaka Riken Co., Ltd. | Method for recovering lithium from waste lithium-ion batteries |
WO2023057754A1 (en) * | 2021-10-06 | 2023-04-13 | Cycladex Ltd | Process |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2803518A (en) * | 1955-05-10 | 1957-08-20 | Foote Mineral Co | Method of recovering lithium values |
US3202477A (en) * | 1962-01-18 | 1965-08-24 | Diamond Alkali Co | Method of producing alkali metal carbonate |
US3278260A (en) * | 1963-02-08 | 1966-10-11 | Kerr Mc Gee Oil Ind Inc | Preparation and purification of lithium chloride |
US4036713A (en) | 1976-03-04 | 1977-07-19 | Foote Mineral Company | Process for the production of high purity lithium hydroxide |
AU542913B2 (en) * | 1981-07-21 | 1985-03-21 | Board Of Trustees Of The Leland Stanford Junior University | Stable supersaturated solutions of sparingly soluble salts |
AU2009238625B8 (en) * | 2008-04-22 | 2012-12-13 | Rockwood Lithium Inc. | Method of making high purity lithium hydroxide and hydrochloric acid |
AU2010341402B2 (en) * | 2010-01-07 | 2014-01-30 | Tianqi Lithium Corporation | Process for the production of lithium carbonate |
CN102167369B (zh) * | 2010-12-06 | 2013-11-06 | 兰州大学 | 一种降低LiCl中NaCl含量的方法 |
AU2011236094B2 (en) * | 2011-01-20 | 2012-11-29 | Rockwood Lithium Inc. | Production of high purity lithium compounds directly from lithium containing brines |
JP2015516507A (ja) | 2012-03-19 | 2015-06-11 | オーバイト アルミナ インコーポレイテッドOrbite Aluminae Inc. | 希土類元素及びレアメタルを回収するプロセス |
AU2013201833B2 (en) | 2012-08-13 | 2014-07-17 | Reed Advanced Materials Pty Ltd | Processing of Lithium Containing Ore |
US10167531B2 (en) * | 2014-03-13 | 2019-01-01 | Reed Advanced Materials Pty Ltd | Processing of lithium containing material |
AR100672A1 (es) * | 2015-01-27 | 2016-10-26 | Reed Advanced Mat Pty Ltd | PROCESAMIENTO DE MATERIAL QUE CONTIENE LITIO INCLUYENDO INYECCIÓN DE HCl |
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