RU2013151413A - CALCINATE METHOD FOR PRODUCING LITHIUM CARBONATE FROM LITHIUM-BASED RAW MATERIALS - Google Patents
CALCINATE METHOD FOR PRODUCING LITHIUM CARBONATE FROM LITHIUM-BASED RAW MATERIALS Download PDFInfo
- Publication number
- RU2013151413A RU2013151413A RU2013151413/05A RU2013151413A RU2013151413A RU 2013151413 A RU2013151413 A RU 2013151413A RU 2013151413/05 A RU2013151413/05 A RU 2013151413/05A RU 2013151413 A RU2013151413 A RU 2013151413A RU 2013151413 A RU2013151413 A RU 2013151413A
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- RU
- Russia
- Prior art keywords
- lithium
- solution
- mother liquor
- ammonia
- lithium carbonate
- Prior art date
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract 13
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract 3
- 239000002994 raw material Substances 0.000 title claims abstract 3
- 239000000243 solution Substances 0.000 claims abstract 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract 18
- 239000012452 mother liquor Substances 0.000 claims abstract 12
- 150000003863 ammonium salts Chemical class 0.000 claims abstract 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract 9
- 229910021529 ammonia Inorganic materials 0.000 claims abstract 9
- 229910052744 lithium Inorganic materials 0.000 claims abstract 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract 8
- 238000005406 washing Methods 0.000 claims abstract 8
- 238000001354 calcination Methods 0.000 claims abstract 7
- 239000013078 crystal Substances 0.000 claims abstract 6
- 230000008021 deposition Effects 0.000 claims abstract 6
- 239000000203 mixture Substances 0.000 claims abstract 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract 4
- 239000001569 carbon dioxide Substances 0.000 claims abstract 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract 4
- 239000002244 precipitate Substances 0.000 claims abstract 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract 3
- 239000012535 impurity Substances 0.000 claims abstract 3
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract 3
- 238000000746 purification Methods 0.000 claims abstract 3
- 238000000926 separation method Methods 0.000 claims abstract 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract 2
- 235000019738 Limestone Nutrition 0.000 claims abstract 2
- 229910002651 NO3 Inorganic materials 0.000 claims abstract 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract 2
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract 2
- JJEJDZONIFQNHG-UHFFFAOYSA-N [C+4].N Chemical compound [C+4].N JJEJDZONIFQNHG-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000002250 absorbent Substances 0.000 claims abstract 2
- 230000002745 absorbent Effects 0.000 claims abstract 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract 2
- 239000000920 calcium hydroxide Substances 0.000 claims abstract 2
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract 2
- 239000000292 calcium oxide Substances 0.000 claims abstract 2
- 235000012255 calcium oxide Nutrition 0.000 claims abstract 2
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000004571 lime Substances 0.000 claims abstract 2
- 239000006028 limestone Substances 0.000 claims abstract 2
- 239000007788 liquid Substances 0.000 claims abstract 2
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract 2
- 159000000002 lithium salts Chemical class 0.000 claims abstract 2
- 239000011259 mixed solution Substances 0.000 claims abstract 2
- 239000012716 precipitator Substances 0.000 claims abstract 2
- 238000011084 recovery Methods 0.000 claims abstract 2
- 238000009938 salting Methods 0.000 claims abstract 2
- 229920006395 saturated elastomer Polymers 0.000 claims abstract 2
- 239000012047 saturated solution Substances 0.000 claims abstract 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims 5
- 238000001556 precipitation Methods 0.000 claims 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 238000005273 aeration Methods 0.000 claims 2
- 239000006227 byproduct Substances 0.000 claims 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims 2
- 238000004821 distillation Methods 0.000 claims 2
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims 2
- 238000005185 salting out Methods 0.000 claims 2
- FZUJWWOKDIGOKH-UHFFFAOYSA-N sulfuric acid hydrochloride Chemical compound Cl.OS(O)(=O)=O FZUJWWOKDIGOKH-UHFFFAOYSA-N 0.000 claims 2
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims 1
- 235000019270 ammonium chloride Nutrition 0.000 claims 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims 1
- 235000011130 ammonium sulphate Nutrition 0.000 claims 1
- 238000010276 construction Methods 0.000 claims 1
- 239000010440 gypsum Substances 0.000 claims 1
- 229910052602 gypsum Inorganic materials 0.000 claims 1
- FGXCQKDTZIXEIT-UHFFFAOYSA-M lithium sulfuric acid chloride Chemical compound [Cl-].[Li+].S(=O)(=O)(O)O FGXCQKDTZIXEIT-UHFFFAOYSA-M 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000002910 solid waste Substances 0.000 claims 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
1. Кальцинатный способ получения карбоната лития из литиеносного сырья, включающий получение продуктивного литийсодержащего раствора, его очистку от примесей, реагентное осаждение карбоната лития углеаммонийным осадителем, отделение осажденного карбоната лития от маточного раствора, промывку и сушку осадка, отличающийся тем, что осаждение карбоната лития из очищенного продуктивного литийсодержащего хлоридного или сульфатного или азотнокислого или смешанного раствора проводят путем его обработки газовой смесью аммиака и углекислого газа, взятых в соотношении 2:1, при охлаждении в ступенчато-противоточном режиме контакта жидкой и газовой фаз; из маточного раствора после отделения карбоната лития высаливают аммонийную соль хлорида или нитрата, добавляя в раствор соответствующую соль лития или насыщенный ею раствор; выделившиеся кристаллы аммонийной соли - NHCl или NHNO, отделяют от маточного раствора, промывают водой и из промытых кристаллов готовят насыщенный раствор аммонийной соли, который подогревают в рекуператоре тепла и подвергают кальцинации путем контакта с негашеной или гашеной известью; выделяющийся при этом аммиак в смеси с углекислым газом, полученным одновременно с известью путем термического разложения известняка, направляют на операцию осаждения карбоната лития; горячий маточный раствор операции кальцинации аэрируют воздухом, удаляя остаточный аммиак, который из воздушного потока абсорбируют разбавленным и подкисленным раствором операции высаливания аммонийной соли; поглотивший аммиак продуктивный литийсодержащий раствор - абсорбент, направляют на операцию осаждения LiCO; очищенны1. Calcine method for producing lithium carbonate from lithium-containing raw materials, including obtaining a productive lithium-containing solution, its purification from impurities, reagent deposition of lithium carbonate with a carbon ammonium precipitator, separating precipitated lithium carbonate from the mother liquor, washing and drying the precipitate, characterized in that the deposition of lithium carbonate from a purified productive lithium-containing chloride or sulfate or nitric acid or mixed solution is carried out by treating it with a gas mixture of ammonia and carbon dioxide o gas taken in the ratio 2: 1, when cooled in a stepwise-countercurrent mode of contact of the liquid and gas phases; from the mother liquor after separation of lithium carbonate, the ammonium salt of chloride or nitrate is salted out by adding the corresponding lithium salt or a solution saturated with it; precipitated ammonium salt crystals — NHCl or NHNO — are separated from the mother liquor, washed with water, and a saturated solution of ammonium salt is prepared from the washed crystals, which is heated in a heat recovery unit and calcined by contact with quicklime or slaked lime; the ammonia released in this case in a mixture with carbon dioxide, obtained simultaneously with lime by thermal decomposition of limestone, is sent to the deposition of lithium carbonate; the hot mother liquor of the calcination operation is aerated with air, removing residual ammonia, which is absorbed from the air stream by the diluted and acidified solution of the ammonium salt salting operation; an ammonia-absorbing productive lithium-containing solution - absorbent, is sent to the LiCO deposition operation; cleared
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2013151413/05A RU2560359C2 (en) | 2013-11-19 | 2013-11-19 | Calcification method of producing lithium carbonate from lithium-bearing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2013151413/05A RU2560359C2 (en) | 2013-11-19 | 2013-11-19 | Calcification method of producing lithium carbonate from lithium-bearing material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| RU2013151413A true RU2013151413A (en) | 2015-05-27 |
| RU2560359C2 RU2560359C2 (en) | 2015-08-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| RU2013151413/05A RU2560359C2 (en) | 2013-11-19 | 2013-11-19 | Calcification method of producing lithium carbonate from lithium-bearing material |
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| RU (1) | RU2560359C2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3689821A1 (en) * | 2017-08-02 | 2020-08-05 | JX Nippon Mining & Metals Corporation | Method for dissolving lithium compound, method for manufacturing lithium carbonate, and method for recovering lithium from lithium ion secondary cell scrap |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230365421A1 (en) * | 2021-04-01 | 2023-11-16 | Li-Technology Pty Ltd | Lithium carbonate recovery process |
| WO2024178460A1 (en) * | 2023-02-27 | 2024-09-06 | ICSIP Pty Ltd | Lithium recovery from sedimentary silicates |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5219550A (en) * | 1989-03-31 | 1993-06-15 | Cyprus Foote Mineral Company | Production of low boron lithium carbonate from lithium-containing brine |
| US6207126B1 (en) * | 1998-07-16 | 2001-03-27 | Chemetall Foote Corporation | Recovery of lithium compounds from brines |
| RU2243157C2 (en) * | 2003-02-11 | 2004-12-27 | Открытое акционерное общество "Новосибирский завод химконцентратов" | Extrahigh-purity lithium carbonate preparation method |
| RU2283283C1 (en) * | 2004-12-30 | 2006-09-10 | Закрытое акционерное общество (ЗАО) "Экостар-Наутех" | Process of producing h-purity lithium carbonate from lithium-bearing chloride brines |
-
2013
- 2013-11-19 RU RU2013151413/05A patent/RU2560359C2/en active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3689821A1 (en) * | 2017-08-02 | 2020-08-05 | JX Nippon Mining & Metals Corporation | Method for dissolving lithium compound, method for manufacturing lithium carbonate, and method for recovering lithium from lithium ion secondary cell scrap |
| US11718895B2 (en) | 2017-08-02 | 2023-08-08 | Jx Nippon Mining & Metals Corporation | Method for dissolving lithium compound, method for manufacturing lithium carbonate, and method for recovering lithium from lithium ion secondary cell scrap |
| US12123074B2 (en) | 2017-08-02 | 2024-10-22 | Jx Metals Circular Solutions Co., Ltd. | Method for dissolving lithium compound, method for manufacturing lithium carbonate, and method for recovering lithium from lithium ion secondary cell scrap |
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| Publication number | Publication date |
|---|---|
| RU2560359C2 (en) | 2015-08-20 |
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| PC43 | Official registration of the transfer of the exclusive right without contract for inventions |
Effective date: 20150921 |
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| PC41 | Official registration of the transfer of exclusive right |
Effective date: 20161013 |
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| PC41 | Official registration of the transfer of exclusive right |
Effective date: 20170519 |