CN117125683A - Method for producing battery-grade lithium phosphate from salt lake brine - Google Patents
Method for producing battery-grade lithium phosphate from salt lake brine Download PDFInfo
- Publication number
- CN117125683A CN117125683A CN202011312713.3A CN202011312713A CN117125683A CN 117125683 A CN117125683 A CN 117125683A CN 202011312713 A CN202011312713 A CN 202011312713A CN 117125683 A CN117125683 A CN 117125683A
- Authority
- CN
- China
- Prior art keywords
- lithium
- phosphate
- salt lake
- brine
- lake brine
- Prior art date
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- Pending
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- 239000012267 brine Substances 0.000 title claims abstract description 37
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 37
- 229910001386 lithium phosphate Inorganic materials 0.000 title claims abstract description 27
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 28
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 15
- 229910019142 PO4 Inorganic materials 0.000 claims description 12
- 239000010452 phosphate Substances 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical group [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000013049 sediment Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 150000002642 lithium compounds Chemical class 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/308—Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The application discloses a method for directly producing lithium phosphate from lithium-containing salt lake brine.
Description
Technical Field
The application belongs to the technical field of inorganic chemical material preparation, and in particular relates to a production method of a lithium phosphate material.
Background
Chinese patent application 2020112772412 proposes a method for producing lithium iron phosphate, which is the positive electrode material of a lithium ion battery, from lithium phosphate as a raw material. The battery-grade lithium phosphate is prepared by the reaction of lithium hydroxide and phosphoric acid, and has higher purity and relatively higher cost. Salt lake brine contains rich lithium, but the process of extracting lithium from salt lake is complex.
Disclosure of Invention
The application mainly solves the technical problems that: the method for directly producing the battery-grade lithium phosphate from the salt lake brine is characterized in that the battery-grade lithium phosphate is directly produced from the salt lake brine, the salt lake brine is not required to be concentrated and then extracted, and the lithium contained in the salt lake brine is not required to be converted into lithium carbonate or other lithium compounds and then converted into lithium phosphate.
In order to achieve the above purpose, the application adopts a technical scheme that:
3Li + +PO 4 3- = Li 3 PO 4
adding phosphate into the lithium-containing salt lake brine, and combining phosphate ions generated by the phosphate with lithium ions in the brine to generate lithium phosphate precipitates.
The lithium-containing salt lake brine is carbonate-type lithium-containing salt lake brine, and the lithium content of the brine is more than 0.5g/L.
The phosphate is sodium phosphate, potassium phosphate or a mixture thereof.
Further, the carbonate type lithium-containing salt lake brine is subjected to pretreatment, wherein the pretreatment is divided into physical filtration and chemical treatment. The physical filtration is mainly micro filtration to remove solid impurities, and the chemical treatment is to strengthen alkali to remove calcium and magnesium ions. The strong base is sodium hydroxide, potassium hydroxide, calcium hydroxide or a compound thereof.
The beneficial effects of the application are as follows: the carbonate type lithium-containing salt lake brine is directly prepared into the battery-grade lithium phosphate by a one-step method, other lithium compounds do not need to be generated to serve as intermediate products, byproducts are avoided, and the production cost of the battery-grade lithium phosphate is reduced.
Drawings
FIG. 1 is a schematic flow chart of producing battery grade lithium phosphate from carbonate type lithium-containing salt lake brine, wherein 1-lithium-containing brine, 2-primary filtration, 3-pretreatment tank, 4-secondary filtration, 5-lithium precipitation reaction tank, 6-tertiary filtration and 7-lithium phosphate precipitation.
Detailed Description
Example 1
Extracting lithium-containing brine 1 from a carbonate-type lithium-containing salt lake, removing solid impurities by primary filtration 2, injecting the solution into a pretreatment tank 3, adding a strong alkali solution into the pretreatment tank 3, adjusting the amount of the added alkali solution according to the concentration of calcium and magnesium ions contained in the brine, adjusting the pH value to be more than 12, removing the calcium and magnesium ions in the brine, filtering the brine for the second time 4 to remove sediment generated by the previous reaction, entering a lithium precipitation reaction tank 5, adding a phosphate solution into the lithium precipitation reaction tank 5, reacting phosphate ions generated by phosphate ionization with lithium ions in the brine to generate lithium phosphate sediment, re-injecting the brine into the salt lake after three times of filtration 6, and cleaning and drying the lithium phosphate sediment 7 to obtain a battery-level lithium phosphate finished product. The strong alkali is sodium hydroxide solution, the phosphate is sodium phosphate, and the sediment generated by pretreatment is mainly magnesium hydroxide and calcium carbonate.
Example two
Extracting lithium-containing brine 1 from a carbonate-type lithium-containing salt lake, removing solid impurities by primary filtration 2, injecting the solution into a pretreatment tank 3, adding strong alkali into the pretreatment tank 3, adjusting the amount of the added strong alkali according to the concentration of calcium and magnesium ions contained in the brine, adjusting the pH value to be more than 12, removing the calcium and magnesium ions in the brine, filtering the brine for the second time 4 to remove sediment generated by the previous reaction, entering a lithium precipitation reaction tank 5, adding phosphate solution into the lithium precipitation reaction tank 5, reacting phosphate ions generated by phosphate ionization with lithium ions in the brine to generate lithium phosphate sediment, re-injecting the brine into the salt lake after three times of filtration 6, and cleaning and drying the lithium phosphate sediment 7 to obtain a battery-level lithium phosphate product. The strong alkali is calcium hydroxide and calcium oxide mixture, the phosphate is sodium phosphate, and the sediment generated by pretreatment is a mixture of magnesium hydroxide and calcium carbonate which are mainly calcium carbonate.
The above is a part of application examples of the application, and the production of lithium phosphate by adding a soluble phosphate solution into lithium-containing salt lake brine pretreated by strong alkali for lithium precipitation reaction belongs to the protection scope of the application.
Claims (4)
1. A method for directly producing lithium phosphate from lithium-containing salt lake brine is characterized by comprising the following steps:
(1) The raw material is carbonate type lithium-containing salt lake brine;
(2) The product is battery grade lithium phosphate;
(3) The production process is that carbonate lithium-containing salt lake brine is filtered, alkali precipitation is enhanced to remove calcium and magnesium ions, lithium ions are precipitated by adding phosphate into the brine, and the precipitation is cleaned and dried to obtain the battery-grade lithium phosphate product.
2. The method for directly producing battery-grade lithium phosphate from lithium-containing salt lake brine according to claim 1, wherein the phosphate is sodium phosphate.
3. The method for directly producing battery grade lithium phosphate from lithium-containing salt lake brine of claim 1, wherein the strong base is sodium hydroxide.
4. The method for directly producing battery-grade lithium phosphate from lithium-containing salt lake brine according to claim 1, wherein the strong base is calcium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011312713.3A CN117125683A (en) | 2020-11-21 | 2020-11-21 | Method for producing battery-grade lithium phosphate from salt lake brine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011312713.3A CN117125683A (en) | 2020-11-21 | 2020-11-21 | Method for producing battery-grade lithium phosphate from salt lake brine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117125683A true CN117125683A (en) | 2023-11-28 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011312713.3A Pending CN117125683A (en) | 2020-11-21 | 2020-11-21 | Method for producing battery-grade lithium phosphate from salt lake brine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117125683A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106507705B (en) * | 2008-12-12 | 2011-07-27 | 核工业北京化工冶金研究院 | The method for removing calcium and magnesium impurity from the high lithium solution of calcium-magnesium-containing |
| KR20120063069A (en) * | 2010-12-07 | 2012-06-15 | 재단법인 포항산업과학연구원 | Manufacturing method of lithium hydroxide and lithium carbonate with high purity from brine |
| CN107787302A (en) * | 2015-04-30 | 2018-03-09 | 浦项产业科学研究院 | The preparation method and its device of lithium hydroxide and lithium carbonate |
| CN108428893A (en) * | 2017-09-21 | 2018-08-21 | 中国地质科学院矿产综合利用研究所 | Preparation method of brine battery-grade lithium carbonate |
| CN109772169A (en) * | 2018-09-18 | 2019-05-21 | 张伟 | A kind of bipolar membrane electrodialysis system and its method for preparing lithium hydroxide |
| CN110357055A (en) * | 2019-08-09 | 2019-10-22 | 深圳市德方纳米科技股份有限公司 | A kind of method and application thereof extracted lithium from salt lake bittern and prepare lithium phosphate |
| KR102059858B1 (en) * | 2019-11-01 | 2019-12-27 | 한국지질자원연구원 | Method for recovering lithium from brine |
-
2020
- 2020-11-21 CN CN202011312713.3A patent/CN117125683A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106507705B (en) * | 2008-12-12 | 2011-07-27 | 核工业北京化工冶金研究院 | The method for removing calcium and magnesium impurity from the high lithium solution of calcium-magnesium-containing |
| KR20120063069A (en) * | 2010-12-07 | 2012-06-15 | 재단법인 포항산업과학연구원 | Manufacturing method of lithium hydroxide and lithium carbonate with high purity from brine |
| CN107787302A (en) * | 2015-04-30 | 2018-03-09 | 浦项产业科学研究院 | The preparation method and its device of lithium hydroxide and lithium carbonate |
| CN108428893A (en) * | 2017-09-21 | 2018-08-21 | 中国地质科学院矿产综合利用研究所 | Preparation method of brine battery-grade lithium carbonate |
| CN109772169A (en) * | 2018-09-18 | 2019-05-21 | 张伟 | A kind of bipolar membrane electrodialysis system and its method for preparing lithium hydroxide |
| CN110357055A (en) * | 2019-08-09 | 2019-10-22 | 深圳市德方纳米科技股份有限公司 | A kind of method and application thereof extracted lithium from salt lake bittern and prepare lithium phosphate |
| KR102059858B1 (en) * | 2019-11-01 | 2019-12-27 | 한국지질자원연구원 | Method for recovering lithium from brine |
Non-Patent Citations (1)
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|---|
| 邱定蕃 等: "《稀贵金属冶金新进展》", 冶金工业出版社, pages: 233 - 234 * |
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