CN102382991A - Method for preparing lithium metal through vacuum hot reduction of iron - Google Patents
Method for preparing lithium metal through vacuum hot reduction of iron Download PDFInfo
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- CN102382991A CN102382991A CN2011103414310A CN201110341431A CN102382991A CN 102382991 A CN102382991 A CN 102382991A CN 2011103414310 A CN2011103414310 A CN 2011103414310A CN 201110341431 A CN201110341431 A CN 201110341431A CN 102382991 A CN102382991 A CN 102382991A
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- iron
- lithium
- vacuum
- purity
- metallic lithium
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 35
- 230000002829 reductive effect Effects 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000009413 insulation Methods 0.000 claims abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 40
- 238000010792 warming Methods 0.000 claims description 16
- 239000012778 molding material Substances 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000005453 pelletization Methods 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 3
- 239000003638 chemical reducing agent Substances 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000008188 pellet Substances 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 16
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 8
- 229910001947 lithium oxide Inorganic materials 0.000 description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 7
- 239000004411 aluminium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 description 3
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 3
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 230000000454 anti-cipatory effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical compound [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a method for preparing lithium metal through vacuum hot reduction of iron. Lithium carbonate with a purity which is larger than or equal with 98% is used as raw material. Iron powder with a purity which is larger than or equal with 98% is used as a reducing agent. The iron powder and the lithium carbonate are mixed. The mixture is prepared to pellet shape or sheet shape. Vacuumizing is performed on the mixture. Calcining and heat insulation are performed. Heat increase is performed in a vacuum. The reduced lithium metal volatilizes in a gaseous state. The lithium metal is obtained after condensing the volatilized gas. According to the method of the invention, lithium carbonate is used as raw material; and the iron with advantages of abundant resource and low price is used as a reducing agent. The method for preparing the lithium metal through vacuum hot reduction of the iron has the following advantages: short flow, simple process, convenient operation, low cost, low environment pollution, etc.
Description
Technical field
The present invention relates to the thermal reduction of a kind of vacuum iron and produce the method for metallic lithium, belong to the technical field that the vacuum metal thermal reduction prepares metallic substance.
Background technology
Lithium is important rare metal, and it all has important purposes aspect civil and military, and along with expanding economy, the Application Areas of lithium is constantly enlarged, and demand constantly increases.At present fused salt electrolysis process is adopted in the preparation of metallic lithium more in industry, though fused salt electrolysis process is produced the metallic lithium technical maturity, yet its cost is high, product purity is low, severe environmental pollution, technical process are long etc.
Proposed a lot of methods about preparing the domestic and international investigators of metallic lithium, 1894 years watts of companies (Bappeh) once prepared metallic lithium with the magnesium reduction Lithium Hydroxide MonoHydrate; Muriate, fluorochemical and sulfide or the reduction with carbon Quilonum Retard of also useful carbide of calcium reduction lithium are produced metallic lithium; Kroll etc., Smeets etc., Stauffer etc. prepare metallic lithium with reduction-oxidation lithiums such as silicon, aluminium, magnesium and triphane respectively; Kunming University of Science and Technology has also obtained metallic lithium with reduction Quilonum Retard, Lithium Oxide 98mins such as carbon, carbide of calcium, aluminium, silicon and aluminum silicon alloys respectively; Yellow Qi Xin etc. has invented with Lithium Hydroxide MonoHydrate and has prepared the method for metallic lithium and with the method for electrical conductivity of molten slag preparing metal lithium at high temperature employing, use Lithium Hydroxide MonoHydrate and Quilonum Retard to be raw material, and aluminium powder is that reductive agent reduces under high-temperature vacuum and prepares metallic lithium; Towering working method and the specific equipment of having invented high-purity lithium metal of anticipatory remark uses Quilonum Retard and lime or white lake to be raw material, ferrosilicon or aluminium powder do reductive agent under vacuum high-temperature, reduce the preparation metallic lithium; Middle village English is inferior, Cooley expense Prokofiev Fu Laji Mil Ke Sitanjinnuo etc. also invented the preparation method of metallic lithium respectively; Use Quilonum Retard and chlorine to be raw material respectively; Make it carry out contact reacts with drying process and obtain Lithium chloride (anhydrous), use resulting Lithium chloride (anhydrous) again, be equipped with metallic lithium through the fusion electrolysis legal system as raw material; Also obtained metallic lithium; This method can be avoided causing the corrosion to device materials by the molten salt of chlorine and Quilonum Retard, and uses Quilonum Retard, aluminum oxide to be raw material, aluminium powder be reductive agent under high-temperature vacuum, reduce the preparation metallic lithium.The somebody has invented from salt lake brine respectively, has contained the method that reclaims lithium lithium ore, waste and old lithium ion battery and the waste and old pole piece, but the primary products of the lithium of preparation are Quilonum Retard or lithium salts.
Summary of the invention
For overcoming problems such as cost height, product purity is low, environmental pollution is big, technical process is long, the method that the present invention provides the thermal reduction of a kind of vacuum iron to produce metallic lithium realizes through following technical proposal.
The method of metallic lithium is produced in the thermal reduction of a kind of vacuum iron, following each step of process:
(1) with purity >=98% Quilonum Retard as raw material, with purity be >=98% iron powder as reductive agent, be that 0.7～2:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed pelletizing or sheet;
(3) step (2) gained molding materials is placed under the vacuum; Pressure≤20Pa, and be warming up to 700 ℃ with the temperature rise rate of 1.5～10 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 0.1～20Pa; Again under vacuum, be warming up to 1100～1400 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 1～8h with the temperature rise rate of 5～20 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
The pelletizing of said step (2) is the pelletizing of Φ 10～50mm.
The sheet of said step (2) is the sheet of 25 * 3～40 * 40mm.
Effect of the present invention and advantage: the present invention is raw material with the Quilonum Retard, and as reductive agent, present method has that flow process is short, technology is simple, easy and simple to handle, characteristics such as cost is low, environmental pollution is little with aboundresources and cheap iron.
Embodiment
To combine embodiment further to illustrate content of the present invention below, but these instances do not limit protection scope of the present invention.
Embodiment 1
(1) with purity 98% Quilonum Retard as raw material, with purity be 98% iron powder as reductive agent, be that 0.7:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed the pelletizing of Φ 10mm;
(3) step (2) gained molding materials being put into steel crucibles places under the vacuum; Pressure 5Pa, and be warming up to 700 ℃ with the temperature rise rate of 2 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 0.2Pa; Again under vacuum, be warming up to 1200 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 1h with the temperature rise rate of 5 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
Embodiment 2
(1) with purity 99% Quilonum Retard as raw material, with purity be 98% iron powder as reductive agent, be that 1:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed the pelletizing of Φ 30mm;
(3) step (2) gained molding materials being put into steel crucibles places under the vacuum; Pressure 15Pa, and be warming up to 700 ℃ with the temperature rise rate of 5 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 10Pa; Again under vacuum, be warming up to 1250 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 4h with the temperature rise rate of 10 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
Embodiment 3
(1) with purity 98% Quilonum Retard as raw material, with purity be 99% iron powder as reductive agent, be that 2:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed the pelletizing of Φ 50mm;
(3) step (2) gained molding materials is placed under the vacuum; Pressure 20Pa, and be warming up to 700 ℃ with the temperature rise rate of 10 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 18Pa; Again under vacuum, be warming up to 1300 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 7h with the temperature rise rate of 20 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
Embodiment 4
(1) with purity 99% Quilonum Retard as raw material, with purity be 99% iron powder as reductive agent, be that 1.5:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed 25 * 3mm sheet;
(3) step (2) gained molding materials is placed under the vacuum; Pressure 18Pa, and be warming up to 700 ℃ with the temperature rise rate of 1.5 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 0.1Pa; Again under vacuum, be warming up to 1100 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 8h with the temperature rise rate of 8 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
Embodiment 5
(1) with purity 98% Quilonum Retard as raw material, with purity be 98% iron powder as reductive agent, be that 0.9:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed 40 * 40mm sheet;
(3) step (2) gained molding materials is placed under the vacuum; Pressure 20Pa, and be warming up to 700 ℃ with the temperature rise rate of 9 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 20Pa; Again under vacuum, be warming up to 1400 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 5h with the temperature rise rate of 15 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
Embodiment 6
(1) with purity 99% Quilonum Retard as raw material, with purity be 98% iron powder as reductive agent, be that 1.8:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed 30 * 20mm sheet;
(3) step (2) gained molding materials is placed under the vacuum; Pressure 10Pa, and be warming up to 700 ℃ with the temperature rise rate of 6 ℃/min and calcine, the Quilonum Retard in the molding materials is decomposed; Be incubated when pressure is 9Pa; Again under vacuum, be warming up to 1200 ℃ of reduction reactions of carrying out iron and Lithium Oxide 98min, insulation 8h with the temperature rise rate of 12 ℃ ∕ min; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
Claims (3)
1. the method for metallic lithium is produced in vacuum iron thermal reduction, it is characterized in that through following each step:
(1) with purity >=98% Quilonum Retard as raw material, with purity be >=98% iron powder as reductive agent, be that 0.7～2:1 is uniformly mixed into mixture with iron powder and Quilonum Retard by mass ratio;
(2) step (1) gained mixture is processed pelletizing or sheet;
(3) step (2) gained molding materials is placed under the vacuum; Pressure≤20Pa; And be warming up to 700 ℃ with the temperature rise rate of 1.5～10 ℃/min and calcine, be incubated when pressure is 0.1～20Pa, again under vacuum; Temperature rise rate with 5～20 ℃ ∕ min is warming up to 1100～1400 ℃, insulation 1～8h; The metallic lithium that is reduced out volatilizees with gaseous state, promptly obtains metallic lithium behind the condensation evaporable gas.
2. method according to claim 1 is characterized in that: the pelletizing of said step (2) is the pelletizing of Φ 10～50mm.
3. method according to claim 1 is characterized in that: the sheet of said step (2) is the sheet of 25 * 3～40 * 40mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103414310A CN102382991A (en) | 2011-11-02 | 2011-11-02 | Method for preparing lithium metal through vacuum hot reduction of iron |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103414310A CN102382991A (en) | 2011-11-02 | 2011-11-02 | Method for preparing lithium metal through vacuum hot reduction of iron |
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| Publication Number | Publication Date |
|---|---|
| CN102382991A true CN102382991A (en) | 2012-03-21 |
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| CN2011103414310A Pending CN102382991A (en) | 2011-11-02 | 2011-11-02 | Method for preparing lithium metal through vacuum hot reduction of iron |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129587A (en) * | 2019-05-27 | 2019-08-16 | 昆明理工大学 | A kind of method that spodumene vacuum metling extracts lithium metal and prepares alusil alloy |
| CN113149039A (en) * | 2021-04-30 | 2021-07-23 | 四川万邦胜辉新能源科技有限公司 | Method for preparing lithium oxide by thermally reducing spodumene |
| CN115418482A (en) * | 2022-08-30 | 2022-12-02 | 重庆赛迪热工环保工程技术有限公司 | Metallurgy solid waste disposal process adopting iron-based vacuum reduction |
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|---|---|---|---|---|
| CN1162022A (en) * | 1997-02-24 | 1997-10-15 | 昆明理工大学 | Method for vacuum smelting lithium |
| CN1299884A (en) * | 1999-12-10 | 2001-06-20 | 中国科学院青海盐湖研究所 | Heat reduction preparation and purification process and equipment of metal lithium |
| CN101016590A (en) * | 2007-02-26 | 2007-08-15 | 黄启新 | Method of preparing lithium from spodumene concentrate |
| CN101445874A (en) * | 2008-12-24 | 2009-06-03 | 大连天熙创展科技有限公司 | Production method for high-purity lithium metal and special equipment thereof |
-
2011
- 2011-11-02 CN CN2011103414310A patent/CN102382991A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1162022A (en) * | 1997-02-24 | 1997-10-15 | 昆明理工大学 | Method for vacuum smelting lithium |
| CN1299884A (en) * | 1999-12-10 | 2001-06-20 | 中国科学院青海盐湖研究所 | Heat reduction preparation and purification process and equipment of metal lithium |
| CN101016590A (en) * | 2007-02-26 | 2007-08-15 | 黄启新 | Method of preparing lithium from spodumene concentrate |
| CN101445874A (en) * | 2008-12-24 | 2009-06-03 | 大连天熙创展科技有限公司 | Production method for high-purity lithium metal and special equipment thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129587A (en) * | 2019-05-27 | 2019-08-16 | 昆明理工大学 | A kind of method that spodumene vacuum metling extracts lithium metal and prepares alusil alloy |
| CN113149039A (en) * | 2021-04-30 | 2021-07-23 | 四川万邦胜辉新能源科技有限公司 | Method for preparing lithium oxide by thermally reducing spodumene |
| CN113149039B (en) * | 2021-04-30 | 2023-03-03 | 四川万邦胜辉新能源科技有限公司 | Method for preparing lithium oxide by thermal reduction of spodumene |
| CN115418482A (en) * | 2022-08-30 | 2022-12-02 | 重庆赛迪热工环保工程技术有限公司 | Metallurgy solid waste disposal process adopting iron-based vacuum reduction |
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Application publication date: 20120321 |