CN1487104A - Lithium preparing process with lithium carbonate - Google Patents
Lithium preparing process with lithium carbonate Download PDFInfo
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- CN1487104A CN1487104A CNA031455573A CN03145557A CN1487104A CN 1487104 A CN1487104 A CN 1487104A CN A031455573 A CNA031455573 A CN A031455573A CN 03145557 A CN03145557 A CN 03145557A CN 1487104 A CN1487104 A CN 1487104A
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Abstract
The lithium preparing process with lithium carbonate includes the following steps: mixing lithium carbonate, lime and alumina in certain proportion; pelletizing the mixture; calcining the mixture pellet at 900-1100 deg.c for lithium carbonate to decompose completely and for contained CO2 to be exhausted completely; crushing the pellet; mixing the obtained powder and silicoferrite in certain ratio; pelletizing the mixture powder; reducing the pellet at 1500-1600 deg.c and vacuum degree lower than or equal to 30 pa to produce lithium vapor; condensation to obtain solid lithium. The present invention has the features of high product purity, low cost, less environmental pollution and less investment in apparatus.
Description
Technical Field
The invention relates to a method for smelting metal, in particular to a method for preparing lithium by using lithium carbonate.
Background
The metal lithium is an important metal raw material in the aspects of military industry and civil use, and the existing electrolytic lithium preparation method has the defects that the product purity is low and is only 97-98 percent; before use, the product is purified by multiple times of distillation, so the product cost is higher; in addition, the method for preparing lithium by electrolysis has the problem of serious environmental pollution, namely, the chlorine generated in the process of preparing lithium by electrolysis can cause serious pollution to the environment; in addition, the equipment investment of the method for producing lithium by electrolysis is also large.
Disclosure of Invention
The invention aims to provide a method for preparing lithium by using lithium carbonate, which has the advantages of high product purity, low cost, small environmental pollution and less equipment investment.
The object of the present invention is achieved by a method for preparing lithium from lithium carbonate, comprising the steps of:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3) Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes according to the weight ratio of 0.8-1.05: 0.819-0.83: 0.256-0.26, and uniformly mixing the powdery lithium carbonate with the powdery quicklime with the purity of more than 96 percent and the granularity of less than 65 meshes;
② making the powder mixture into powder with particle size n of 10 mm-20 mm and specific gravity of 1.6-2g/cm3The solid particles of (4);
③ calcining the solid particles at 900-1100 deg.C until the lithium carbonate is decomposed completely and the carbon dioxide is exhausted completely, and keeping the solid particles after calcining;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) in a weight ratio of 0.9-1.2: 0.193-0.21, respectively, and mixing the powder and ferrosilicon powder with silicon content of 75-85% and particle size of 65-130 meshes;
⑥ making the powder mixture into powder with particle size n of 10 mm-20 mm and specific gravity of 1.8-2g/cm3The solid particles of (4);
⑦ performing reduction reaction on the solid particles obtained in the previous step at 1500-1600 ℃ and vacuum degree P less than or equal to 30Pa to generate lithium vapor;
⑧ condensing the lithium vapor to obtain solid lithium.
Because the lithium is extracted from the lithium carbonate by adopting the redox method, and the raw materials are granulated, and the pure heat source and the vacuum heating method are selected for smelting, the purity of the lithium prepared by the method can reach 99 percent, 99.9 percent of the lithium prepared by the method is about 70 percent and 99 percent of the lithium prepared by the method is about 30 percent through actual tests; the recovery rate of lithium is more than 93 percent; because the lithium prepared by the method has high purity, the method can omit the distillation and purification steps when in use, and thus the cost for preparing the lithium by the method is low; in addition, the method for preparing the lithium does not generate a large amount of gas polluting the environment, so the environmental pollution is small; in addition, the invention does not need an electrolysis device with a complex and expensive structure, so the investment requirement of the invention on equipment is less.
Detailed Description
In the following, embodiments of the present invention will be further described with reference to the accompanying drawings, a method for preparing lithium from lithium carbonate, comprising the steps of:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3) Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes according to the weight ratio of 0.8-1.05: 0.819-0.83: 0.256-0.26, and uniformly mixing the powdery lithium carbonate with the powdery quicklime with the purity of more than 96 percent and the granularity of less than 65 meshes;
② making the powder mixture into powder with particle size n of 10 mm-20 mm and specific gravity of 1.6-2g/cm3The solid particles of (4); one of the purposes of granulating the powdery mixed material is to facilitate the thermal decomposition of the lithium carbonate and discharge all decomposed carbon dioxide gas;
③ calcining the solid particles at 900-1100 deg.C until the lithium carbonate is decomposed completely, and the carbon dioxide is exhausted completely, and the obtained calcined solid particles are ready for use;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) in a weight ratio of 0.9-1.2: 0.193-0.21, respectively, and mixing the powderand ferrosilicon powder with silicon content of 75-85% and particle size of 65-130 meshes;
⑥ making the powder mixture into powder with particle size n of 10 mm-20 mm and specific gravity of 1.8-2g/cm3The solid particles of (4); one of the purposes of processing the powdery raw materials into solid particles in the step is to ensure that the raw materials have a relatively stable ratio so as to facilitate the oxidation-reduction reactionIn addition, the pollution of dust to the purity of the product can be effectively reduced after granulation;
⑦ reducing the solid particles at 1500-1600 deg.C and vacuum degree P less than 30Pa to generate lithium vapor, wherein the lithium oxide and silicon iron generate oxidation-reduction reaction to generate lithium, iron and silicon dioxide, and lithium is changed into lithium vapor at high temperature;
⑧ condensing the lithium vapor to obtain solid lithium with purity up to 99%.
The pure heat source in step ③ is formed by burning natural gas, coal gas, acetylene gas, fuel oil, electricity or alcohol.
The impure heat source in step ③ is a heat source formed by burning pulverized coal, lignite, or firewood.
Example 1:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3) Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes respectively according to the weight ratio of 0.8 to 0.819 to 0.256, and uniformly mixing the powdery lithium carbonate with the powdery quicklime;
② making the above powder mixture into powder with particle diameter n of 10mm and specific gravity of 1.6g/cm3The solid particles of (4);
③ calcining the solid particles obtained in the previous step at 900 ℃ in a rotary kiln until all lithium carbonate in the particles is decomposed and all carbon dioxide contained in the particles is discharged, and keeping the obtained calcined solid particles for later use;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) in a weight ratio of 0.9: 0.193, respectively, and mixing the powder with ferrosilicon powder containing 75% silicon and having a particle size of 65 mesh;
⑥ making the above powder mixture into powder with particle diameter n of 10mm and specific gravity of 1.8g/cm3The solid particles of (4);
⑦ performing reduction reaction on the solid particles prepared in the previous step in a vacuum electric furnace at 1500 ℃ and a vacuum degree P of less than or equal to 30Pa to generate lithium vapor;
⑧ condensing the lithium vapor to obtain solid lithium.
Example 2:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3)＝0.925∶0.8245∶Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes according to the weight ratio of 0.258 respectively, and uniformly mixing the powdery lithium carbonate with the powdery quicklime;
② making the above powder mixture into powder with particle diameter n of 15mm and specific gravity of 1.8g/cm3The solid particles of (4);
③ calcining the solid particles obtained in the previous step at 1000 deg.C in a rotary kiln until all lithium carbonate in the particles is decomposed and all carbon dioxide contained in the particles is exhausted, and keeping the obtained calcined solid particles for later use;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) 1.05: 0.2015 in weight ratio, respectively, and mixing the powder with ferrosilicon powder containing 80% silicon and 97.5 mesh;
⑥ making the above powder mixture into powder with particle diameter n of 15mm and specific gravity of 1.9g/cm3The solid particles of (4);
⑦ performing reduction reaction on the solid particles prepared in the previous step in a vacuum electric furnace at 1550 ℃ and under the condition that the vacuum degree P is less than or equal to 30Pa to generate lithium vapor;
⑧ condensing the lithium vapor to obtain solid lithium.
Example 3:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3) Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes according to the weight ratio of 1.05 to 0.83 to 0.26, and uniformly mixing the powdery lithium carbonate with the powdery quicklime;
② making the above powder mixture into powder with particle diameter n of 20mm and specific gravity of 2g/cm3The solid particles of (4);
③ calcining the solid particles obtained in the previous step at 1100 deg.C in a rotary kiln until all lithium carbonate in the particles is decomposed and all carbon dioxide contained in the particles is exhausted, and keeping the obtained calcined solid particles for later use;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) 1.2: 0.21 at a weight ratio of 85% silicon content and 130 mesh ferrosilicon, and mixing them;
⑥ making the above powder mixture into powder with particle diameter n of 20mm and specific gravity of 2g/cm3The solid particles of (4);
⑦ performing reduction reaction on the solid particles prepared in the previous step in a vacuum electric furnace at 1600 ℃ and under the condition that the vacuum degree P is less than or equal to 30Pa to generate lithium vapor;
⑧ condensing the lithium vapor to obtain solid lithium.
Example 4:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3) Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes according to the weight ratio of 0.925 to 0.8245 to 0.258, and uniformly mixing the powdery lithium carbonate with the powdery quicklime;
② making the above powder mixture into powder with particle diameter n of 15mm and specific gravity of 1.8g/cm3The solid particles of (4);
③ calcining the solid particles obtained in the previous step at 1000 deg.C in a rotary kiln until all lithium carbonate in the particles is decomposed and all carbon dioxide contained in the particles is exhausted, and keeping the obtained calcined solid particles for later use;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) 1.05: 0.2015 in weight ratio, respectively, and mixing the powder with ferrosilicon powder containing 80% silicon and 97.5 mesh;
⑥ making the above powder mixture into powder with particle diameter n of 15mm and specific gravity of 1.9g/cm3The solid particles of (4);
⑦ performing reduction reaction on the solid particles prepared in the previous step in a vacuum electric furnace at 1550 ℃ and under the condition that the vacuum degree P is less than or equal to 30Pa to generate lithium vapor;
⑧ condensing the lithium vapor to obtain solid lithium;
⑨ vacuum packaging the solid lithium ingot.
The reaction equations of the present invention at steps ③ and ⑦ are as follows:
Claims (3)
1. a method for preparing lithium by using lithium carbonate is characterized by comprising the following steps:
① lithium carbonate (Li)2CO3) Calcium lime (CaO) and alumina (Al)2O3) Weighing powdery lithium carbonate with the purity of more than 99 percent and the granularity of less than 65 meshes, powdery quicklime with the purity of more than 96 percent and the granularity of less than 80 meshes and powdery alumina with the purity of more than 98 percent and the granularity of less than 65 meshes according to the weight ratio of 0.8-1.05: 0.819-0.83: 0.256-0.26, and uniformly mixing the powdery lithium carbonate with the powdery quicklime with the purity of more than 96 percent and the granularity of less than 65 meshes;
② making the powder mixture into powder with particle size n of 10 mm-20 mm and specific gravityIs 1.6-2g/cm3The solid particles of (4);
③ calcining the solid particles at 900-1100 deg.C until the lithium carbonate is decomposed completely and the carbon dioxide is exhausted completely, and keeping the solid particles after calcining;
④ pulverizing the calcined solid particles obtained in the previous step into powder with a particle size of less than 100 meshes for later use;
⑤ weighing the powder obtained in the above step and ferrosilicon (Si (Fe)) in a weight ratio of 0.9-1.2: 0.193-0.21, respectively, and mixing the powder and ferrosilicon powder with silicon content of 75-85% and particle size of 65-130 meshes;
⑥ making the powder mixture into powder with particle size n of 10 mm-20 mm and specific gravity of 1.8-2g/cm3The solid particles of (4);
⑦ performing reduction reaction on the solid particles obtained in the previous step at 1500-1600 ℃ and vacuum degree P less than or equal to 30Pa to generate lithium vapor;
⑧ condensing the lithium vapor to obtain solid lithium.
2. The method of claim 1, wherein the pure heat source in step ③ is natural gas, coal gas, acetylene gas, fuel oil, electricity or alcohol.
3. The method of claim 1, wherein the impure heat source in step ③ is a heat source generated by burning pulverized coal, lignite or firewood.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03145557 CN1213158C (en) | 2003-07-02 | 2003-07-02 | Lithium preparing process with lithium carbonate |
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| CN 03145557 CN1213158C (en) | 2003-07-02 | 2003-07-02 | Lithium preparing process with lithium carbonate |
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| CN1487104A true CN1487104A (en) | 2004-04-07 |
| CN1213158C CN1213158C (en) | 2005-08-03 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101642815A (en) * | 2009-09-04 | 2010-02-10 | 黄启新 | Method for preparing metal lithium at high temperature employing the electrical conductivity of molten slag |
| US8643930B2 (en) | 2007-08-31 | 2014-02-04 | Alliance For Sustainable Energy, Llc | Thin film lithium-based batteries and electrochromic devices fabricated with nanocomposite electrode materials |
| CN104178645A (en) * | 2014-08-19 | 2014-12-03 | 北京神雾环境能源科技集团股份有限公司 | Method for preparing metallic lithium |
| CN113526474A (en) * | 2020-12-31 | 2021-10-22 | 深圳市研一新材料有限责任公司 | Lithium nitride particles, and method and apparatus for producing same |
-
2003
- 2003-07-02 CN CN 03145557 patent/CN1213158C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8643930B2 (en) | 2007-08-31 | 2014-02-04 | Alliance For Sustainable Energy, Llc | Thin film lithium-based batteries and electrochromic devices fabricated with nanocomposite electrode materials |
| CN101642815A (en) * | 2009-09-04 | 2010-02-10 | 黄启新 | Method for preparing metal lithium at high temperature employing the electrical conductivity of molten slag |
| CN104178645A (en) * | 2014-08-19 | 2014-12-03 | 北京神雾环境能源科技集团股份有限公司 | Method for preparing metallic lithium |
| CN104178645B (en) * | 2014-08-19 | 2017-03-01 | 北京神雾环境能源科技集团股份有限公司 | The method preparing lithium metal |
| CN113526474A (en) * | 2020-12-31 | 2021-10-22 | 深圳市研一新材料有限责任公司 | Lithium nitride particles, and method and apparatus for producing same |
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| CN1213158C (en) | 2005-08-03 |
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