CN110885090A - Method for preparing battery-grade lithium carbonate by using lepidolite as raw material through one-step method - Google Patents
Method for preparing battery-grade lithium carbonate by using lepidolite as raw material through one-step method Download PDFInfo
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention provides a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method, which is characterized in that the lepidolite is used as the raw material and auxiliary materials to be mixed, and then the raw material and the auxiliary materials are mixed and roasted in a rotary kiln device to extract lithium. And the process for extracting lithium by using chloride roasting has less influence on the environment, improves the recovery rate of lithium, has stable process and easy operation, and is beneficial to realizing industrial production.
Description
The technical field is as follows:
the invention relates to a method for extracting high-purity lithium carbonate from a lepidolite raw material, in particular to a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method.
Background art:
lithium carbonate is an important chemical raw material and an important raw material for manufacturing a new energy lithium battery. With the emergence of the national new energy development plan, the lithium battery new energy becomes one of the energy industries which are key in national support development; the lithium carbonate of the sulfur battery is used as an important basic raw material for the development of new energy of the lithium battery, the demand of the lithium carbonate is increasingly large, and the price of the lithium carbonate is increasingly high.
In the prior art, lithium ores are generally adopted to prepare lithium salts to prepare lepidolite raw material powder, and the technological method for extracting lithium by roasting in a rotary kiln is more. When the process method is used for extracting the lithium carbonate, the solid-to-solid ratio of the roasting material leaching solution is relatively small, the content of lithium ions in the leaching solution is usually lower, and is only a few grams/liter, and the concentration is lower. The solid-to-solid ratio of the roasting material leaching solution is relatively small, the corresponding stirring strength requirement is high, but the requirement is difficult to be met by a conventional stirrer, so that the lithium extraction yield is low. On the other hand, the single calcination mode and the stirring and mixing method for the extract have great influence on the lithium extraction yield of the lepidolite preparation. For example, chinese patent application 201811411885.9 discloses a method for extracting lithium salt from lithium ore, which is a technical scheme of extracting lithium salt by using a chloride system, wherein a chloride system roasting process is used when acid leaching extraction and other processes are performed on lepidolite, and when a chloride system is used for roasting and extracting lithium, the corrosion of equipment and facilities used in the lithium extraction process is relatively high, so that the corrosion prevention requirements on the equipment and related devices are high when the technical scheme is used, and the influence on the environment is relatively large. The lithium prepared by the process has low yield and large equipment investment, so the production cost is high and the benefit of industrial production is poor.
In addition, when the lithium carbonate is prepared by using lepidolite as a raw material, a battery-grade lithium carbonate product is usually extracted through a process of firstly producing industrial-grade lithium carbonate and then through a corresponding refining process, but cannot be prepared through direct precipitation in a one-step method.
Therefore, how to provide a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material in one step method is not required to be a process for producing industrial-grade lithium carbonate, but is directly precipitated to prepare a battery-grade lithium carbonate product. And the process of roasting and extracting lithium by using the chloride system has less influence on the environment, namely, a crude product of lithium carbonate is prepared, and the crude product is centrifugally separated, washed and dried to obtain the finished product of battery-grade lithium carbonate. And the roasting process method and the related auxiliary material composition are not involved. And the method improves the recovery rate of lithium, has large yield, low energy consumption, low production cost, stable process, easy operation and control.
The invention content is as follows:
the invention aims to provide a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method, which is characterized in that after the lepidolite is used as the raw material and is mixed with auxiliary materials, the raw material and the auxiliary materials are mixed and then roasted in a rotary kiln device to extract lithium, and the method comprises the steps of crushing lepidolite concentrate powder, mixing and proportioning, roasting, leaching and extracting lithium, removing impurities, precipitating lithium to prepare battery-grade lithium carbonate and the like, and does not need a process for producing industrial-grade lithium carbonate, but directly precipitates to prepare a battery-grade lithium carbonate product. And the process for extracting lithium by using chloride roasting has less influence on the environment, improves the recovery rate of lithium, has stable process and easy operation, and is beneficial to realizing industrial production.
The invention 1 discloses a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method, which is characterized in that the lepidolite is used as a raw material and is mixed with auxiliary materials, and then the raw material and the auxiliary materials are mixed and roasted in a rotary kiln device to extract lithium, and comprises the following steps:
1) crushing to prepare lepidolite concentrate powder: crushing lepidolite by a crushing device, removing weak magnetic iron minerals by a high-gradient magnetic separator, and sieving by a sieve with more than 100 meshes to obtain lepidolite concentrate powder;
2) and mixing ingredients: fully mixing lepidolite concentrate powder with composite salt to obtain a lepidolite mixture, wherein the composite salt is inorganic salt consisting of anionic non-chloride ions;
3) and roasting: placing the lepidolite mixture in a rotary kiln device, drying at low temperature, and then calcining at high temperature, wherein the calcined material is called as calcined clinker or calcined material for short;
4) leaching and extracting lithium: mixing the roasted material and water or dilute sulfuric acid solution to obtain a solid-liquid mixed solution, soaking, controlling the soaking time to be 2-3 hours, and controlling the solid-liquid mass ratio to be 1: 1.5-2, filtering to remove residues, washing filter residues with water, and recycling the washing liquid to obtain a leaching solution;
5) and removing impurities from the leaching solution: selectively removing impurities from the leachate obtained in the step 4) to obtain a refined lithium solution;
6) and (3) carbonizing and precipitating lithium: filling high-purity carbon dioxide gas into the refined lithium solution with the adjusted pH value, and washing and filtering to obtain a battery-grade lithium carbonate product and a lithium precipitation mother solution;
7) recovery of potassium sodium rubidium cesium salt: concentrating, cooling, crystallizing, drying and the like the lithium precipitation mother liquor, recovering potassium sodium salt, returning to recycle, and feeding the liquor after recovering potassium sodium salt into a rubidium-cesium extraction system to recover rubidium-cesium salt.
2. The method for preparing battery grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1, wherein the magnetic field intensity on the surface of the magnetic pole of the high-gradient magnetic separator in the step 1) is controlled to be H less than or equal to 1800A/m.
3. The method for preparing battery-grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1, wherein the compound salt in the step 2) is one or a mixed salt of more than two of lithium sulfate, sodium sulfate, calcium sulfate, magnesium sulfate, ferric sulfate, calcium carbonate, sodium carbonate and potassium carbonate. The preferable composition is one or more of sodium sulfate, potassium sulfate, calcium sulfate, sodium carbonate and calcium carbonate.
4. The method for preparing the battery-grade lithium carbonate by using the lepidolite as the raw material in one step according to claim 1, wherein the low temperature and the high temperature in the step 3) are respectively controlled to be not more than 250 ℃ and not more than 940 ℃, and the calcination time is controlled to be 0.2 to 1 hour.
5. The method for preparing battery grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1 or 3, wherein the adding amount of the composite salt is controlled to be 25-80 wt% of the mass of the lepidolite concentrate powder.
6. The method for preparing battery grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1, wherein in the step 3) when the calcine is subjected to high-temperature calcination in a rotary kiln device, a high-temperature calcination additive is added into the rotary kiln device, wherein the high-temperature calcination additive is calcium carbonate gangue with the particle size of less than or equal to 1mm, and the amount of the high-temperature calcination additive is controlled to be 0.5-3.0wt% of the mass of the calcine.
The main production process steps of the invention are as follows: lepidolite concentrate powder → batching → roasting → clinker → leaching solution → selective impurity removal → refined lithium liquid → slag discharge → carbonization lithium precipitation → lithium precipitation mother liquid → potassium sodium recovery → concentrated mother liquid → battery grade lithium carbonate product.
1. The invention provides a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method. The extracted lithium salt and lithium carbonate can be directly applied to the synthesis of the anode and cathode materials and the electrolyte of the lithium battery; the lepidolite adopts a composite salt method fluorine-fixing roasting transformation technology, and solves the problems of high requirements on corrosion resistance of equipment and facilities and great influence on environment in the roasting process of a chloride system. Meanwhile, the recovery rate is improved, and the production cost is reduced. The recovery rate of lithium is high, the comprehensive recovery rate of lithium is more than 83%, the energy consumption is low, the process is stable, the operation and the control are easy, and the cyclic utilization of byproducts and wastewater can be realized; is a production method with small influence on the environment.
The ratio of the raw material consumption of lepidolite to the product cost (based on the current price of the product) using lepidolite as the raw material and adopting different process technologies is shown in table 1
Description of the drawings: the production cost of the battery-grade lithium carbonate product prepared by the one-step method is lower, and the purity of the product is higher and reaches 99.72%.
By using the method of the invention and using lepidolite concentrate powder as raw material, the index of lithium recovery rate is shown in table 2,
| the lithium yield% | 83.57 |
| The leached slag contains lithium% | 0.13 |
The extraction rate of rare metals in the lepidolite was 83% or more.
The lithium carbonate produced by the method has the purity of over 99.7 percent through detection, the technical indexes are shown in table 3,
description of the drawings: the metal elements in table 3 each represent an ion content.
The specific implementation mode is as follows:
the concentrations referred to in the examples are mass concentrations.
The invention relates to a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method, which is used for extracting lithium by adopting a method of mixing the lepidolite as the raw material and auxiliary materials and then roasting the mixture in a rotary kiln device, and comprises the following steps:
1) crushing lepidolite to prepare lepidolite concentrate powder, crushing lepidolite by using a crushing device, then carrying out magnetic separation on the magnetic pole surface of a high-gradient magnetic separator until the magnetic field intensity is less than or equal to 1800A/m to remove main impurities, namely weak magnetic iron minerals, and then sieving the lepidolite concentrate powder by using a sieve with more than 100 meshes to obtain the lepidolite concentrate powder;
2) mixing ingredients, namely fully mixing the lepidolite concentrate powder with a composite salt to obtain a lepidolite mixture, wherein the composite salt is one or more than two of lithium sulfate, sodium sulfate, calcium sulfate, magnesium sulfate, ferric sulfate, calcium carbonate, sodium carbonate and potassium carbonate; the preferable composition of the compound salt is one or a mixture of more of sodium sulfate, potassium sulfate, calcium sulfate, sodium carbonate and calcium carbonate; controlling the adding amount of the composite salt to be 25-80 wt% of the mass of the lepidolite concentrate powder; the addition amount is preferably controlled to be 40-60%;
3) roasting, namely placing the lepidolite mixture in a rotary kiln device, drying at a low temperature, and then calcining at a high temperature to obtain a roasted material; namely, the low-temperature calcination temperature is controlled not to exceed 250 ℃, the low-temperature calcination time is controlled between 30 minutes and 1 hour, the high-temperature calcination temperature is controlled between 800 ℃ and 940 ℃, and the calcination time is controlled between 0.2 and 1 hour; in order to improve the roasting efficiency, when the roasted sand material is subjected to high-temperature roasting in a rotary kiln device, adding a high-temperature roasting additive into the rotary kiln device, wherein the high-temperature roasting additive is calcium carbonate powder with the granularity of less than or equal to 1mm, generally adding the calcium carbonate powder with the particle size of 0.5 mm, and simultaneously controlling the amount of the high-temperature roasting additive to be 0.5-3 wt% of the mass of the roasted sand material; preferably 1.5 wt% is added;
4) leaching and extracting lithium, mixing the roasted material and water or a dilute sulfuric acid solution to form a solid-liquid mixed solution, soaking, and controlling the mass concentration of the added dilute sulfuric acid to be 15-35% of the dilute sulfuric acid solution, preferably 20% of the dilute sulfuric acid solution; controlling the dipping time to be 2-3 hours, and controlling the solid-liquid mass ratio to be 1: 1.5-2, filtering to remove residues, washing filter residues with water, and recycling the washing liquid to obtain a leaching solution;
5) and removing impurities from the leaching solution: selectively removing impurities from the leachate obtained in the step 4) to obtain a refined lithium solution;
6) and (3) carbonizing and precipitating lithium: charging high-purity carbon dioxide gas into the refined lithium solution after the pH value is adjusted, and washing and filtering to obtain a battery-grade lithium carbonate product and a lithium precipitation mother solution;
7) recovery of potassium sodium rubidium cesium salt: concentrating, cooling, crystallizing, drying and the like the lithium precipitation mother liquor, recovering potassium sodium salt, returning to recycle, and feeding the liquor after recovering potassium sodium salt into a rubidium-cesium extraction system to recover rubidium-cesium salt.
The lithium yield is high, and the comprehensive lithium yield is more than 83 percent. The purity of the battery-grade lithium carbonate produced by the one-step method reaches 99.7 percent, the energy consumption can be saved by 30 percent, and the operation is easy.
Example 1
The lepidolite raw material produced by tantalum-niobium lithium ore in Yichun is taken, the main chemical components of the lepidolite raw material are as shown in the following table (wt%), and the balance is fluorine,
| Li2O | K2O | Na2O | AL2O3 | SiO2 | Fe2O3 | Rb2O | Cs2O |
| 4.32 | 7.51 | 0.46 | 23.8 | 54.32％ | 0.38 | 1.66 | 0.28 |
1) crushing the lepidolite raw material by using a crushing device, removing weak magnetic iron minerals by using a high-gradient magnetic separator, and sieving by using a sieve with more than 100 meshes to obtain lepidolite concentrate powder;
2) mixing ingredients, namely fully mixing lepidolite concentrate powder with compound salt potassium sulfate and sodium sulfate, controlling the adding amount of the potassium sulfate and the sodium sulfate to be 45% of the mass of the lepidolite concentrate powder, wherein the ratio of the potassium sulfate to the sodium sulfate respectively accounts for fifty percent, and thus obtaining a lepidolite mixture;
3) roasting, namely placing the lepidolite mixture in a rotary kiln device, drying at a low temperature, and then calcining at a high temperature to obtain a roasted material; in the roasting process of the embodiment, a plasma generator device can be used for roasting, namely, the lepidolite mixture is placed in the plasma generator for heating reaction, and the reaction temperature is controlled to be 800-940 ℃, so that a roasted material is obtained;
4) leaching and extracting lithium, mixing the roasted material and water or dilute sulfuric acid solution to form solid-liquid mixed solution, preferably using dilute sulfuric acid with the mass concentration of 5-10 wt%, and soaking for 2-3 hours, wherein the solid-liquid mass ratio is controlled to be 1: 1.5-2, filtering to remove residues, washing filter residues with water, and recycling the washing liquid to obtain a leaching solution; or the following process can be adopted for leaching and extracting lithium, when the leaching treatment is carried out, the pressure and the heating are carried out to the temperature of 90 ℃ to below 100 ℃, meanwhile, the pressure is increased, the reaction pressure is controlled to be about 1.5 atmospheric pressures, the stirring is carried out to fully react, the reaction time is generally controlled to be 1-1.5 hours, and the leaching solution is obtained;
5) removing impurities from the leachate, and selectively removing impurities from the leachate obtained in the step 4) to obtain a refined lithium solution;
6) and (3) carbonizing and precipitating lithium: filling high-purity carbon dioxide gas into the refined lithium solution with the adjusted pH value, and washing and filtering to obtain a battery-grade lithium carbonate product and a lithium precipitation mother solution;
7) recovery of potassium sodium rubidium cesium salt: concentrating, cooling, crystallizing, drying and the like the lithium precipitation mother liquor, recovering potassium sodium salt, returning to recycle, and feeding the liquor after recovering potassium sodium salt into a rubidium-cesium extraction system to recover rubidium-cesium salt.
Claims (6)
1. A method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through a one-step method is characterized in that the lepidolite is used as a raw material and is mixed with auxiliary materials, and lithium is extracted by adopting a method of mixing the raw material and the auxiliary materials and then roasting in a rotary kiln device, and comprises the following steps:
1) crushing lepidolite concentrate powder, crushing lepidolite by using a crushing device, removing weak magnetic iron minerals by using a high-gradient magnetic separator, and sieving by using a sieve with more than 100 meshes to obtain lepidolite concentrate powder;
2) mixing ingredients, namely fully mixing the lepidolite concentrate powder with composite salt to obtain a lepidolite mixture, wherein the composite salt is inorganic salt consisting of anionic non-chloride ions;
3) and roasting: placing the lepidolite mixture in a rotary kiln device, drying at low temperature, then calcining at high temperature, and roasting the roasted material;
4) leaching and extracting lithium, mixing the roasted material and water or dilute sulfuric acid solution to form solid-liquid mixed solution, soaking, controlling the soaking time to be 2-3 hours, and controlling the solid-liquid mass ratio to be 1: 1.5-2, filtering to remove residues, washing filter residues with water, and recycling the washing liquid to obtain a leaching solution;
5) removing impurities from the leachate, and selectively removing impurities from the leachate obtained in the step 4) to obtain a refined lithium solution;
6) and (3) carbonizing and precipitating lithium: charging high-purity carbon dioxide gas into the refined lithium solution after the pH value is adjusted, and washing and filtering to obtain a battery-grade lithium carbonate product and a lithium precipitation mother solution;
7) recovery of potassium sodium rubidium cesium salt: concentrating, cooling, crystallizing and drying the lithium precipitation mother liquor, recovering potassium sodium salt, returning to recycle, and feeding the solution after recovering potassium sodium salt into a rubidium-cesium extraction system to recover rubidium-cesium salt.
2. The method for preparing battery grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1, wherein the magnetic field intensity on the surface of the magnetic pole of the high-gradient magnetic separator in the step 1) is controlled to be H less than or equal to 1800A/m.
3. The method for preparing battery-grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1, wherein the compound salt in the step 2) is one or a mixed salt of more than two of lithium sulfate, sodium sulfate, calcium sulfate, magnesium sulfate, ferric sulfate, calcium carbonate, sodium carbonate and potassium carbonate.
4. The method for preparing the battery-grade lithium carbonate by using the lepidolite as the raw material in one step according to claim 1, wherein in the step 3), the low temperature and the high temperature are respectively controlled to be not more than 250 ℃ and more than 940 ℃, and the calcination time is controlled to be 0.2 to 1 hour.
5. The method for preparing battery grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1 or 3, wherein the adding amount of the composite salt is controlled to be 25-80 wt% of the mass of the lepidolite concentrate powder.
6. The method for preparing battery grade lithium carbonate by using lepidolite as a raw material in one step according to claim 1, wherein in the step 3) when the calcine is subjected to high-temperature calcination in a rotary kiln device, a high-temperature calcination additive is added into the rotary kiln device, wherein the high-temperature calcination additive is calcium carbonate powder with the particle size of less than or equal to 1mm, and the amount of the high-temperature calcination additive is controlled to be 0.5-3.0wt% of the mass of the calcine.
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| CN111498873A (en) * | 2020-04-21 | 2020-08-07 | 华南理工大学 | Carbonate roasting method and system for extracting lithium carbonate from lepidolite |
| CN112142080A (en) * | 2020-09-28 | 2020-12-29 | 江西永兴特钢新能源科技有限公司 | Method for preparing battery-grade lithium carbonate by freezing, circulating and recycling lithium precipitation concentrated mother solution |
| CN112176185A (en) * | 2020-09-28 | 2021-01-05 | 江西永兴特钢新能源科技有限公司 | Method for removing fluorine from lepidolite roasting leaching solution |
| CN112374512A (en) * | 2020-11-12 | 2021-02-19 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by removing impurities from lepidolite clinker |
| CN112624161A (en) * | 2020-12-31 | 2021-04-09 | 江西南氏锂电新材料有限公司 | Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite |
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| CN111498873A (en) * | 2020-04-21 | 2020-08-07 | 华南理工大学 | Carbonate roasting method and system for extracting lithium carbonate from lepidolite |
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| CN112142080A (en) * | 2020-09-28 | 2020-12-29 | 江西永兴特钢新能源科技有限公司 | Method for preparing battery-grade lithium carbonate by freezing, circulating and recycling lithium precipitation concentrated mother solution |
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