CN112624161B - Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite - Google Patents
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Abstract
The invention discloses a method for preparing battery-grade lithium carbonate by taking lepidolite as a raw material, which comprises the steps of crushing the 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; weighing lepidolite concentrate powder and oxalic acid according to the mass ratio of 3-6, adding the mixture into a ball mill, ball-milling and mixing for 24-48h to obtain precursor powder, and adding the precursor powder into a rotary kiln, and roasting at 600-800 ℃ for 0.5-2h to obtain a roasted material; concentrated sulfuric acid and a roasting material are adopted to carry out solid phase reaction at a medium-low temperature, and then water is used for leaching and dissolving alkali sulfate; continuously inducing crystallization and removing impurities by adding different crystallization inducers; and finally, reacting the obtained lithium hydroxide solution with carbon dioxide to prepare the battery-grade lithium carbonate. The lepidolite mineral powder and oxalic acid are mechanically activated and then roasted, the oxalic acid plays a role in catalytic activation in the roasting process, then concentrated sulfuric acid is used for mechanical mixing and leaching, and then crystallization and impurity removal are carried out to obtain the lithium carbonate.
Description
Technical Field
The invention relates to the technical field of non-ferrous metal smelting, in particular to a method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite.
Background
Lepidolite is an important mineral resource and has a chemical composition of K { Li2-xAl1+x[Al2xSi4-2xO10](OH,F)2(x = 0-0.5), which is a potassium and lithium-based aluminosilicate, one of mica minerals, which is rich in rare metal materials, lithium, potassium, rubidium, cesium, aluminum, and the like. With the increasing shortage of world energy, the development and utilization of new energy are common problems in the world and are more and more emphasized by various countries; lithium and its salts such as lithium carbonate and lithium sulfate areSince lepidolite contains lithium metal, which is a basic material of the lithium new energy industry, the development and application of the lepidolite are a popular problem at present.
The lithium tantalum-niobium ore in Yichun, jiangxi is the largest lithium tantalum-niobium ore in Asia at present, the lithium tantalum-niobium ore is rich in resources, the content of lithium dioxide in lepidolite reaches 4.5%, and the method has the advantage condition of extracting lithium carbonate resources. Therefore, the method for extracting lithium carbonate by using lepidolite as a raw material has a wide market prospect and good economic benefit.
From the existing production process, the production yield of lithium carbonate is not ideal, the comprehensive production benefit is not high, the input-output ratio is insufficient, and the industrial production is difficult to realize. The existing method for preparing lithium carbonate by using lepidolite as a raw material mainly comprises a sulfuric acid method or a potassium sulfate calcination method, wherein the potassium sulfate consumption is too high, the energy consumption is high, the material flow flux is large, and the lithium recovery rate is low, so that the product cost for preparing lithium carbonate and lithium sulfate is too high.
In addition, when the existing lithium carbonate is prepared by taking lepidolite as a raw material, the process of firstly producing industrial-grade lithium carbonate is generally carried out, and then a battery-grade lithium carbonate product is extracted through a corresponding refining process, but the battery-grade lithium carbonate product cannot be prepared through direct precipitation in a one-step method.
Patent CN201911421655.5 previously filed by the applicant discloses a method for preparing battery-grade lithium carbonate by using lepidolite as a raw material through one-step method, which is characterized in that 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 are roasted in a rotary kiln device, the roasted material and water or dilute sulfuric acid solution are mixed to form a solid-liquid mixed solution, the impregnation is carried out, the impregnation time is controlled to be 2-3 hours, and 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; selectively removing impurities from the leachate to obtain a refined lithium solution; 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; 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 method introduces the compound salt and needs a more complex impurity removal process. In the traditional process for extracting lithium by roasting lepidolite, the lepidolite is roasted together with auxiliary materials such as calcium sulfate, limestone and the like.
Disclosure of Invention
The invention aims to provide a method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite comprises the following steps:
s1, crushing lepidolite through a crushing device, removing weak magnetic iron minerals through a high-gradient magnetic separator, and sieving through a sieve with more than 100 meshes to obtain lepidolite concentrate powder; weighing lepidolite concentrate powder and oxalic acid according to a mass ratio of 3-6;
s2, adding concentrated sulfuric acid and the roasting material into grinding equipment together for mechanical grinding, carrying out solid-phase reaction in the mixing process, transferring the mixture after mechanical grinding into an extraction tank, adding water, soaking, leaching and dissolving alkali sulfate salt, and filtering and separating to obtain a leaching solution;
s3, separating out aluminum sulfate rubidium cesium alum salt and aluminum sulfate potassium alum salt at different temperature ranges by adopting a method of adding different crystallization inducers to continuously induce crystallization and impurity removal;
s4, neutralizing, crystallizing and removing impurities by adopting potassium hydroxide to obtain aluminum hydroxide and potassium sulfate, using the aluminum hydroxide to neutralize excessive sulfuric acid, and supplementing the potassium sulfate to obtain aluminum sulfate potassium alum salt;
and S5, finally reacting the obtained lithium hydroxide solution with carbon dioxide to prepare the battery-grade lithium carbonate.
In the step S2, the mass ratio of concentrated sulfuric acid to the roasting material is 1:1-6.
In the step S3, the crystallization temperature of aluminum sulfate rubidium alum salt and aluminum sulfate cesium alum salt is controlled to be 55-65 ℃, and the crystallization temperature of aluminum potassium sulfate is controlled to be 5-15 ℃.
Step S4, adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and a filtrate C; cooling the filtrate C to 5-15 ℃, adding a crystallization inducer into the filtrate C, crystallizing to obtain potassium sulfate, and filtering to obtain a filtrate D; and (3) using aluminum hydroxide to neutralize excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain aluminum sulfate potassium alum salt, and filtering to obtain filtrate E, namely the lithium hydroxide solution.
Specifically, the crystallization inducer of the present invention is a precipitating substance that can be present in current systems from 500nm to 5um, preferably a homoacidic precipitating substance.
The invention has the beneficial effects that: the lepidolite mineral powder and oxalic acid are mechanically activated and then roasted, and the oxalic acid plays a role in catalytic activation in the roasting process, so that the subsequent leaching is facilitated, and the leaching rate is improved. Different crystallization inducers are added to continuously induce crystallization and impurity removal, and aluminum sulfate cesium alum salt, aluminum sulfate potassium alum salt and the like are respectively precipitated in different temperature ranges. The potassium hydroxide is adopted for neutralization, crystallization and impurity removal, the obtained byproducts such as the aluminum hydroxide and the potassium sulfate can be recycled in a green way, the aluminum hydroxide is used for neutralizing excessive sulfuric acid, the potassium sulfate is supplemented to obtain aluminum sulfate potassium alum salt, the consumption of alkali such as the potassium hydroxide required in the neutralization process can be reduced, energy conservation and emission reduction are realized, the aluminum sulfate potassium alum salt with higher purity can be prepared through the process, and the comprehensive utilization of aluminum, potassium and sulfate radicals in the lepidolite is realized.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
A method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite comprises the following steps:
s1, crushing lepidolite through a crushing device, removing weak magnetic iron minerals through a high-gradient magnetic separator, and sieving through a sieve with more than 100 meshes to obtain lepidolite concentrate powder; weighing lepidolite concentrate powder and oxalic acid according to the mass ratio of 3-6, adding the mixture into a ball mill, ball-milling and mixing for 24-48h to obtain precursor powder, and adding the precursor powder into a rotary kiln, and roasting at 600-800 ℃ for 0.5-2h to obtain a roasted material;
s2, adding concentrated sulfuric acid and the roasting material together according to a mass ratio of 1:1-6, adding the mixture into grinding equipment, mechanically grinding the mixture for 24-72 hours, performing solid-phase reaction in the mixing process, transferring the mechanically ground mixture of lithium mica powder and concentrated sulfuric acid into an extraction cylinder, adding water with the mass of 3-10 times that of the mixture, soaking the mixture for 24-96 hours, leaching and dissolving alkali sulfate salt, and filtering and separating the mixture to obtain leachate, wherein the leachate mainly contains potassium salt, aluminum salt, lithium salt, rubidium salt and cesium salt;
s3, controlling the temperature of the leaching solution at 55-65 ℃, adding an aluminum rubidium sulfate and aluminum cesium sulfate crystallization inducer, separating out aluminum rubidium sulfate alum salt and aluminum cesium sulfate alum salt, and filtering to obtain filtrate A; cooling the filtrate A to 5-15 ℃, adding a potassium aluminum sulfate crystallization inducer to separate out potassium aluminum sulfate salt, and filtering to obtain a filtrate B, wherein the crystallization inducer is a precipitate with the particle size of 500nm to-5 um;
s4, adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and a filtrate C; cooling the filtrate C to 5-15 deg.C, adding crystallization inducer which is potassium sulfate particle or insoluble precipitate under the condition, the particle size is 500 nm-5 um, crystallizing to obtain potassium sulfate, and filtering to obtain filtrate D; using aluminum hydroxide to neutralize excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain potassium aluminum sulfate alum salt, and filtering to obtain filtrate E, namely lithium hydroxide solution;
and S5, finally reacting the obtained lithium hydroxide solution with carbon dioxide to prepare the battery-grade lithium carbonate.
Example 1
Crushing lepidolite by a crushing device, then 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; mixing lepidolite concentrate powder and oxalic acid according to a mass ratio of 3:1, adding the mixture into a ball mill, ball-milling and mixing for 24 hours to obtain precursor powder, and adding the precursor powder into a rotary kiln, and roasting for 0.5 hour at 800 ℃ to obtain a roasted material; adding 100g of concentrated sulfuric acid and 100g of roasting material into a ball milling tank for mechanical grinding for 24 hours, carrying out solid-phase reaction in the mixing process, transferring the mechanically ground lithium mica powder-concentrated sulfuric acid mixture into an extraction tank, adding 2000g of water, soaking for 24 hours, leaching and dissolving alkali metal sulfate, filtering and separating to obtain a leachate, wherein the leachate mainly contains potassium salt, aluminum salt, lithium salt, rubidium salt and cesium salt; controlling the temperature of the leaching solution at 65 ℃, adding aluminum rubidium sulfate crystals serving as seed crystals serving as crystallization inducers, separating out aluminum rubidium sulfate alum salt and aluminum cesium sulfate alum salt, and filtering to obtain filtrate A; cooling the filtrate A to 15 ℃, adding an aluminum potassium sulfate crystallization inducer to separate out potassium aluminum sulfate salt, and filtering to obtain filtrate B; adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and filtrate C; cooling the filtrate C to 15 ℃, adding a crystallization inducer into the filtrate C, crystallizing to obtain potassium sulfate, and filtering to obtain a filtrate D; using aluminum hydroxide to neutralize excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain potassium aluminum sulfate alum salt, and filtering to obtain filtrate E, namely lithium hydroxide solution; and finally, reacting the obtained lithium hydroxide solution with carbon dioxide to prepare 9.63g of battery-grade lithium carbonate.
Example 2
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; mixing lepidolite concentrate powder with oxalic acid according to a mass ratio of 4:1, adding the mixture into a ball mill, ball-milling and mixing for 24 hours to obtain precursor powder, and adding the precursor powder into a rotary kiln, and roasting for 0.5 hour at 800 ℃ to obtain a roasted material; s1, adding 100g of concentrated sulfuric acid and 200g of roasting material into a ball milling tank for mechanical grinding for 36 hours, carrying out solid-phase reaction in the mixing process, transferring the mechanically ground lithium mica powder-concentrated sulfuric acid mixture into an extraction tank, adding 2000g of water, soaking for 36 hours, leaching and dissolving alkali metal sulfate, filtering and separating to obtain a leachate, wherein the leachate mainly contains potassium salt, aluminum salt, lithium salt, rubidium salt and cesium salt; controlling the temperature of the leaching solution at 60 ℃, adding aluminum rubidium sulfate and aluminum cesium sulfate crystallization inducers to separate out aluminum rubidium sulfate alum salt and aluminum cesium sulfate alum salt, and filtering to obtain filtrate A; cooling the filtrate A to 10 ℃, adding an aluminum potassium sulfate crystallization inducer to separate out potassium aluminum sulfate salt, and filtering to obtain filtrate B; adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and filtrate C; cooling the filtrate C to 10 ℃, adding a crystallization inducer into the filtrate C, crystallizing to obtain potassium sulfate, and filtering to obtain a filtrate D; using aluminum hydroxide to neutralize excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain potassium aluminum sulfate alum salt, and filtering to obtain filtrate E, namely lithium hydroxide solution; and finally, reacting the obtained lithium hydroxide solution with carbon dioxide to prepare 22.08g of battery-grade lithium carbonate.
Example 3
Crushing lepidolite by a crushing device, then 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; mixing lepidolite concentrate powder and oxalic acid according to a mass ratio of 5:1, adding the mixture into a ball mill, ball-milling and mixing for 36 hours to obtain precursor powder, and adding the precursor powder into a rotary kiln, and roasting at 700 ℃ for 1 hour to obtain a roasted material; adding 100g of concentrated sulfuric acid and 400g of roasting material into a ball milling tank for mechanical grinding for 36 hours, carrying out solid-phase reaction in the mixing process, transferring the mechanically ground lithium mica powder-concentrated sulfuric acid mixture into an extraction tank, adding 2000g of water, soaking for 24 hours, leaching and dissolving alkali metal sulfate, filtering and separating to obtain a leachate, wherein the leachate mainly contains potassium salt, aluminum salt, lithium salt, rubidium salt and cesium salt; controlling the temperature of the leaching solution at 55 ℃, adding aluminum rubidium sulfate and aluminum cesium sulfate crystallization inducers to separate out aluminum rubidium sulfate alum salt and aluminum cesium sulfate alum salt, and filtering to obtain filtrate A; cooling the filtrate A to 15 ℃, adding a potassium aluminum sulfate crystallization inducer, separating out potassium aluminum sulfate alum salt, and filtering to obtain a filtrate B; adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and filtrate C; cooling the filtrate C to 15 ℃, adding a crystallization inducer into the filtrate C, crystallizing to obtain potassium sulfate, and filtering to obtain a filtrate D; using aluminum hydroxide for neutralizing excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain potassium aluminum sulfate alum salt, and filtering to obtain filtrate E, namely lithium hydroxide solution; finally, the obtained lithium hydroxide solution was reacted with carbon dioxide to prepare 40.13g of cell-grade lithium carbonate.
Example 4
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; mixing lepidolite concentrate powder and oxalic acid according to a mass ratio of 6:1, adding the mixture into a ball mill, ball-milling and mixing for 48 hours to obtain precursor powder, and adding the precursor powder into a rotary kiln, and roasting for 2 hours at 600 ℃ to obtain a roasted material; adding 100g of concentrated sulfuric acid and 400g of roasted materials into a ball milling tank together, mechanically grinding for 48 hours, carrying out solid-phase reaction in the mixing process, transferring the mechanically ground lithium mica powder-concentrated sulfuric acid mixture into an extraction cylinder, adding 2100g of water, soaking for 24 hours, leaching and dissolving alkali sulfate salt, filtering and separating to obtain a leachate, wherein the leachate mainly contains potassium salt, aluminum salt, lithium salt, rubidium salt and cesium salt; controlling the temperature of the leaching solution at 55 ℃, adding aluminum rubidium sulfate and aluminum cesium sulfate crystallization inducers to separate out aluminum rubidium sulfate alum salt and aluminum cesium sulfate alum salt, and filtering to obtain filtrate A; cooling the filtrate A to 5 ℃, adding a potassium aluminum sulfate crystallization inducer, separating out potassium aluminum sulfate alum salt, and filtering to obtain a filtrate B; adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and filtrate C; cooling the filtrate C to 5 ℃, adding a crystallization inducer into the filtrate C, crystallizing to obtain potassium sulfate, and filtering to obtain a filtrate D; using aluminum hydroxide for neutralizing excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain potassium aluminum sulfate alum salt, and filtering to obtain filtrate E, namely lithium hydroxide solution; finally, the obtained lithium hydroxide solution was reacted with carbon dioxide to prepare 41.16g of battery-grade lithium carbonate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (3)
1. A method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite is characterized by comprising the following steps:
s1, crushing lepidolite through a crushing device, removing weak magnetic iron minerals through a high-gradient magnetic separator, and sieving through a sieve with more than 100 meshes to obtain lepidolite concentrate powder; weighing lepidolite concentrate powder and oxalic acid according to a mass ratio of 3-6;
s2, adding concentrated sulfuric acid and the roasting material into grinding equipment for mechanical grinding, carrying out solid-phase reaction in the mixing process, transferring the mixture after mechanical grinding into an extraction tank, adding water, soaking, leaching and dissolving alkali metal sulfate, and filtering and separating to obtain a leaching solution;
s3, controlling the temperature of the leaching solution at 55-65 ℃, adding an aluminum rubidium sulfate and aluminum cesium sulfate crystallization inducer, separating out aluminum rubidium sulfate alum salt and aluminum cesium sulfate alum salt, and filtering to obtain filtrate A; cooling the filtrate A to 5-15 ℃, adding an aluminum potassium sulfate crystallization inducer to separate out potassium aluminum sulfate salt, and filtering to obtain filtrate B;
s4, adding potassium hydroxide into the filtrate B for neutralization until no precipitate is generated, and filtering the precipitate after neutralization to obtain aluminum hydroxide and a filtrate C; cooling the filtrate C to 5-15 ℃, adding a crystallization inducer into the filtrate C, crystallizing to obtain potassium sulfate, and filtering to obtain a filtrate D; using aluminum hydroxide to neutralize excessive sulfuric acid, supplementing potassium sulfate according to the addition amount of the aluminum hydroxide, crystallizing to obtain potassium aluminum sulfate alum salt, and filtering to obtain filtrate E, namely lithium hydroxide solution;
and S5, finally reacting the obtained lithium hydroxide solution with carbon dioxide to prepare the battery-grade lithium carbonate.
2. The method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite as claimed in claim 1, wherein in step S2, the mass ratio of concentrated sulfuric acid to the roasting material is 1:1-6.
3. The method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite as claimed in claim 1, wherein the crystallization inducing agent is a precipitated substance of 500nm to 5 um.
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| CN114752784B (en) * | 2022-03-04 | 2023-06-20 | 华南理工大学 | Technology for improving lithium leaching rate in lepidolite |
| CN115216645B (en) * | 2022-07-09 | 2023-05-02 | 志存锂业集团有限公司 | Method for extracting lithium from electrolytic aluminum waste residue by mixed salt calcination |
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