CN111362286A - In-situ preparation method of lithium carbonate - Google Patents
In-situ preparation method of lithium carbonate Download PDFInfo
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- CN111362286A CN111362286A CN202010263064.6A CN202010263064A CN111362286A CN 111362286 A CN111362286 A CN 111362286A CN 202010263064 A CN202010263064 A CN 202010263064A CN 111362286 A CN111362286 A CN 111362286A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses an in-situ preparation method of lithium carbonate, which comprises the following steps: dissolving lithium chloride in absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution; coating a film on the surface of the alumina porous foam body in a manner of leaching and lifting lithium alcohol solution, and drying at constant temperature to obtain a coated foam body; putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 2-4h at constant temperature and constant pressure to obtain a foaming body with a lithium carbonate film; soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 2-4h, removing the foaming body, filtering, soaking the filter material in a sodium hydroxide solution for 30-40min, filtering again, washing the filter material in absolute ethyl alcohol, and drying to obtain the lithium carbonate. The invention solves the problem of the dependency of the prior art on the dispersing agent, utilizes the in-situ reaction system of the solid-gas structure to uniformly distribute the lithium carbonate particles on the surface of the foaming body, and obtains the uniformly dispersed lithium carbonate particles in a stripping mode.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to an in-situ preparation method of lithium carbonate.
Background
The lithium ion battery has high capacity, high voltage, low energy consumption, no memory effect, no public hazard and small volume. The battery has the advantages of less self-discharge, more cycle times and the like, is widely applied to electronic products such as mobile phones, PDAs, notebook computers, portable compact discs and the like, gradually expands to the fields of electric automobiles, space technology, national defense industry and the like, and is one of the most concerned novel batteries at present. The nano-scale electrode material of the lithium ion battery has the characteristics of small grain size, large specific surface area, high ion diffusion coefficient and the like, is beneficial to the embedding and the separation of lithium ions in active materials of inner layers of particles, improves the utilization rate of the active materials, improves the charge-discharge cycle performance of the materials, and can also improve the charge-discharge rate by increasing the contact area of the electrode and electrolyte, thereby having qualitative breakthrough on improving the performance of the lithium ion battery.
In recent years, lithium has been rapidly applied to high and new technical fields, particularly new energy and new materials. With the maturity of various lithium extraction technologies, the development cost of industrial-grade lithium carbonate is reduced, the price is greatly reduced, the demand gradually tends to be saturated, the market space is gradually reduced, and the competition is increasingly intense. Meanwhile, with the expansion of market demand for high-purity lithium salt in the field of energy and new materials and the continuous progress of technological research, the production of high-purity lithium carbonate has already been step into an industrialized express way. However, in the existing preparation process, the dispersing agent is adopted to realize the rapid dispersion of the lithium carbonate, and the dispersing agent needs to be removed under the conditions of high temperature and the like, so that the process is complex, and the purity of the lithium carbonate is easy to reduce.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an in-situ preparation method of lithium carbonate, which solves the problem of the dependency of the prior art on a dispersing agent, utilizes an in-situ reaction system of a solid-gas structure to uniformly distribute lithium carbonate particles on the surface of a foaming body, and obtains the uniformly dispersed lithium carbonate particles in a stripping mode.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
an in-situ preparation method of lithium carbonate comprises the following steps:
step 1, dissolving lithium chloride in absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 20-40g/L, the ultrasonic frequency of the ultrasonic dispersion is 40-80kHz, and the temperature is 10-30 ℃;
step 2, coating a film on the surface of the alumina porous foam in a manner of leaching and lifting lithium alcohol solution, and drying at constant temperature to obtain a coated foam; the dipping speed of dipping and pulling is 200-400mm/min, the retention time is 3-6s, the pulling speed is 100-300mm/min, the temperature is 10-20 ℃, and the temperature for constant-temperature drying is 80-90 ℃; the porosity of the alumina porous foam is 60 to 100 ppi; the pretreatment method of the aluminum oxide comprises the following steps: step a, sequentially soaking alumina into distilled water and absolute ethyl alcohol for microwave reaction, and drying to obtain a clean foaming body, wherein the microwave power of the microwave reaction is 200-500W, and the temperature isThe temperature is 10-20 ℃, and the drying temperature is 100-120 ℃; step b, spraying dilute hydrochloric acid on the specific surface of the clean foaming body uniformly to form a liquid film, and then quickly drying to obtain the alumina porous foaming body with rough surface, wherein the pH value of the dilute hydrochloric acid is 5-6, and the spraying amount of the liquid film is 0.2-0.6mL/cm2；
Step 3, putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 2-4h at constant temperature and constant pressure to obtain a foaming body with a lithium carbonate film; the volume concentration of the water vapor of the low-humidity carbon dioxide gas is 2-5%, the temperature of the constant temperature and the constant pressure is 100-120 ℃, and the pressure is 0.2-0.4 MPa;
step 4, soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 2-4h, removing the foaming body, filtering, placing the filter material in a sodium hydroxide solution for soaking for 30-40min, filtering again, placing the filter material in absolute ethyl alcohol for washing, and drying to obtain lithium carbonate; the ultrasonic frequency of the ultrasonic stripping is 40-60kHz, the temperature is 40-50 ℃, the concentration of the sodium hydroxide is 0.002-0.007mol/L, and the drying temperature is 80-90 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of the dependency of the prior art on the dispersing agent, utilizes the in-situ reaction system of the solid-gas structure to uniformly distribute the lithium carbonate particles on the surface of the foaming body, and obtains the uniformly dispersed lithium carbonate particles in a stripping mode.
2. According to the invention, a good surface film structure is formed by utilizing the solubility of lithium chloride, the conversion of lithium chloride and the generation of lithium carbonate are realized by utilizing the control of a gas environment, the effect of stable dispersion is achieved, and a dispersing agent is not required.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
An in-situ preparation method of lithium carbonate comprises the following steps:
step 1, dissolving lithium chloride in absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 20-40g/L, the ultrasonic frequency of the ultrasonic dispersion is 40-80kHz, and the temperature is 10-30 ℃; the low-temperature ultrasound forms high-frequency vibration, lithium chloride is quickly dissolved in absolute ethyl alcohol and is uniformly dispersed, meanwhile, the ultrasound brings heat energy to cause the temperature of the whole solvent to rise, and the temperature is within a certain range, so that the absolute ethyl alcohol can be prevented from being evaporated due to heat; the step can obtain a uniformly dispersed lithium chloride ethanol solution;
step 2, coating a film on the surface of the alumina porous foam in a manner of leaching and lifting lithium alcohol solution, and drying at constant temperature to obtain a coated foam; the dipping speed of dipping and pulling is 200-400mm/min, the retention time is 3-6s, the pulling speed is 100-300mm/min, the temperature is 10-20 ℃, the temperature of constant-temperature drying is 80-90 ℃, the alumina porous foaming body is dipped and pulled into the lithium alcohol liquid, lithium chloride in the lithium alcohol liquid can be uniformly dispersed in a liquid film on the surface of the alumina porous foaming body by utilizing the film forming property of absolute ethyl alcohol, so that the uniform film coating effect is achieved, then, under the condition of constant-temperature drying, absolute ethyl alcohol is converted into ethanol steam to be rapidly discharged, the melting point of the lithium chloride is higher, and the lithium chloride is still remained on the surface of the alumina porous foaming body, so that the surface of the foaming body is a lithium chloride film; the porosity of the alumina porous foaming body is 60-100ppi, the foaming body with the porosity can ensure the uniform dispersion of the lithium chloride film, and a sufficient dispersion space is formed for reaction, and further, the alumina foaming body with the porous structure has a large specific surface, so that lithium chloride is converted into a large-area lithium chloride film as much as possible; the pretreatment method of the aluminum oxide comprises the following steps: step a, sequentially soaking alumina into distilled water and absolute ethyl alcohol for microwave reaction, and drying to obtain a clean foaming body, wherein the microwave power of the microwave reaction is 200-20 ℃ and the drying temperature is 100-120 ℃; step b, spraying dilute hydrochloric acid on the specific surface of the clean foaming body uniformly to form a liquid film, and then quickly drying to obtain the alumina porous foaming body with rough surface, wherein the pH value of the dilute hydrochloric acid is 5-6, and the spraying amount of the liquid film is 0.2-0.6mL/cm2The adoption of the alumina with rough surface can increase the adhesion and connectivity of lithium chloride on the surface of the alumina in a large gradient manner, thereby preventing the falling-off problem of the lithium chloride;
step 3, putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 2-4h at constant temperature and constant pressure to obtain a foaming body with a lithium carbonate film; the volume concentration of the steam of the low-humidity carbon dioxide gas is 2-5%, the constant temperature and constant pressure are 100-120 ℃, the pressure is 0.2-0.4MPa, the steam and the lithium chloride react under the conditions of constant temperature and constant pressure and are converted into lithium carbonate particles under the atmosphere of the carbon dioxide, and based on the whole reaction system, the lithium carbonate cannot be displaced because no solvent is contained, so that the lithium chloride is converted into the lithium carbonate particles in situ;
step 4, soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 2-4h, removing the foaming body, filtering, placing the filter material in a sodium hydroxide solution for soaking for 30-40min, filtering again, placing the filter material in absolute ethyl alcohol for washing, and drying to obtain lithium carbonate; the ultrasonic frequency of the ultrasonic stripping is 40-60kHz, the temperature is 40-50 ℃, the lithium carbonate can be separated from the alumina foam body by the ultrasonic stripping in the absolute ethyl alcohol, the separation effect of the lithium carbonate is achieved, the lithium carbonate can be completely stripped by the sufficient ultrasonic stripping, the concentration of the sodium hydroxide is 0.002-0.007mol/L, and the drying temperature is 80-90 ℃; and (3) putting the stripped particles into a sodium hydroxide solution, removing alumina impurities in the filter material by utilizing the solubility of sodium hydroxide to alumina and the insolubility of lithium carbonate, still maintaining the deposition of lithium carbonate, completely collecting lithium carbonate after filtering, simultaneously dissolving the residual sodium hydroxide by absolute ethyl alcohol, obtaining the lithium carbonate material after washing by absolute ethyl alcohol, and drying.
Example 1
An in-situ preparation method of lithium carbonate comprises the following steps:
step 1, dissolving lithium chloride in 1L of absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 20g/L, the ultrasonic frequency of the ultrasonic dispersion is 40kHz, and the temperature is 10 ℃;
step 2, coating the aluminum oxide porous film by a lithium alcohol solution leaching and pulling methodDrying the surface of the foaming body at constant temperature to obtain a film-coated foaming body; the dipping speed of dipping and pulling is 200mm/min, the retention time is 3s, the pulling speed is 100mm/min, the temperature is 10 ℃, and the temperature for constant-temperature drying is 80 ℃; the porosity of the alumina porous foam was 60 ppi; the pretreatment method of the aluminum oxide comprises the following steps: step a, sequentially soaking alumina into distilled water and absolute ethyl alcohol for microwave reaction, and drying to obtain a clean foaming body, wherein the microwave power of the microwave reaction is 200W, the temperature is 10 ℃, and the drying temperature is 100 ℃; step b, uniformly spraying dilute hydrochloric acid on the specific surface of the clean foaming body to form a liquid film, and then quickly drying to obtain the alumina porous foaming body with a rough surface, wherein the pH value of the dilute hydrochloric acid is 5, and the spraying amount of the liquid film is 0.2mL/cm2；
Step 3, putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 2 hours at constant temperature and constant pressure to obtain the foaming body with the lithium carbonate film; the volume concentration of the water vapor of the low-humidity carbon dioxide gas is 2%, the temperature of the constant temperature and the constant pressure is 100 ℃, and the pressure is 0.2 MPa;
step 4, soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 2 hours, removing the foaming body, filtering, placing the filter material in a sodium hydroxide solution for soaking for 30 minutes, filtering again, placing the filter material in absolute ethyl alcohol for washing, and drying to obtain lithium carbonate; the ultrasonic frequency of the ultrasonic stripping is 40kHz, the temperature is 40 ℃, the concentration of the sodium hydroxide is 0.002mol/L, and the drying temperature is 80 ℃.
The lithium carbonate of this example had a purity of 99.93%, a yield of 99.2% and a particle size distribution range of 5 to 10 μm.
Example 2
An in-situ preparation method of lithium carbonate comprises the following steps:
step 1, dissolving lithium chloride in 1L of absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 40g/L, the ultrasonic frequency of the ultrasonic dispersion is 80kHz, and the temperature is 30 ℃;
step 2, plating a film on the alumina in a manner of leaching and pulling the lithium alcohol solutionDrying the surface of the porous foaming body at constant temperature to obtain a film-coated foaming body; the dipping speed of dipping and pulling is 400mm/min, the retention time is 6s, the pulling speed is 300mm/min, the temperature is 20 ℃, and the temperature for constant-temperature drying is 90 ℃; the porosity of the alumina porous foam is 100 ppi; the pretreatment method of the aluminum oxide comprises the following steps: step a, sequentially soaking alumina into distilled water and absolute ethyl alcohol for microwave reaction, and drying to obtain a clean foaming body, wherein the microwave power of the microwave reaction is 500W, the temperature is 20 ℃, and the drying temperature is 120 ℃; step b, uniformly spraying dilute hydrochloric acid on the specific surface of the clean foaming body to form a liquid film, and then quickly drying to obtain the alumina porous foaming body with a rough surface, wherein the pH value of the dilute hydrochloric acid is 6, and the spraying amount of the liquid film is 0.6mL/cm2；
Step 3, putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 4 hours at constant temperature and constant pressure to obtain the foaming body with the lithium carbonate film; the volume concentration of the water vapor of the low-humidity carbon dioxide gas is 5%, the temperature of the constant temperature and the constant pressure is 120 ℃, and the pressure is 0.4 MPa;
step 4, soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 4 hours, removing the foaming body, filtering, placing the filter material in a sodium hydroxide solution for soaking for 30-40min, filtering again, placing the filter material in absolute ethyl alcohol for washing, and drying to obtain lithium carbonate; the ultrasonic frequency of the ultrasonic stripping is 60kHz, the temperature is 50 ℃, the concentration of the sodium hydroxide is 0.007mol/L, and the drying temperature is 90 ℃.
The lithium carbonate of this example had a purity of 99.94%, a yield of 99.3% and a particle size distribution range of 10 to 20 μm.
Example 3
An in-situ preparation method of lithium carbonate comprises the following steps:
step 1, dissolving lithium chloride in 1L of absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 30g/L, the ultrasonic frequency of the ultrasonic dispersion is 60kHz, and the temperature is 20 ℃;
step 2, plating a film by leaching and pulling the lithium alcohol solutionDrying the surface of the alumina porous foam at constant temperature to obtain a coated foam; the dipping speed of dipping and pulling is 300mm/min, the retention time is 5s, the pulling speed is 200mm/min, the temperature is 15 ℃, and the temperature for constant-temperature drying is 85 ℃; the porosity of the alumina porous foam was 80 ppi; the pretreatment method of the aluminum oxide comprises the following steps: step a, sequentially soaking alumina into distilled water and absolute ethyl alcohol for microwave reaction, and drying to obtain a clean foaming body, wherein the microwave power of the microwave reaction is 400W, the temperature is 15 ℃, and the drying temperature is 110 ℃; step b, uniformly spraying dilute hydrochloric acid on the specific surface of the clean foaming body to form a liquid film, and then quickly drying to obtain the alumina porous foaming body with a rough surface, wherein the pH value of the dilute hydrochloric acid is 6, and the spraying amount of the liquid film is 0.4mL/cm2；
Step 3, putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 3 hours at constant temperature and constant pressure to obtain the foaming body with the lithium carbonate film; the volume concentration of the water vapor of the low-humidity carbon dioxide gas is 4%, the temperature of the constant temperature and the constant pressure is 110 ℃, and the pressure is 0.3 MPa;
step 4, soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 3 hours, removing the foaming body, filtering, placing the filter material in a sodium hydroxide solution for soaking for 35 minutes, filtering again, placing the filter material in absolute ethyl alcohol for washing, and drying to obtain lithium carbonate; the ultrasonic frequency of the ultrasonic stripping is 50kHz, the temperature is 45 ℃, the concentration of the sodium hydroxide is 0.005mol/L, and the drying temperature is 85 ℃.
The lithium carbonate of this example had a purity of 99.93%, a yield of 99.1% and a particle size distribution range of 8 to 20 μm.
In summary, the invention has the following advantages:
1. the invention solves the problem of the dependency of the prior art on the dispersing agent, utilizes the in-situ reaction system of the solid-gas structure to uniformly distribute the lithium carbonate particles on the surface of the foaming body, and obtains the uniformly dispersed lithium carbonate particles in a stripping mode.
2. According to the invention, a good surface film structure is formed by utilizing the solubility of lithium chloride, the conversion of lithium chloride and the generation of lithium carbonate are realized by utilizing the control of a gas environment, the effect of stable dispersion is achieved, and a dispersing agent is not required.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (8)
1. An in-situ preparation method of lithium carbonate is characterized by comprising the following steps: the method comprises the following steps:
step 1, dissolving lithium chloride in absolute ethyl alcohol, and performing constant-temperature ultrasonic dispersion to form a lithium alcohol solution;
step 2, coating a film on the surface of the alumina porous foam in a manner of leaching and lifting lithium alcohol solution, and drying at constant temperature to obtain a coated foam;
step 3, putting the film-coated foaming body into a reaction kettle, introducing low-humidity carbon dioxide gas, and reacting for 2-4h at constant temperature and constant pressure to obtain a foaming body with a lithium carbonate film;
and 4, soaking the foaming body with the lithium carbonate film in an absolute ethyl alcohol solution for ultrasonic stripping for 2-4h, removing the foaming body, filtering, then placing the filter material in a sodium hydroxide solution for soaking for 30-40min, then filtering again, then placing the filter material in absolute ethyl alcohol for washing, and drying to obtain the lithium carbonate.
2. A method for the in situ preparation of lithium carbonate according to claim 1, characterized in that: the concentration of the lithium chloride in the absolute ethyl alcohol in the step 1 is 20-40g/L, the ultrasonic frequency of ultrasonic dispersion is 40-80kHz, and the temperature is 10-30 ℃.
3. The in situ preparation method of lithium carbonate according to claim 1, characterized in that: the dipping speed of dipping and pulling is 200-400mm/min, the retention time is 3-6s, the pulling speed is 100-300mm/min, the temperature is 10-20 ℃, and the temperature for constant-temperature drying is 80-90 ℃; the porosity of the alumina porous foam is 60 to 100 ppi.
4. The in situ preparation method of lithium carbonate according to claim 1, characterized in that: the pretreatment method of the aluminum oxide comprises the following steps: step a, sequentially soaking alumina into distilled water and absolute ethyl alcohol for microwave reaction, and drying to obtain a clean foaming body; and b, uniformly spraying dilute hydrochloric acid on the specific surface of the clean foaming body to form a liquid film, and then quickly drying to obtain the alumina porous foaming body with a rough surface.
5. The in situ preparation method of lithium carbonate according to claim 4, characterized in that: the microwave power of the microwave reaction in the step a is 200-500W, the temperature is 10-20 ℃, and the drying temperature is 100-120 ℃.
6. The in situ preparation method of lithium carbonate according to claim 4, characterized in that: the pH value of the dilute hydrochloric acid in the step b is 5-6, and the spraying amount of the liquid membrane is 0.2-0.6mL/cm2。
7. The in situ preparation method of lithium carbonate according to claim 1, characterized in that: the volume concentration of the water vapor of the low-humidity carbon dioxide gas in the step 3 is 2-5%, the temperature of the constant temperature and the constant pressure is 100-120 ℃, and the pressure is 0.2-0.4 MPa.
8. The in situ preparation method of lithium carbonate according to claim 1, characterized in that: the ultrasonic frequency of the ultrasonic stripping in the step 4 is 40-60kHz, the temperature is 40-50 ℃, the concentration of the sodium hydroxide is 0.002-0.007mol/L, and the drying temperature is 80-90 ℃.
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| CN113526561A (en) * | 2021-07-15 | 2021-10-22 | 湖北亿纬动力有限公司 | Positive electrode lithium supplement material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113526561A (en) * | 2021-07-15 | 2021-10-22 | 湖北亿纬动力有限公司 | Positive electrode lithium supplement material and preparation method and application thereof |
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