CN111439763A - Preparation method of lithium carbonate - Google Patents
Preparation method of lithium carbonate Download PDFInfo
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- CN111439763A CN111439763A CN202010215858.5A CN202010215858A CN111439763A CN 111439763 A CN111439763 A CN 111439763A CN 202010215858 A CN202010215858 A CN 202010215858A CN 111439763 A CN111439763 A CN 111439763A
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- lithium carbonate
- lithium
- sodium hydroxide
- precipitate
- ethanol solution
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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
Abstract
The invention discloses a preparation method of lithium carbonate, which comprises the steps of adding lithium chloride into absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution; adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution; adding the lithium chloride ethanol solution into the sodium hydroxide ethanol solution by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the carbon dioxide and the lithium chloride ethanol solution together, performing ultrasonic reaction to obtain a suspended ethanol solution, performing reduced pressure distillation reaction, cooling and filtering to obtain a mixed precipitate; and heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain turbid liquid, filtering the turbid liquid while the turbid liquid is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain the lithium carbonate. The invention solves the problem that the purity of lithium carbonate is reduced due to the fact that a dispersing agent is still used in the prior art, and realizes quick impurity removal of lithium carbonate by utilizing the solubility difference of lithium carbonate and sodium chloride to obtain the lithium carbonate with higher purity.
Description
Technical Field
The invention belongs to the field of chemical industry, relates to the field of lithium batteries, and particularly relates to a preparation method of lithium carbonate.
Background
The lithium carbonate has wide application, and particularly has very important economic value and social benefit as the raw material of the lithium battery in the current new energy industry. Therefore, the efficient preparation of high-purity lithium carbonate under specific regional conditions is of great significance to the development of new energy industry in China.
Carbonation is also a basic raw material for the manufacture of lithium ion batteries. In recent years, with the large-scale explosion of power automobiles and energy storage batteries, the lithium carbonate has a higher and higher proportion in the aspect of batteries. In the application of the lithium carbonate in the battery, the influence of the particle size and the dispersity of the lithium carbonate on the application performance is large. For example, in the process of preparing lithium iron phosphate by a solid-phase synthesis method, iron phosphate or other phosphorus and iron sources are used as raw materials, lithium carbonate and other auxiliary materials are added and fully mixed, and then the mixture is sintered to obtain the lithium iron phosphate material. Lithium carbonate with poor fluidity and dispersibility may be non-uniformly dispersed on the surfaces of other raw and auxiliary materials, resulting in poor consistency of the product. Therefore, the conventional method adopts a dispersing agent as an auxiliary material to carry out rapid dispersion, but the addition of the dispersing agent not only causes the change of a reaction system, but also brings certain impurities to cause the reduction of the purity of the lithium carbonate.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of lithium carbonate, which solves the problem that the purity of lithium carbonate is reduced due to the fact that a dispersant is still used in the prior art, and realizes rapid impurity removal of lithium carbonate by utilizing the solubility difference of lithium carbonate and sodium chloride to obtain the lithium carbonate with higher purity.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of lithium carbonate comprises the following steps:
step 1, adding lithium chloride into absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 20-40 g/L, the temperature of constant-temperature stirring is 10-20 ℃, and the stirring speed is 1000-2000 r/min;
step 2, adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution, wherein the concentration of the sodium hydroxide in the absolute ethyl alcohol is 20-40 g/L, the stirring speed at constant temperature is 10-20 ℃, and the stirring speed is 1000-2000r/min to obtain sodium hydroxide alcohol solution;
step 3, adding lithium chloride ethanol liquid into sodium hydroxide ethanol liquid by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the lithium chloride ethanol liquid together with the lithium chloride ethanol liquid, performing ultrasonic reaction to obtain suspended ethanol liquid, performing reduced pressure distillation reaction, cooling and filtering to obtain a mixed precipitate, wherein the volume of the lithium chloride ethanol liquid is 70-80% of the volume of the sodium hydroxide ethanol liquid, the dropping speed is 2-4m L/min, the volume ratio of carbon dioxide gas to the lithium chloride ethanol liquid is 2-3:1, the ultrasonic dispersion temperature is 30-50 ℃, the ultrasonic frequency is 40-80kHz, the reduced pressure distillation pressure is 80-90 ℃ under the atmospheric pressure, the temperature is 70-80 ℃, and the volume after the reduced pressure distillation is 20-30% of the volume of the suspended ethanol liquid;
and 4, heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain a suspension, filtering the suspension while the solution is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain lithium carbonate, wherein the temperature of the distilled water is 40-60 ℃, the slow adding speed is 5-10m L/min, the temperature of the hot filtering is 50-70 ℃, 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 that the purity of lithium carbonate is reduced due to the fact that a dispersing agent is still used in the prior art, and realizes quick impurity removal of lithium carbonate by utilizing the solubility difference of lithium carbonate and sodium chloride to obtain the lithium carbonate with higher purity.
2. The invention utilizes the solubility of lithium chloride and sodium hydroxide in ethanol, and is assisted by the insolubility of sodium chloride and lithium carbonate in ethanol, thereby achieving the effect of promoting the reaction.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
A preparation method of lithium carbonate comprises the following steps:
step 1, adding lithium chloride into absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 20-40 g/L, the stirring temperature at the constant temperature is 10-20 ℃, the stirring speed is 1000-2000r/min, and the lithium chloride is dissolved in the absolute ethyl alcohol to form a good dissolving system;
step 2, adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution, wherein the concentration of the sodium hydroxide in the absolute ethyl alcohol is 20-40 g/L, the stirring speed at constant temperature is 10-20 ℃, and the stirring speed is 1000-2000r/min to obtain sodium hydroxide alcohol solution;
step 3, adding a lithium chloride ethanol solution into a sodium hydroxide ethanol solution by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the lithium chloride ethanol solution together with the lithium chloride ethanol solution, obtaining a suspended ethanol solution through an ultrasonic reaction, cooling and filtering after the reduced pressure distillation reaction to obtain a mixed precipitate, wherein the volume of the lithium chloride ethanol solution is 70-80% of the volume of the sodium hydroxide ethanol solution, the dropping speed is 2-4m L/min, the volume ratio of carbon dioxide gas to the lithium chloride ethanol solution is 2-3:1, the ultrasonic dispersion temperature is 30-50 ℃, the ultrasonic frequency is 40-80kHz, the pressure of the reduced pressure distillation is 80-90 ℃, the temperature is 70-80 ℃, the volume after the reduced pressure distillation is 20-30% of the volume of the suspended ethanol solution, in the step, lithium chloride and carbon dioxide react with sodium hydroxide to convert into sodium chloride and lithium bicarbonate with poor solubility in ethanol, in the reduced pressure distillation reaction, most of the ethanol is recycled, the ethanol solvent is greatly reduced, the solute concentration in the ethanol is increased, further the sodium chloride and lithium carbonate are separated out, the lithium carbonate is further cooled, the lithium carbonate is further precipitated after the lithium carbonate is filtered, the lithium carbonate is precipitated by using a sodium carbonate and the sodium carbonate, the lithium carbonate is precipitated, the lithium carbonate precipitated by using a sodium carbonate precipitated under the sodium carbonate precipitated;
and 4, heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain a suspension, filtering the suspension while the solution is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain lithium carbonate, wherein the temperature of the distilled water is 40-60 ℃, the slow adding speed is 5-10m L/min, the temperature of the hot filtering is 50-70 ℃, and the drying temperature is 80-90 ℃.
Example 1
A preparation method of lithium carbonate comprises the following steps:
step 1, adding lithium chloride into 1L absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 20 g/L, the temperature of constant-temperature stirring is 10 ℃, and the stirring speed is 1000 r/min;
step 2, adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution, wherein the concentration of the sodium hydroxide in the absolute ethyl alcohol is 20 g/L, the stirring speed at constant temperature is 10 ℃, and the stirring speed is 1000 r/min;
step 3, adding lithium chloride ethanol liquid into sodium hydroxide ethanol liquid by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the lithium chloride ethanol liquid together with the lithium chloride ethanol liquid, carrying out ultrasonic reaction to obtain suspended ethanol liquid, carrying out reduced pressure distillation reaction, cooling and filtering to obtain a mixed precipitate, wherein the volume of the lithium chloride ethanol liquid is 70% of that of the sodium hydroxide ethanol liquid, the dropping speed is 2m L/min, the volume ratio of carbon dioxide gas to the lithium chloride ethanol liquid is 2:1, the ultrasonic dispersion temperature is 30 ℃, the ultrasonic frequency is 40kHz, the pressure of the reduced pressure distillation is 80 ℃ under the atmospheric pressure, the temperature is 70 ℃, and the volume after the reduced pressure distillation is 20% of that of the suspended ethanol liquid;
and 4, heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain a suspension, filtering the suspension while the solution is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain lithium carbonate, wherein the temperature of the distilled water is 40 ℃, the slow adding speed is 5m L/min, the hot filtering temperature is 50 ℃, and the drying temperature is 80 ℃.
The lithium carbonate of this example had a purity of 99.97%, a yield of 95.2% and a particle size distribution range of 50 to 100 μm.
Example 2
A preparation method of lithium carbonate comprises the following steps:
step 1, adding lithium chloride into 1L absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 40 g/L, the stirring temperature at constant temperature is 20 ℃, and the stirring speed is 2000 r/min;
step 2, adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution, wherein the concentration of the sodium hydroxide in the absolute ethyl alcohol is 40 g/L, the stirring speed at constant temperature is 20 ℃, and the stirring speed is 2000r/min to obtain sodium hydroxide alcohol solution;
step 3, adding lithium chloride ethanol liquid into sodium hydroxide ethanol liquid by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the lithium chloride ethanol liquid together with the lithium chloride ethanol liquid, carrying out ultrasonic reaction to obtain suspended ethanol liquid, carrying out reduced pressure distillation reaction, cooling and filtering to obtain a mixed precipitate, wherein the volume of the lithium chloride ethanol liquid is 80% of that of the sodium hydroxide ethanol liquid, the dropping speed is 4m L/min, the volume ratio of carbon dioxide gas to the lithium chloride ethanol liquid is 3:1, the ultrasonic dispersion temperature is 50 ℃, the ultrasonic frequency is 80kHz, the pressure of the reduced pressure distillation is 90 ℃ under the atmospheric pressure, the temperature is 80 ℃, and the volume after the reduced pressure distillation is 30% of that of the suspended ethanol liquid;
and 4, heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain a suspension, filtering the suspension while the solution is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain lithium carbonate, wherein the temperature of the distilled water is 60 ℃, the slow adding speed is 10m L/min, the hot filtering temperature is 70 ℃, and the drying temperature is 90 ℃.
The lithium carbonate of this example had a purity of 99.98%, a yield of 96.1% and a particle size distribution range of 100-200 μm.
Example 3
A preparation method of lithium carbonate comprises the following steps:
step 1, adding lithium chloride into 1L absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution, wherein the concentration of the lithium chloride in the absolute ethyl alcohol is 30 g/L, the temperature of constant-temperature stirring is 15 ℃, and the stirring speed is 1500 r/min;
step 2, adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution, wherein the concentration of the sodium hydroxide in the absolute ethyl alcohol is 30 g/L, the stirring speed at constant temperature is 15 ℃, and the stirring speed is 1500 r/min;
step 3, adding lithium chloride ethanol liquid into sodium hydroxide ethanol liquid by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the lithium chloride ethanol liquid together with the lithium chloride ethanol liquid, carrying out ultrasonic reaction to obtain suspended ethanol liquid, carrying out reduced pressure distillation reaction, cooling and filtering to obtain a mixed precipitate, wherein the volume of the lithium chloride ethanol liquid is 75% of that of the sodium hydroxide ethanol liquid, the dropping speed is 3m L/min, the volume ratio of carbon dioxide gas to the lithium chloride ethanol liquid is 3:1, the ultrasonic dispersion temperature is 40 ℃, the ultrasonic frequency is 60kHz, the pressure of the reduced pressure distillation is 85 ℃ under the atmospheric pressure, the temperature is 75 ℃, and the volume after the reduced pressure distillation is 25% of that of the suspended ethanol liquid;
and 4, heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain a suspension, filtering the suspension while the solution is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain lithium carbonate, wherein the temperature of the distilled water is 50 ℃, the slow adding speed is 8m L/min, the hot filtering temperature is 60 ℃, and the drying temperature is 85 ℃.
The lithium carbonate of this example had a purity of 99.98%, a yield of 95.5% and a particle size distribution in the range of 80 to 100 μm.
In summary, the invention has the following advantages:
1. the invention solves the problem that the purity of lithium carbonate is reduced due to the fact that a dispersing agent is still used in the prior art, and realizes quick impurity removal of lithium carbonate by utilizing the solubility difference of lithium carbonate and sodium chloride to obtain the lithium carbonate with higher purity.
2. The invention utilizes the solubility of lithium chloride and sodium hydroxide in ethanol, and is assisted by the insolubility of sodium chloride and lithium carbonate in ethanol, thereby achieving the effect of promoting the reaction.
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 (5)
1. A preparation method of lithium carbonate is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding lithium chloride into absolute ethyl alcohol, stirring at constant temperature until the lithium chloride is completely dissolved to obtain lithium chloride ethanol solution;
step 2, adding sodium hydroxide into absolute ethyl alcohol, stirring at constant temperature until the sodium hydroxide is completely dissolved to obtain sodium hydroxide alcohol solution;
step 3, adding the lithium chloride ethanol solution into the sodium hydroxide ethanol solution by using a pipeline, simultaneously flushing carbon dioxide into the pipeline, flushing the carbon dioxide and the lithium chloride ethanol solution together, performing ultrasonic reaction to obtain a suspended ethanol solution, performing reduced pressure distillation reaction, cooling and filtering to obtain a mixed precipitate;
and 4, heating distilled water and slowly adding the distilled water into the mixed precipitate until the precipitate is continuously reduced to obtain turbid liquid, filtering the turbid liquid while the turbid liquid is hot to obtain lithium carbonate precipitate, washing the lithium carbonate precipitate for a plurality of times by using absolute ethyl alcohol, and drying the lithium carbonate precipitate to obtain the lithium carbonate.
2. The method for preparing lithium carbonate as recited in claim 1 wherein the concentration of lithium chloride in absolute ethanol in step 1 is 20-40 g/L, the temperature of the isothermal stirring is 10-20 ℃, and the stirring speed is 1000-2000 r/min.
3. The method for preparing lithium carbonate as claimed in claim 1, wherein in the step 2, the concentration of the sodium hydroxide in the absolute ethanol is 20-40 g/L, the stirring speed at constant temperature is 10-20 ℃, and the stirring speed is 1000-2000 r/min.
4. The method for preparing lithium carbonate according to claim 1, wherein the volume of the lithium chloride ethanol solution in the step 3 is 70-80% of the volume of the sodium hydroxide ethanol solution, the dropping speed is 2-4m L/min, the volume ratio of the carbon dioxide gas to the lithium chloride ethanol solution is 2-3:1, the ultrasonic dispersion temperature is 30-50 ℃, the ultrasonic frequency is 40-80kHz, the pressure of the reduced pressure distillation is 80-90 ℃ under the atmospheric pressure, the temperature is 70-80 ℃, and the volume after the reduced pressure distillation is 20-30% of the volume of the suspension ethanol solution.
5. The method for preparing lithium carbonate according to claim 1, wherein the temperature of the distilled water in the step 4 is 40-60 ℃, the slow addition speed is 5-10m L/min, the hot filtration temperature is 50-70 ℃, and the drying temperature is 80-90 ℃.
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| CN202010215858.5A CN111439763A (en) | 2020-03-25 | 2020-03-25 | Preparation method of lithium carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114933320A (en) * | 2022-04-29 | 2022-08-23 | 广东马车动力科技有限公司 | Method for refining lithium chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114933320A (en) * | 2022-04-29 | 2022-08-23 | 广东马车动力科技有限公司 | Method for refining lithium chloride |
| CN114933320B (en) * | 2022-04-29 | 2024-03-29 | 广东马车动力科技有限公司 | Lithium chloride refining method |
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Application publication date: 20200724 |