CN111333090A - Preparation method of high-purity lithium carbonate - Google Patents
Preparation method of high-purity lithium carbonate Download PDFInfo
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- CN111333090A CN111333090A CN202010215841.XA CN202010215841A CN111333090A CN 111333090 A CN111333090 A CN 111333090A CN 202010215841 A CN202010215841 A CN 202010215841A CN 111333090 A CN111333090 A CN 111333090A
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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 belongs to the field of chemical industry, relates to the field of lithium batteries, and particularly relates to a preparation method of high-purity lithium carbonate, which comprises the following steps: step 1, slowly adding lithium chloride into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution; step 2, adding ammonium bicarbonate into distilled water, stirring at low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution; step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 1-3 hours to obtain a mixed solution; and 4, adding the mixed solution into a reaction kettle to perform constant-temperature spray reaction, standing and settling, blowing the tail with dry nitrogen, and cooling to obtain the high-purity lithium carbonate. The invention solves the problems of complex process and low efficiency caused by impurity removal process in the prior art, and the lithium carbonate crystal nucleus structure is formed by utilizing the rapid vaporization of the raw material and the product formed by the spray reaction system, thereby greatly improving the complete conversion of the lithium carbonate.
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 high-purity 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.
Lithium carbonate is used as an important basic lithium salt, is widely used in the fields of high technologies such as magnetic materials, atomic energy industry, photoelectric information and the like, is particularly used as a raw material of a novel lithium ion battery anode material and electrolyte, is commonly used for producing high-purity secondary lithium salts such as high-purity lithium chloride, lithium bromide, lithium fluoride, lithium perchlorate and the like, and further is used for preparing the battery anode material and the electrolyte, so that the nano lithium carbonate has important significance for realizing the application of a nano material in a lithium ion battery. The existing method for synthesizing the nano-grade lithium carbonate mainly comprises an aqueous solution method, a gas-liquid phase contact method and the like. The preparation method is complicated, and a certain impurity removal process is needed, so that the efficiency is low, and the cost is increased.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of high-purity lithium carbonate, which solves the problems of complex process and low efficiency caused by impurity removal process in the prior art, and a spray reaction system is utilized to form rapid vaporization of raw materials and products to form a lithium carbonate crystal nucleus structure, so that the complete conversion of lithium carbonate is greatly improved.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of high-purity lithium carbonate comprises the following steps:
step 1, slowly adding lithium chloride into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution; the concentration of lithium chloride in distilled water is 30-60g/L, the slow adding speed is 2-5g/min, the low-temperature ultrasonic temperature is 10-20 ℃, and the ultrasonic frequency is 40-80 kHz;
step 2, adding ammonium bicarbonate into distilled water, stirring at low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution; the concentration of the ammonium bicarbonate in the distilled water is 70-140g/L, the low-temperature stirring temperature is 15-20 ℃, and the stirring speed is 1000-;
step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 1-3 hours to obtain a mixed solution; the molar quantity of lithium chloride in the lithium chloride solution is 80-90% of that of ammonium bicarbonate in the ammonium bicarbonate solution, the slowly dropwise adding speed is 10-20mL/min, the stirring speed of low-temperature stirring is 1000-2000r/min, the temperature is 10-15 ℃, and the temperature of low-temperature standing is 10-15 ℃;
step 4, adding the mixed solution into a reaction kettle for constant-temperature spray reaction, standing and settling, blowing tail by adopting dry nitrogen, and cooling to obtain high-purity lithium carbonate; the temperature of constant-temperature spraying is 100-120 ℃, and the spraying amount is 1-4mL/cm2The temperature of nitrogen blowing is 100-120 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problems of complex process and low efficiency caused by impurity removal process in the prior art, and the lithium carbonate crystal nucleus structure is formed by utilizing the rapid vaporization of the raw material and the product formed by the spray reaction system, thereby greatly improving the complete conversion of the lithium carbonate.
2. The invention utilizes the vaporization problem of the raw materials in the solvent to form effective solid-liquid separation, and simultaneously, the raw materials and the solvent are converted into steam, thereby realizing the high purity of the lithium carbonate without impurity formation.
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 high-purity lithium carbonate comprises the following steps:
step 1, slowly adding lithium chloride into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution; the concentration of lithium chloride in distilled water is 30-60g/L, the slow adding speed is 2-5g/min, the low-temperature ultrasonic temperature is 10-20 ℃, and the ultrasonic frequency is 40-80 kHz; slowly adding lithium chloride into distilled water, forming a stable lithium chloride solution by utilizing the good dissolution characteristic of the lithium chloride, and accelerating the rapid dispersion and dissolution of the lithium chloride by a low-temperature ultrasonic mode to form a stable and uniform solution;
step 2, adding ammonium bicarbonate into distilled water, stirring at low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution; the concentration of the ammonium bicarbonate in the distilled water is 70-140g/L, the low-temperature stirring temperature is 15-20 ℃, the stirring speed is 1000-2000r/min, the ammonium bicarbonate is dissolved in the distilled water under the low-temperature condition, a good dissolving effect can be formed, and meanwhile, in order to solve the dissolving characteristic of the ammonium bicarbonate, the stirring is carried out under the low-temperature condition, so that good stability is achieved, and an ammonium bicarbonate solution which is uniformly dispersed is formed;
step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 1-3 hours to obtain a mixed solution; the molar quantity of lithium chloride in the lithium chloride solution is 80-90% of that of ammonium bicarbonate in the ammonium bicarbonate solution, the slowly dropwise adding speed is 10-20mL/min, the stirring speed of low-temperature stirring is 1000-2000r/min, the temperature is 10-15 ℃, the temperature of low-temperature standing is 10-15 ℃, the lithium chloride solution is slowly dropwise added into the ammonium bicarbonate solution, and on the basis that the lithium chloride solution and the ammonium bicarbonate solution both use distilled water as a solvent, good intersolubility can be formed, meanwhile, the lithium chloride and the ammonium bicarbonate can react to be converted into lithium bicarbonate, the lithium chloride is rapidly surrounded by the ammonium bicarbonate along with the dropwise adding of the lithium chloride to form rapid conversion, and the ammonium bicarbonate still remains until the dropwise adding is completed, so that the reaction is further promoted; based on the fact that ammonium bicarbonate, lithium bicarbonate and ammonium chloride are dissolved in water, the total dispersion of all the substances in distilled water can be effectively promoted in a low-temperature standing mode, and a good dispersion mutual-solubility effect is achieved;
step 4, adding the mixed solution into a reaction kettle for constant-temperature spray reaction, standing and settling, blowing tail by adopting dry nitrogen, and cooling to obtain high-purity lithium carbonate; the temperature of constant-temperature spraying is 100-120 ℃, and the spraying amount is 1-4mL/cm2The temperature of nitrogen blowing is 100-120 ℃; the mixed solution is uniformly sprayed into a reaction kettle through constant-temperature spraying reaction to form fine water particles, in the process, ammonium bicarbonate and ammonium chloride are heated and decomposed to form ammonia gas, hydrogen chloride, distilled water and carbon dioxide, meanwhile, lithium bicarbonate is converted into lithium carbonate, carbon dioxide and distilled water under the self-heating condition, in the whole spraying reaction process, the decomposition temperature of the lithium bicarbonate, the ammonium bicarbonate and the ammonium chloride is basically not higher than 100 ℃, and in the decomposition process, the decomposition temperature of the lithium bicarbonate, the ammonium bicarbonate and the ammonium chloride is basically not higher than 100 DEG CThe lithium carbonate can be evaporated before the distilled water, so that the lithium carbonate is used as crystals to form crystal nuclei in fine water particles; standing and settling under the temperature condition, replacing other gases by using dry nitrogen in a tail blowing mode after the lithium carbonate is completely settled, ensuring the internal drying, and converting other gases in the whole reaction system into gaseous state, thereby obtaining high-purity lithium carbonate; thus, the purge gas in the reaction process can be discharged into water again for recycling, and can be converted into ammonium bicarbonate solution for reuse.
Example 1
A preparation method of high-purity lithium carbonate comprises the following steps:
step 1, slowly adding 30g of lithium chloride into 1L of distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution; the slow adding speed is 2-5g/min, the low-temperature ultrasonic temperature is 10 ℃, and the ultrasonic frequency is 40 kHz;
step 2, adding 70g of ammonium bicarbonate into 1L of distilled water, and stirring at a low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution; the low-temperature stirring temperature is 15 ℃, and the stirring speed is 1000 r/min;
step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 1h to obtain a mixed solution; the volume of the lithium chloride solution is 100 percent of the volume of the ammonium bicarbonate solution, the slowly dropwise adding speed is 10mL/min, the stirring speed of low-temperature stirring is 1000r/min, the temperature is 10 ℃, and the temperature of low-temperature standing is 10 ℃;
step 4, adding the mixed solution into a reaction kettle for constant-temperature spray reaction, standing and settling, blowing tail by adopting dry nitrogen, and cooling to obtain high-purity lithium carbonate; the temperature of constant temperature spraying is 100 ℃, and the spraying amount is 1mL/cm2The temperature of nitrogen blowing tail is 100 ℃.
This example produced 26.09g of lithium carbonate in 99.8% yield and 99.9% purity having a particle size distribution in the range of 1-5 μm.
Example 2
A preparation method of high-purity lithium carbonate comprises the following steps:
step 1, slowly adding 60g of lithium chloride into 1L of distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution; the slow adding speed is 5g/min, the low-temperature ultrasonic temperature is 20 ℃, and the ultrasonic frequency is 80 kHz;
step 2, adding 140g of ammonium bicarbonate into 1L of distilled water, and stirring at a low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution; the low-temperature stirring temperature is 20 ℃, and the stirring speed is 2000 r/min;
step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 3 hours to obtain a mixed solution; the volume of the lithium chloride solution is 83 percent of that of the ammonium bicarbonate solution, the slowly dropwise adding speed is 20mL/min, the stirring speed of low-temperature stirring is 2000r/min, the temperature is 15 ℃, and the temperature of low-temperature standing is 15 ℃;
step 4, adding the mixed solution into a reaction kettle for constant-temperature spray reaction, standing and settling, blowing tail by adopting dry nitrogen, and cooling to obtain high-purity lithium carbonate; the temperature of constant temperature spraying is 120 ℃, and the spraying amount is 4mL/cm2The temperature of nitrogen blowing tail was 120 ℃.
This example produced 52.24g of lithium carbonate with a yield of 99.9% and a purity of 99.9% and a particle size distribution in the range of 4-10 μm.
Example 3
A preparation method of high-purity lithium carbonate comprises the following steps:
step 1, slowly adding 40g of lithium chloride into 1L of distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution; the slow adding speed is 2-5g/min, the low-temperature ultrasonic temperature is 15 ℃, and the ultrasonic frequency is 60 kHz;
step 2, adding ammonium bicarbonate into distilled water, stirring at low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution; the concentration of ammonium bicarbonate in distilled water is 110g/L, the low-temperature stirring temperature is 18 ℃, and the stirring speed is 1500 r/min;
step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 2 hours to obtain a mixed solution; the volume of the lithium chloride solution is 125 percent of that of the ammonium bicarbonate solution, the slowly dropwise adding speed is 15mL/min, the stirring speed of low-temperature stirring is 1500r/min, the temperature is 13 ℃, and the low-temperature standing temperature is 13 ℃;
step 4, adding the mixed solution into a reaction kettle for constant-temperature spray reaction, standing and settling, blowing tail by adopting dry nitrogen, and cooling to obtain high-purity lithium carbonate; the temperature of constant temperature spraying is 110 ℃, and the spraying amount is 3mL/cm2The temperature of nitrogen blowing tail is 110 ℃.
This example produced 34.79g of lithium carbonate with a yield of 99.8% and a purity of 99.9% and a particle size distribution in the range of 3-8 μm.
In summary, the invention has the following advantages:
1. the invention solves the problems of complex process and low efficiency caused by impurity removal process in the prior art, and the lithium carbonate crystal nucleus structure is formed by utilizing the rapid vaporization of the raw material and the product formed by the spray reaction system, thereby greatly improving the complete conversion of the lithium carbonate.
2. The invention utilizes the vaporization problem of the raw materials in the solvent to form effective solid-liquid separation, and simultaneously, the raw materials and the solvent are converted into steam, thereby realizing the high purity of the lithium carbonate without impurity formation.
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 high-purity lithium carbonate is characterized by comprising the following steps: the method comprises the following steps:
step 1, slowly adding lithium chloride into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain a lithium chloride solution;
step 2, adding ammonium bicarbonate into distilled water, stirring at low temperature until the ammonium bicarbonate is completely dissolved to form an ammonium bicarbonate solution;
step 3, slowly dripping the lithium chloride solution into the ammonium bicarbonate solution, uniformly stirring at a low temperature until the dripping is finished, and standing at the low temperature for 1-3 hours to obtain a mixed solution;
and 4, adding the mixed solution into a reaction kettle to perform constant-temperature spray reaction, standing and settling, blowing the tail with dry nitrogen, and cooling to obtain the high-purity lithium carbonate.
2. The method for producing high-purity lithium carbonate according to claim 1, characterized in that: the concentration of the lithium chloride in the distilled water in the step 1 is 30-60g/L, the slow adding speed is 2-5g/min, the low-temperature ultrasonic temperature is 10-20 ℃, and the ultrasonic frequency is 40-80 kHz.
3. The method for producing high-purity lithium carbonate according to claim 1, characterized in that: the concentration of the ammonium bicarbonate in the distilled water in the step 2 is 70-140g/L, the low-temperature stirring temperature is 15-20 ℃, and the stirring speed is 1000-2000 r/min.
4. The method for producing high-purity lithium carbonate according to claim 1, characterized in that: the molar quantity of lithium chloride in the lithium chloride solution in the step 3 is 80-90% of that of ammonium bicarbonate in the ammonium bicarbonate solution, the slowly dropwise adding speed is 10-20mL/min, the stirring speed of low-temperature stirring is 1000-2000r/min, the temperature is 10-15 ℃, and the temperature of low-temperature standing is 10-15 ℃.
5. The method for producing high-purity lithium carbonate according to claim 1, characterized in that: the temperature of the constant-temperature spraying in the step 4 is 100-120 ℃, and the spraying amount is 1-4mL/cm2The temperature of nitrogen blowing is 100-120 ℃.
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| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
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| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
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