CN115849414A - Method for preparing ultrapure lithium carbonate with uniform and stable particle size - Google Patents
Method for preparing ultrapure lithium carbonate with uniform and stable particle size Download PDFInfo
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Abstract
The invention discloses a method for preparing ultrapure lithium carbonate with uniform and stable granularity, which comprises the following steps: preparing a lithium bicarbonate solution; pyrolyzing by adopting an improved pyrolysis device; centrifuging; washing with water and centrifuging again; and (4) calcining. According to the invention, carbon dioxide is introduced into the pyrolysis kettle, the increase of the air pressure in the kettle is visually shown, and the pressure in the kettle body of the pyrolysis kettle is kept constant in a pressure relief mode of the exhaust valve, so that crystals are uniformly precipitated and grown, the particle size of the obtained ultrapure lithium carbonate is stable and uniform, the condition of fluctuating particle size index is avoided, and the industrial standard is met.
Description
Technical Field
The invention relates to the technical field of lithium carbonate preparation, in particular to a method for preparing ultrapure lithium carbonate with uniform and stable granularity.
Background
At present, the requirements of various industries on lithium base material lithium carbonate are more and more strict, and especially in special industries such as high-end chips, the requirements on the quality of the ultra-pure lithium carbonate not only reflect the requirements on chemical indexes, but also reflect the strict requirements on physical indexes. The requirements of the chemical indexes comprise that the main content reaches more than 99.999 percent, the physical index requirements mainly comprise the requirements on the granularity, and the YS/T582-2013 standard requires that the lithium carbonate D10 is more than or equal to 1,3 and is more than or equal to D50 and is more than or equal to 8,9 and is more than or equal to D90 and is less than or equal to 15. However, in the existing lithium carbonate preparation method, the granularity of the method capable of obtaining the ultrapure lithium carbonate cannot be stabilized in the requirements of YS/T582-2013 standard, and similarly, the purity of the lithium carbonate which has the granularity stabilized in the requirements of YS/T582-2013 standard cannot reach more than 99.999 percent.
Disclosure of Invention
The invention aims to overcome the technical problem that the existing lithium carbonate preparation method cannot simultaneously consider the purity of over 99.999 percent and the granularity requirement in the YS/T582-2013 standard, and provides a method for preparing ultrapure lithium carbonate with uniform and stable granularity.
In order to realize the purpose, the invention adopts the following technical scheme:
a method for preparing ultrapure lithium carbonate with uniform and stable particle size, comprising the steps of:
step one, preparing and purifying a lithium bicarbonate solution: injecting pure water into a carbonization kettle, starting stirring, adding battery-grade lithium carbonate, then introducing carbon dioxide to fully react, testing the Li content in the lithium bicarbonate solution when the solution is clear and transparent, purifying when the Li content is 8g/L, and obtaining the purified solution which is the qualified lithium bicarbonate solution;
purifying the lithium bicarbonate solution: (1) and (4) performing four-stage precise filtration on the qualified lithium bicarbonate solution prepared in the step one. The lithium bicarbonate solution was first passed through a 0.5 μm filter bag to filter out the larger particulate impurities. Then passed through a 0.05 micron filter cartridge to continue filtering out small particle impurities. And finally, the filter core passes through 2 channels of 0.01 micron filter elements continuously. (2) And (2) enabling the lithium bicarbonate solution filtered in the step (1) to pass through cation exchange resin, wherein the cation exchange resin is prepared by mixing a plurality of resins with strong specific ion exchange capacity, and adding the resins into an ion exchange column for use (such as Ca, mg and other ions difficult to remove impurities). Then, SO is removed by anion exchange resin 4 2- . (3) And the lithium bicarbonate after ion exchange passes through a filter element with the diameter of 0.01 mu m again to obtain qualified lithium bicarbonate solution.
Step two, adopting a pyrolysis device to carry out pyrolysis: the pyrolysis device comprises a pyrolysis kettle body, a liquid inlet, a steam pipe and a stirring device are arranged at the top of the pyrolysis kettle body, a liquid outlet is arranged at the bottom of the pyrolysis kettle body, and the liquid outlet is communicated with the centrifugal machine; still be equipped with air inlet, gas vent, temperature sensor and pressure gauge on the pyrolysis cauldron body, air inlet and CO 2 The air source is communicated, the exhaust port is sequentially communicated with the gas drier and the carbonization kettle, and the air inlet is arranged on the gas drierAnd the exhaust port is respectively provided with an air inlet valve and an exhaust valve; the pressure gauge is electrically connected with a signal input end of the PLC, and a signal output end of the PLC is respectively and electrically connected with the air inlet valve and the exhaust valve;
the pyrolysis operation is as follows:
starting a stirring device, and injecting the qualified lithium bicarbonate solution in the step one into the pyrolysis kettle body until the liquid level of the lithium bicarbonate solution rises to 2/3 of the volume of the pyrolysis kettle; at a rate of 1Kg/m 3 Adding the lithium bicarbonate solution, adding ultrapure lithium carbonate with the purity of more than 99.999 percent as a seed crystal, and then adding carbon dioxide into the kettle body of the pyrolysis kettle through an air inlet to ensure that the air pressure in the kettle reaches 0.5-5Mpa; introducing steam into the kettle through a steam pipe to start heating, monitoring through a temperature sensor, heating the temperature in the kettle to be above 90 ℃, gradually becoming turbid in the heating process, precipitating lithium carbonate, releasing a large amount of carbon dioxide, and controlling the opening and closing of an air inlet valve and an exhaust valve through a PLC (programmable logic controller) to keep the pressure in the kettle at 0.5-5Mpa; when the temperature in the kettle rises to 95 ℃ and the pressure in the kettle does not change after 20min, manually opening an exhaust valve, drying the gas in the kettle by a gas dryer, introducing the gas into a carbonization kettle for preparing a lithium bicarbonate solution, discharging lithium carbonate slurry from a liquid outlet of the pyrolysis kettle to a centrifugal machine for centrifugation, and closing the centrifugal machine when no water drops flow down from a liquid outlet of the centrifugal machine to obtain wet lithium carbonate;
step three, washing and centrifuging again: washing the wet lithium carbonate in the second step, and centrifuging again, wherein the water content in the centrifuged lithium carbonate is controlled to be less than or equal to 5%;
step four, calcining: calcining the lithium carbonate centrifuged in the third step for 2 hours at the temperature of between 400 and 600 ℃ to obtain the ultrapure lithium carbonate with the purity of more than or equal to 99.999 percent.
Preferably, according to the technical scheme of the invention, the purity of the battery-grade lithium carbonate is 99.5%.
Preferably, in the first step, the reaction time is 2-4h.
Preferably, in the second step, the temperature rise rate is 0.5-1 ℃/min, preferably 1 ℃/min.
Preferably, in the second step, the moisture content of the wet lithium carbonate after centrifugation is less than or equal to 5 percent.
Preferably, in the third step, the solid-to-liquid ratio of the wet lithium carbonate washing is 1:5.
Compared with the existing lithium carbonate preparation method, the method has the following beneficial effects:
1. according to the invention, the pressure in the pyrolysis kettle body is kept constant by means of carbon dioxide supplement and exhaust valve pressure relief, the particle size of the obtained ultrapure lithium carbonate is stable and uniform, the condition that the particle size index is suddenly high or low is avoided, and the requirement of YS/T582-2013 standard on the particle size of the ultrapure lithium carbonate is met.
2. LiHCO according to the chemical reaction equation 2 for lithium bicarbonate pyrolysis 3 =Li 2 CO 3 +CO 2 +H 2 O showed that a large amount of carbon dioxide was generated as the reaction proceeded in the forward direction, and lithium carbonate precipitated and grown crystals as the forward reaction. If a large amount of crystals are precipitated and grow up instantly, the granularity of the crystals is not uniform, and the ultrapure lithium carbonate cannot be used. The applicant thought that by controlling the rate at which the reaction proceeds in the forward direction, lithium carbonate is allowed to grow uniformly per unit time. The method for controlling the forward reaction rate of the invention is to adjust the amount of carbon dioxide in the pyrolysis kettle, and the more products, the slower the forward reaction rate and the trend of the forward reaction are known from factors influencing the reaction rate. Therefore, carbon dioxide is introduced into the pyrolysis kettle, the pressure in the kettle is visually increased, and the effect of controlling the forward reaction rate can be achieved by controlling the pressure in the reaction kettle to be a constant value, so that crystals are uniformly precipitated and grown, the stable and uniform particle size of the ultrapure lithium carbonate is ensured, and the industrial requirements are met.
Drawings
FIG. 1 is a schematic view of a pyrolysis apparatus used in the present invention;
reference numerals: 1. a pyrolysis kettle body; 2. a liquid inlet; 3. a liquid outlet; 4. a centrifuge; 5. an air inlet; 6. an exhaust port; 7. a pressure gauge; 8. CO 2 2 A gas source; 9. a gas dryer; 10. carbonizing the kettle; 11. a temperature sensor; 12. a steam pipe; 13. and (4) a stirring device.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
In the following embodiments, the continuous pyrolysis apparatus is shown in fig. 1, and includes a pyrolysis kettle body 1, a liquid inlet 2, a steam pipe 12 and a stirring apparatus 13 are arranged at the top of the pyrolysis kettle body 1, a liquid outlet 3 is arranged at the bottom of the pyrolysis kettle body, and the liquid outlet 3 is communicated with a centrifuge 4; still be equipped with air inlet 5, gas vent 6, temperature sensor 11 and pressure gauge 7 on the pyrolysis cauldron body 1, air inlet 5 and CO 2 The gas source 8 is communicated, the exhaust port 6 is sequentially communicated with the gas drier 9 and the carbonization kettle 10, and the gas inlet 5 and the exhaust port 6 are respectively provided with a gas inlet valve and an exhaust valve; and the pressure gauge 7 is electrically connected with a signal input end of the PLC, and a signal output end of the PLC is respectively electrically connected with the air inlet valve and the exhaust valve.
The pyrolysis operation is as follows: starting the stirring device 13, and injecting the qualified lithium bicarbonate solution into the pyrolysis kettle body 1 until the liquid level of the lithium bicarbonate solution rises to 2/3 of the volume of the pyrolysis kettle; at a rate of 1Kg/m 3 Adding the lithium bicarbonate solution, adding ultrapure lithium carbonate with the purity of more than 99.999 percent as seed crystal, and then adding carbon dioxide into the pyrolysis kettle body 1 through the air inlet 5 to ensure that the pressure in the kettle reaches 0.5-5Mpa; let in steam through steam pipe 12 to the cauldron and begin to heat up, through temperature sensor 11 monitoring, with temperature rise to more than 90 ℃ in the cauldron, the intensification in-process, solution becomes muddy gradually, and lithium carbonate is appeared, releases a large amount of carbon dioxide, must pass through opening and close of PLC controller control admission valve and discharge valve, makes the cauldron internal pressure keep at 0.5-5Mpa, specifically does: the pressure value in the pyrolysis kettle is preset through a PLC (programmable logic controller), when the pressure gauge 7 measures that the pressure in the kettle exceeds the preset value, a signal is transmitted to the PLC, and the PLC controls an exhaust valve on an exhaust port 6 to be opened to release the pressure; when the pressure gauge 7 measures that the pressure in the kettle is smaller than a preset value, a signal is transmitted to the PLC, the PLC controls the air inlet valve on the air inlet 5 to be opened, and carbon dioxide is supplemented, so that the pressure is constant at the preset value. Finally, when the temperature in the kettle rises to 95 ℃ and the pressure in the kettle does not change after 20min, manually opening an exhaust valve, drying the gas in the kettle by a gas dryer 9, introducing the gas into a carbonization kettle 10 for preparing a lithium bicarbonate solution, and discharging lithium carbonate slurry from the pyrolysis kettleThe port 3 is discharged to the centrifuge 4 for centrifugation, and when no water drops flow down from the liquid outlet of the centrifuge 4, the centrifuge 4 is closed to obtain wet lithium carbonate.
Example 1:
the method for preparing the ultrapure lithium carbonate with uniform and stable particle size provided by the embodiment comprises the following steps:
(1) Will be 5m 3 Is injected into the pure water of 8m 3 Starting stirring in the carbonization kettle, taking 237.6kg of battery-grade lithium carbonate (purity: 99.5%, moisture: 10%), adding a small amount of the battery-grade lithium carbonate into the carbonization kettle for many times, introducing carbon dioxide for reaction, testing the content of Li in the lithium bicarbonate solution when the solution is clear and transparent, purifying when the content of Li is 8g/L, and obtaining a purified solution which is a qualified lithium bicarbonate solution; purifying the lithium bicarbonate solution: (1) and (4) performing four-stage precise filtration on the qualified lithium bicarbonate solution prepared in the step one. The lithium bicarbonate solution was first passed through a 0.5 μm filter bag to filter out the larger particulate impurities. Then passed through a 0.05 micron filter cartridge to continue filtering out small particle impurities. And finally, the filter core passes through 2 channels of 0.01 micron filter elements continuously. (2) And (2) enabling the lithium bicarbonate solution filtered in the step (1) to pass through cation exchange resin, wherein the cation exchange resin is prepared by mixing a plurality of resins with strong specific ion exchange capacity, and adding the resins into an ion exchange column for use (such as Ca, mg and other ions difficult to remove impurities). Then, SO is removed by anion exchange resin 4 2- . (3) And the lithium bicarbonate after ion exchange passes through a filter element with the diameter of 0.01 mu m again to obtain qualified lithium bicarbonate solution.
(2) The stirring device 13 of the pyrolysis kettle is started to mix 2m 3 Injecting the qualified lithium bicarbonate solution into a pyrolysis kettle, and adding 2kg of ultrapure lithium carbonate with the purity of more than 99.999 percent as a crystal seed; then adding carbon dioxide into the closed pyrolysis kettle to enable the air pressure in the kettle to reach 3.5Mpa; and (3) starting to heat up, wherein the temperature is raised to 95 ℃ at the last step according to the temperature rise of 1 ℃/min, and the pressure in the pyrolysis kettle is controlled to be kept at 3.5MPa all the time. When the temperature is raised to 95 ℃ and the air pressure in the kettle is kept unchanged within 20min, manually opening an exhaust valve, drying the gas in the kettle by a gas dryer 9, introducing the gas into a carbonization kettle 10 for preparing a lithium bicarbonate solution, discharging lithium carbonate slurry from a liquid outlet 3 of a pyrolysis kettle to a centrifuge 4 for centrifugation, and discharging the liquid when the centrifuge 4 discharges the liquidWhen no water drops flow downwards, the centrifuge 4 is closed to obtain wet lithium carbonate, and the moisture content of the wet lithium carbonate is 4.9%.
(3) And washing the wet lithium carbonate with water at a solid-to-liquid ratio of 1:5 at 90 ℃ for 30min. And then, centrifuging again, wherein the water content of the lithium carbonate after centrifuging is 5 percent.
(4) And calcining the centrifuged lithium carbonate for 2 hours at the temperature of 450 ℃. The test purity after drying is 99.9992%, D10:2.2 μm, D50:4.6 μm, D90:10.8 μm.
Examples 2 to 12
Examples 2-12 the experimental procedures and the like were the same as in example 1 except that the pressure in the pyrolysis tank was changed by introducing carbon dioxide. The data pair ratios are shown in table 1.
TABLE 1 pressure in pyrolysis kettle and index for ultrapure lithium carbonate in examples 2-12
As can be seen from the data in Table 1, as the amount of carbon dioxide supplied to the pyrolysis kettle increases, the particle size of the prepared ultrapure lithium carbonate becomes smaller and smaller, and the particle size tends to the YS/T582-2013 standard. When the pressure is increased to 3.5Mpa, the granularity index completely meets the YS/T582-2013 standard, and the granularity change is not obvious when the pressure is continuously increased. Considering that the pressure is too large, the pyrolysis speed is slowed down, and the production efficiency and the production safety are affected. During pyrolysis of carbonization liquid obtained by 2m ethanol distillation, ultrapure lithium carbonate is preferably precipitated under the condition that the pressure is 3.5Mpa, and the particle size of the prepared ultrapure lithium carbonate meets the YS/T582-2013 standard. The purity is over 99.999 percent, and the chemical index is stable.
Examples 13 to 18
Examples 13-18 the procedure of example 1 was repeated except that example 1 was repeated to verify that the purity and particle size index of the ultra-pure lithium carbonate prepared by the process of controlling particle size by introducing carbon dioxide were stable, and the results are shown in table 2.
TABLE 2 index for ultrapure lithium carbonate in examples 13-18
As can be seen from the data in Table 2, the ultrapure lithium carbonate prepared by the method has uniform and stable granularity, the granularity index meets the YS/T582-2013 standard after repeated times, and the purity index is also stabilized to be more than 99.999%.
Comparative example 1: the pressure is adjusted without introducing carbon dioxide in the traditional process
(1) And (2) pouring pure water obtained by 5m flowering in a carbonization reaction kettle for carrying out ethanol distillation at 8m, starting stirring, adding 237.6kg of battery-grade lithium carbonate (purity: 99.5% and water content: 10%) into the carbonization reaction kettle for a small amount of times, introducing carbon dioxide for reaction, testing the content of Li in the lithium bicarbonate solution when the solution is clear and transparent, and purifying and removing impurities through ion exchange resin when the content of Li is 8g/L, wherein the purified solution is the qualified lithium bicarbonate solution. Purifying the lithium bicarbonate solution: (1) and (4) performing four-stage precise filtration on the qualified lithium bicarbonate solution prepared in the step one. The lithium bicarbonate solution was first passed through a 0.5 μm filter bag to filter out the larger particulate impurities. Then passed through a 0.05 micron filter cartridge to continue filtering out small particle impurities. And finally, the filter core passes through 2 channels of 0.01 micron filter elements continuously. (2) And (2) enabling the lithium bicarbonate solution filtered in the step (1) to pass through cation exchange resin, wherein the cation exchange resin is prepared by mixing a plurality of resins with strong specific ion exchange capacity, and adding the resins into an ion exchange column for use (such as Ca, mg and other ions difficult to remove impurities). Then, SO is removed by anion exchange resin 4 2- . (3) And the lithium bicarbonate after ion exchange passes through a filter element with the diameter of 0.01 mu m again to obtain a purified qualified lithium bicarbonate solution.
(2) And starting the pyrolysis reaction kettle for stirring, injecting the qualified lithium bicarbonate solution with the diameter of 2m into the pyrolysis kettle, and adding 2kg of seed crystal. And introducing steam into the top of the pyrolysis kettle to start heating, heating to 1 ℃/min to finally raise the temperature to 95 ℃, and preserving the temperature for 20min after the temperature in the kettle is raised to 95 ℃. The lithium carbonate slurry is then discharged from the pyrolysis kettle.
(3) And (3) performing solid-liquid separation on the lithium carbonate slurry in the step (2), separating by using a centrifugal machine, and closing the centrifugal machine when no water drops flow downwards from a liquid outlet of the centrifugal machine to obtain wet lithium carbonate, wherein the moisture content of the wet lithium carbonate is ensured to be 4.7%.
(4) And (3) washing the wet lithium carbonate in the step (3) with water according to the solid-to-liquid ratio of 1:5, wherein the water washing temperature is 90 ℃, and the water washing time is 30min. Then the mixture is centrifuged again, and the mixture is centrifuged again, the lithium carbonate moisture after centrifugation was 4.9%.
(5) And (4) calcining the lithium carbonate obtained in the step (4) for 2 hours at the temperature of 450 ℃. The index of the obtained ultrapure lithium carbonate is shown in table 3.
Comparative examples 2 to 6
Comparative examples 2 to 6 the other steps were the same as in comparative example 1 except that comparative example 1 was repeated to verify whether the purity and particle size indexes of ultrapure lithium carbonate prepared by the conventional process were stable, and the results are shown in table 3.
TABLE 3 index for ultrapure lithium carbonate in comparative examples 1-6
As can be seen from the data in Table 3, the particle size index of the ultrapure lithium carbonate prepared by the conventional pyrolysis method is unstable, suddenly increases and suddenly decreases, and the ultrapure lithium carbonate does not meet the YS/T582-2013 standard. And when the particle size is larger, the wrapped impurities are more, so that the purity of the prepared ultrapure lithium carbonate is unstable and sometimes is lower than the index of 99.999%.
Claims (6)
1. A method for preparing ultrapure lithium carbonate with uniform and stable particle size is characterized by comprising the following steps:
step one, preparing and purifying a lithium bicarbonate solution: injecting pure water into a carbonization kettle, starting stirring, adding battery-grade lithium carbonate, then introducing carbon dioxide to fully react, testing the Li content in the lithium bicarbonate solution when the solution is clear and transparent, purifying when the Li content is 8g/L, and obtaining a purified solution which is a qualified lithium bicarbonate solution;
step two, adopting a pyrolysis device to carry out pyrolysis: the pyrolysis device comprises a pyrolysis kettle body (1), wherein a liquid inlet (2), a steam pipe (12) and a stirring device (13) are arranged at the top of the pyrolysis kettle body (1), and a liquid outlet is arranged at the bottom of the pyrolysis kettle bodyThe liquid outlet (3) is communicated with the centrifugal machine (4); still be equipped with air inlet (5), gas vent (6), temperature sensor (11) and pressure gauge (7) on pyrolysis cauldron body (1), air inlet (5) and CO 2 The gas source (8) is communicated, the exhaust port (6) is sequentially communicated with the gas drier (9) and the carbonization kettle (10), and the gas inlet (5) and the exhaust port (6) are respectively provided with a gas inlet valve and an exhaust valve; the pressure gauge (7) is electrically connected with a signal input end of the PLC, and a signal output end of the PLC is electrically connected with the air inlet valve and the exhaust valve respectively;
the pyrolysis operation is as follows:
starting a stirring device (13), and injecting the qualified lithium bicarbonate solution in the step one into the pyrolysis kettle body (1) until the liquid level of the lithium bicarbonate solution rises to 2/3 of the volume of the pyrolysis kettle; at a rate of 1Kg/m 3 Adding the lithium bicarbonate solution, adding ultrapure lithium carbonate with the purity of more than 99.999 percent as a seed crystal, and then adding carbon dioxide into a pyrolysis kettle body (1) through an air inlet (5) to ensure that the pressure in the kettle reaches 0.5-5Mpa; introducing steam into the kettle through a steam pipe (12) to start heating, monitoring through a temperature sensor (11), heating the temperature in the kettle to be above 90 ℃, and controlling the opening and closing of an air inlet valve and an exhaust valve through a PLC (programmable logic controller) in the heating process to keep the pressure in the kettle at 0.5-5Mpa; when the temperature in the kettle rises to 95 ℃ and the pressure in the kettle does not change after 20min, manually opening an exhaust valve, drying the gas in the kettle by a gas dryer (9), and then introducing the gas into a carbonization kettle (10) for preparing a lithium bicarbonate solution, discharging lithium carbonate slurry from a liquid outlet (3) of the pyrolysis kettle to a centrifuge (4) for centrifugation, and when no water drops flow down from a liquid outlet of the centrifuge (4), closing the centrifuge (4) to obtain wet lithium carbonate;
step three, washing and centrifuging again: washing the wet lithium carbonate in the second step, and centrifuging again, wherein the water content in the centrifuged lithium carbonate is controlled to be less than or equal to 5%;
step four, calcining: calcining the lithium carbonate centrifuged in the third step for 2 hours at the temperature of 400-600 ℃ to obtain the ultrapure lithium carbonate with the purity of more than or equal to 99.999%.
2. The method of preparing ultrapure lithium carbonate having uniform and stable particle size according to claim 1 wherein the battery grade lithium carbonate has a purity of 99.5%.
3. The method of preparing ultrapure lithium carbonate having uniform and stable particle size according to claim 1, wherein in step two, the temperature increase rate is from 0.5 to 1 ℃/min.
4. The method of preparing ultrapure lithium carbonate having uniform and stable particle size according to claim 3 wherein said temperature increase rate is 1 ℃/min.
5. The method of preparing ultrapure lithium carbonate having uniform and stable particle size according to any one of claims 1 to 4, wherein in step two, the moisture content of the wet lithium carbonate after centrifugation is less than or equal to 5%.
6. The method of preparing ultrapure lithium carbonate having uniform and stable particle size according to any one of claims 1 to 4, wherein in step three, the solid-to-liquid ratio of the wet lithium carbonate water washing is 1:5.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4124684A (en) * | 1976-08-10 | 1978-11-07 | Ministere Des Richesses Naturelles, Gouvernement Du Quebec | Continuous production of lithium carbonate |
| CN103833053A (en) * | 2014-01-21 | 2014-06-04 | 四川天齐锂业股份有限公司 | Method of preparing high-purity lithium carbonate of the 5 N grade |
| CN106365182A (en) * | 2016-08-30 | 2017-02-01 | 荆门市格林美新材料有限公司 | Method for preparing battery grade lithium carbonate by using impulse type hydrogenated industrial grade lithium carbonate |
| WO2018234614A1 (en) * | 2017-06-22 | 2018-12-27 | Outotec (Finland) Oy | Method of extracting lithium compound(s) |
| CN114477245A (en) * | 2022-02-24 | 2022-05-13 | 宁夏天霖新材料科技有限公司 | Method for preparing lithium carbonate of battery by continuously carbonizing industrial-grade lithium carbonate |
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- 2022-12-22 CN CN202211654559.7A patent/CN115849414B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4124684A (en) * | 1976-08-10 | 1978-11-07 | Ministere Des Richesses Naturelles, Gouvernement Du Quebec | Continuous production of lithium carbonate |
| CN103833053A (en) * | 2014-01-21 | 2014-06-04 | 四川天齐锂业股份有限公司 | Method of preparing high-purity lithium carbonate of the 5 N grade |
| CN106365182A (en) * | 2016-08-30 | 2017-02-01 | 荆门市格林美新材料有限公司 | Method for preparing battery grade lithium carbonate by using impulse type hydrogenated industrial grade lithium carbonate |
| WO2018234614A1 (en) * | 2017-06-22 | 2018-12-27 | Outotec (Finland) Oy | Method of extracting lithium compound(s) |
| CN114477245A (en) * | 2022-02-24 | 2022-05-13 | 宁夏天霖新材料科技有限公司 | Method for preparing lithium carbonate of battery by continuously carbonizing industrial-grade lithium carbonate |
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