CN114291831A - Method for producing battery-grade lithium carbonate by continuously precipitating lithium through extracting lithium from lepidolite - Google Patents
Method for producing battery-grade lithium carbonate by continuously precipitating lithium through extracting lithium from lepidolite Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 174
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 174
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 60
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 229910052629 lepidolite Inorganic materials 0.000 title claims abstract description 26
- 230000001376 precipitating effect Effects 0.000 title claims abstract description 20
- 230000032683 aging Effects 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002386 leaching Methods 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 136
- 238000006243 chemical reaction Methods 0.000 claims description 76
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 68
- 238000003756 stirring Methods 0.000 claims description 58
- 238000001556 precipitation Methods 0.000 claims description 46
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 8
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 230000002431 foraging effect Effects 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000010924 continuous production Methods 0.000 abstract description 4
- 238000005137 deposition process Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000012423 maintenance Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of lithium carbonate production, and particularly relates to a method for producing battery-grade lithium carbonate by continuously precipitating lithium by extracting lithium from lepidolite, which comprises the following specific steps of: mixing materials, molding, roasting, leaching, concentrating, separating, removing impurities, precipitating lithium, aging, washing lithium, drying, crushing and packaging to obtain the battery-grade lithium carbonate. The invention realizes continuous production by adopting the continuous lithium deposition process, can improve the production efficiency and the product quality stability, has large yield, can save equipment investment, equipment maintenance cost and labor cost, achieves the purposes of cost reduction, efficiency improvement and energy saving, and has good economic benefit.
Description
Technical Field
The invention belongs to the technical field of lithium carbonate production, and particularly relates to a method for producing battery-grade lithium carbonate by continuously precipitating lithium by extracting lithium from lepidolite.
Background
With the development of new energy, the market demand of lithium carbonate will be explosively increased. Lithium ore resources are rich in China, lithium extraction from lithium ore is the main mode for obtaining lithium carbonate at present, and the lithium is generally obtained by destroying the original ore structure of spodumene, lepidolite and other ores containing high lithium in a high-temperature and grinding mode, dissolving lithium out in a soluble lithium salt mode and then precipitating the lithium.
Lithium carbonate is used as a positive electrode material for synthesizing various lithium batteries, and the quality of lithium carbonate is also very required in use. At present, in order to obtain the lithium carbonate meeting the electrode material, the lithium deposition process in production generally adopts intermittent production or multiple lithium deposition modes, so that the manufacturing process of the lithium carbonate is more complicated and long in time, high in energy consumption and low in yield, cannot meet the requirement of high yield, and is not beneficial to the development of enterprises.
The invention patent with the application number of 201710953038.4 discloses a continuous lithium precipitation tank and a continuous lithium precipitation process for battery lithium carbonate, wherein although the continuous lithium precipitation tank is used for precipitating lithium, a soda lye inlet and a concentrated lithium sulfate purifying solution inlet are far away from each other and are added in sequence, so that the contact between the soda lye and the lithium solution is not facilitated, the agglomeration is easy to form, the reaction is insufficient, and the product quality is influenced.
Disclosure of Invention
The invention aims to provide a method for producing battery-grade lithium carbonate by continuously precipitating lithium by extracting lithium from lepidolite, which can continuously react in a lithium precipitation process, has high capacity and can save equipment investment, and simultaneously, the lithium solution and the sodium carbonate solution are simultaneously added to a set position, are in timely contact, fully react, have good product quality stability, can reduce labor input, save energy, reduce consumption and have good economic benefit.
A method for producing battery-grade lithium carbonate by continuously precipitating lithium by extracting lithium from lepidolite comprises the following specific steps:
s1, mixing lepidolite and auxiliary materials, forming, roasting, leaching, removing impurities, concentrating, and treating with ion resin exchange resin to obtain a lithium solution;
s2, dissolving sodium carbonate with water, and precisely filtering to obtain a sodium carbonate solution;
s3, continuously and parallelly flowing the lithium solution of S1 and the sodium carbonate solution of S2 into a lithium precipitation reaction kettle through adjacent pipelines, accurately measuring the adding amount and flow rate of the lithium solution and the sodium carbonate solution, then heating the lithium precipitation reaction kettle, controlling the temperature to be 80-100 ℃, and rapidly stirring and mixing through a stirring paddle for reaction;
s4, the solution after the mixed reaction of S3 overflows along an overflow port at the upper part of the lithium precipitation reaction kettle and flows into an aging kettle for aging;
s5, separating the lithium carbonate slurry in the aging kettle of S4 through a centrifugal machine to obtain a lithium carbonate wet material;
and S6, washing lithium from the lithium carbonate wet material obtained in the step S5 with pure water, centrifuging, drying, crushing and packaging to obtain a finished product of battery-grade lithium carbonate.
According to the technical scheme, the lithium solution and the lithium carbonate solution are continuously added through adjacent pipelines by adopting a continuous lithium deposition process, so that the reaction is timely and sufficient, agglomeration is not formed, the reduction of the wrapping of impurity ions is facilitated, and the production efficiency and the product quality are improved; meanwhile, the continuous production can effectively reduce the occurrence of equipment scaling phenomenon, reduce the equipment maintenance cost and frequent operation of staff, save energy and reduce consumption.
Preferably, in the above technical solution S1, the concentration of lithium oxide in the lithium solution is controlled to be 25 to 50 g/L.
Preferably, in the technical scheme S2, the concentration of sodium carbonate in the sodium carbonate solution is controlled to be 15-30%.
Preferably, in the above technical solution S3, the addition amounts of the lithium solution and the sodium carbonate solution are calculated according to the molar ratio of substance n lithium oxide: n sodium carbonate 1: 1.05 plus or minus 0.1; the flow rates of the lithium solution and the sodium carbonate solution are less than or equal to 10.0m3H; and controlling the pH of the reaction liquid to be between 11 and 14 in the mixed reaction. According to the technical scheme, according to the lithium precipitation reaction principle, the reaction is more sufficient and the obtained product is purer by controlling the molar ratio and the flow of the lithium solution and the sodium carbonate solution.
Preferably, in the above technical scheme, a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, an upper layer of blade and a lower layer of blade are respectively arranged in the middle and at the bottom of the stirring paddle, pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right below the bottom blade, and the bottom blade is installed in an upward pushing manner.
This technical scheme is for sinking one of lithium reaction stirring mode, through the pipeline entry adjacent setting with lithium solution and sodium carbonate solution under the bottom blade, the blade is the push-up formula, is sent to the upper portion of sinking lithium reation kettle after the solution reaction is accomplished, then flows to next production processes through the overflow mouth, and reaction rate is fast, can realize continuity production, saves and sinks the lithium time.
Preferably, in the above technical scheme, a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, an upper layer of blade and a lower layer of blade are respectively arranged in the middle and at the bottom of the stirring paddle, pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right above the bottom blade, and the bottom blade is installed in a downward pushing manner.
This technical scheme is for sinking lithium reaction stirring mode two, through the adjacent setting directly over the bottom blade of pipeline entry with lithium solution and sodium carbonate solution, the blade is the push down formula, and solution pushes down through the blade, and the back is accomplished in the reaction, upwards along sinking lithium reation kettle's lateral wall, then flows to next production processes through the overflow mouth, and reaction rate is fast, can realize continuity production, saves and sinks the lithium time.
Preferably, in the above technical scheme, a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, an upper layer of blade and a lower layer of blade are respectively arranged in the middle and at the bottom of the stirring paddle, pipeline inlets for the lithium solution and the sodium carbonate solution are adjacently arranged right below the middle blade, and the middle blade is installed in a downward pushing manner.
This technical scheme is three for sinking lithium reaction stirring mode, through the adjacent setting under the middle part blade of the pipeline entry with lithium solution and sodium carbonate solution, the blade is the push down formula, and solution passes through the blade and pushes down, and the back is accomplished in the reaction, and it is direct upwards or upwards along the lateral wall that sinks lithium reation kettle to promote through bottom blade, then flows to next production processes through the overflow mouth, and reaction rate is fast, can realize continuity production, saves and sinks the lithium time.
Preferably, in the above technical scheme, a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, an upper layer of blade and a lower layer of blade are respectively arranged in the middle and at the bottom of the stirring paddle, an inverted trapezoidal central cylinder is sleeved outside the middle blade, pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right above the inverted trapezoidal central cylinder, and the middle blade is installed in a downward pushing manner.
This technical scheme is four for sinking lithium reaction stirring mode, through adjacent setting up the pipeline entry with lithium solution and sodium carbonate solution directly over the hollow center section of thick bamboo of falling trapezoidal, the blade is the push down formula, after solution entered into the center section of thick bamboo, push down through the blade, at the interior pre-reaction of center section of thick bamboo, then flow downwards, it is direct upwards or upwards along the lateral wall that sinks lithium reation kettle to promote through bottom blade, then flow to next production process through the overflow mouth, the reaction rate is fast, can realize continuity of production, save and sink the lithium time.
Preferably, in the above technical scheme, in S4, the temperature of the aging kettle is 80-100 ℃, and the aging time is 20-120 min.
The invention also provides a continuous lithium precipitation reaction kettle, which comprises a tank body 1, a stirring paddle 2, a heating plate 3 and an overflow port 4, wherein the stirring paddle 2 is arranged in the middle of the tank body 1, the lower part of the stirring paddle 2 extends to the bottom of the tank body 1, the middle part and the bottom of the stirring paddle 2 are respectively provided with a middle blade 5 and a bottom blade 6, and the access ports of a lithium solution pipe 7 and a sodium carbonate solution pipe 8 are respectively adjacently arranged right above or right below the bottom blade 6 or right below the middle blade 5; the heating plate 3 is arranged on the side wall of the tank body 1, and the overflow port 4 is arranged on the upper part of the side wall of the tank body 1 and communicated with an aging tank of the next working procedure.
Compared with the prior art, the method has the beneficial effects that:
1. according to the invention, by accurately measuring the molar ratio and the feeding flow rate of the lithium solution and the sodium carbonate solution, and adjacently arranging inlets of two reaction liquids at different parts of the stirring paddle blade and adjusting the installation mode of the blade, the purposes of quick reaction and quick transfer of the reaction liquids are achieved, the product quality is finally improved, and continuous production is realized.
2. According to the invention, two reaction liquids are adjacently arranged, so that the reaction liquids are contacted in time, the reaction is fast, no agglomeration is formed, the impurity ion wrapping is reduced, and the product quality is improved;
3. the invention adopts the continuous lithium deposition process to realize continuous production, can improve the production efficiency, increase the yield, save the equipment investment, the equipment maintenance cost and the labor cost, achieve the purposes of cost reduction, efficiency improvement and energy saving, and have good economic benefit.
Drawings
FIG. 1 is a flow chart of a process for producing battery-grade lithium carbonate by continuously depositing lithium according to the present invention;
FIG. 2 is a schematic structural diagram of a continuous lithium precipitation reaction kettle in example 1 of the present invention;
FIG. 3 is a schematic structural diagram of a continuous lithium precipitation reaction kettle in example 2 of the present invention;
FIG. 4 is a schematic structural diagram of a continuous lithium precipitation reaction kettle in example 3 of the present invention;
FIG. 5 is a schematic structural diagram of a continuous lithium deposition reaction kettle in example 4 of the present invention.
Number designations in the schematic drawings illustrate that:
1. a tank body; 2. a stirring paddle; 3. heating plates; 4. an overflow port; 5. a middle blade; 6 bottom blade; 7. a lithium solution tube; 8. a sodium carbonate solution pipe; 9. a central cartridge.
Detailed Description
The technical features of the present invention described above and those described in detail below (as an embodiment) can be combined with each other to form a new or preferred technical solution, but the present invention is not limited to these embodiments, and the embodiments also do not limit the present invention in any way.
The experimental procedures in the following examples are conventional unless otherwise specified. The formulations according to the following examples are all commercially available products and are commercially available, unless otherwise specified.
The invention is described in further detail below with reference to the figures and examples:
example 1
A continuous lithium precipitation reaction kettle is shown in figure 2 and comprises a tank body 1, a stirring paddle 2, a heating plate 3 and an overflow port 4, wherein the stirring paddle 2 is arranged in the middle of the tank body 1, the lower part of the stirring paddle 2 extends to the bottom of the tank body 1, a middle blade 5 and a bottom blade 6 are respectively arranged in the middle and at the bottom of the stirring paddle 2, and access ports of a lithium solution pipe 7 and a sodium carbonate solution pipe 8 are respectively adjacently arranged right below the bottom blade 6; the heating plate 3 is arranged on the side wall of the tank body 1, and the overflow port 4 is arranged on the upper part of the side wall of the tank body 1 and communicated with an aging tank of the next working procedure.
Example 2
A continuous lithium precipitation reaction kettle is shown in figure 3 and comprises a tank body 1, a stirring paddle 2, a heating plate 3 and an overflow port 4, wherein the stirring paddle 2 is arranged in the middle of the tank body 1, the lower part of the stirring paddle 2 extends to the bottom of the tank body 1, a middle blade 5 and a bottom blade 6 are respectively arranged in the middle and at the bottom of the stirring paddle 2, and access ports of a lithium solution pipe 7 and a sodium carbonate solution pipe 8 are respectively adjacently arranged right above the bottom blade 6; the heating plate 3 is arranged on the side wall of the tank body 1, and the overflow port 4 is arranged on the upper part of the side wall of the tank body 1 and communicated with an aging tank of the next working procedure.
Example 3
A continuous lithium precipitation reaction kettle is shown in figure 4 and comprises a tank body 1, a stirring paddle 2, a heating plate 3 and an overflow port 4, wherein the stirring paddle 2 is arranged in the middle of the tank body 1, the lower part of the stirring paddle 2 extends to the bottom of the tank body 1, a middle blade 5 and a bottom blade 6 are respectively arranged in the middle and at the bottom of the stirring paddle 2, and access ports of a lithium solution pipe 7 and a sodium carbonate solution pipe 8 are respectively adjacently arranged under the middle blade 5; the heating plate 3 is arranged on the side wall of the tank body 1, and the overflow port 4 is arranged on the upper part of the side wall of the tank body 1 and communicated with an aging tank of the next working procedure.
Example 4
A continuous lithium precipitation reaction kettle is shown in figure 5 and comprises a tank body 1, a stirring paddle 2, a heating plate 3 and an overflow port 4, wherein the stirring paddle 2 is arranged in the middle of the tank body 1, the lower part of the stirring paddle 2 extends to the bottom of the tank body 1, a middle blade 5 and a bottom blade 6 are respectively arranged in the middle and at the bottom of the stirring paddle 2, an inverted trapezoidal hollow central cylinder 9 is sleeved outside the middle blade, and access ports of a lithium solution pipe 7 and a sodium carbonate solution pipe 8 are respectively adjacently arranged right above the central cylinder 9; the heating plate 3 is arranged on the side wall of the tank body 1, and the overflow port 4 is arranged on the upper part of the side wall of the tank body 1 and communicated with an aging tank of the next working procedure.
Example 5
A method for producing battery-grade lithium carbonate by continuously precipitating lithium by extracting lithium from lepidolite adopts the preparation of the continuous lithium precipitation reaction kettle in the embodiment 1, and comprises the following specific steps, wherein the flow chart is shown in figure 1:
s1, mixing lepidolite and auxiliary materials, forming, roasting, leaching, impurity removal, concentration and ion resin exchange resin treatment to obtain a lithium solution, wherein the concentration of lithium oxide in the lithium solution is controlled to be 25-50 g/L;
s2, dissolving sodium carbonate with water, and performing precision filtration to obtain a sodium carbonate solution, wherein the concentration of sodium carbonate in the sodium carbonate solution is controlled to be 15-30%;
s3, continuously and parallelly flowing the lithium solution of S1 and the sodium carbonate solution of S2 into a lithium precipitation reaction kettle through adjacent pipelines, accurately metering the adding amount and flow rate of the lithium solution and the sodium carbonate solution, and oxidizing lithium according to a substance molar ratio n: n sodium carbonate 1: ratio of 1.05 + -0.1 and flow rate of 5.0m3Adding the solution for one hour, heating the lithium precipitation reaction kettle to 80 ℃, rapidly stirring and mixing the solution for reaction by a stirring paddle, and controlling the pH value of the reaction solution to be 11-14;
s4, overflowing the solution after the mixed reaction of S3 along an overflow port at the upper part of the lithium precipitation reaction kettle, flowing into an aging kettle for aging, controlling the temperature of the aging kettle at 80 ℃, and the aging time at 100 min;
s5, separating the lithium carbonate slurry in the aging kettle of S4 through a centrifugal machine to obtain a lithium carbonate wet material;
and S6, washing lithium from the lithium carbonate wet material obtained in the step S5 with pure water, centrifuging, drying, crushing and packaging to obtain a finished product of battery-grade lithium carbonate.
Example 6
A method for producing battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction adopts the continuous lithium precipitation reaction kettle in the embodiment 2 to prepare, and comprises the following specific steps:
s1, mixing lepidolite and auxiliary materials, forming, roasting, leaching, impurity removal, concentration and ion resin exchange resin treatment to obtain a lithium solution, wherein the concentration of lithium oxide in the lithium solution is controlled to be 25-50 g/L;
s2, dissolving sodium carbonate with water, and performing precision filtration to obtain a sodium carbonate solution, wherein the concentration of sodium carbonate in the sodium carbonate solution is controlled to be 15-30%;
s3, mixing the lithium solution of S1 withAnd S2, continuously and parallelly flowing the sodium carbonate solution into a lithium precipitation reaction kettle through adjacent pipelines, accurately metering the adding amount and flow rate of the lithium solution and the sodium carbonate solution, and performing mass molar ratio n-lithium oxide: n sodium carbonate 1: ratio of 1.05 + -0.1 and flow rate of 6.0m3Adding the solution for one hour, heating the lithium precipitation reaction kettle to 85 ℃, rapidly stirring and mixing the solution for reaction by a stirring paddle, and controlling the pH value of the reaction solution to be 11-14;
s4, overflowing the solution after the mixed reaction of S3 along an overflow port at the upper part of the lithium precipitation reaction kettle, flowing into an aging kettle for aging, controlling the temperature of the aging kettle at 85 ℃ and the aging time at 60 min;
s5, separating the lithium carbonate slurry in the aging kettle of S4 through a centrifugal machine to obtain a lithium carbonate wet material;
and S6, washing lithium from the lithium carbonate wet material obtained in the step S5 with pure water, centrifuging, drying, crushing and packaging to obtain a finished product of battery-grade lithium carbonate.
Example 7
A method for producing battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction adopts the continuous lithium precipitation reaction kettle in the embodiment 3 to prepare, and comprises the following specific steps:
s1, mixing lepidolite and auxiliary materials, forming, roasting, leaching, impurity removal, concentration and ion resin exchange resin treatment to obtain a lithium solution, wherein the concentration of lithium oxide in the lithium solution is controlled to be 25-50 g/L;
s2, dissolving sodium carbonate with water, and performing precision filtration to obtain a sodium carbonate solution, wherein the concentration of sodium carbonate in the sodium carbonate solution is controlled to be 15-30%;
s3, continuously and parallelly flowing the lithium solution of S1 and the sodium carbonate solution of S2 into a lithium precipitation reaction kettle through adjacent pipelines, accurately metering the adding amount and flow rate of the lithium solution and the sodium carbonate solution, and oxidizing lithium according to a substance molar ratio n: n sodium carbonate 1: ratio of 1.05 + -0.1 and flow rate of 8.0m3Adding the solution for one hour, heating the lithium precipitation reaction kettle to 90 ℃, rapidly stirring and mixing the solution for reaction by a stirring paddle, and controlling the pH value of the reaction solution to be 11-14;
s4, overflowing the solution after the mixed reaction of S3 along an overflow port at the upper part of the lithium precipitation reaction kettle, flowing into an aging kettle for aging, controlling the temperature of the aging kettle at 90 ℃ and the aging time at 40 min;
s5, separating the lithium carbonate slurry in the aging kettle of S4 through a centrifugal machine to obtain a lithium carbonate wet material;
and S6, washing lithium from the lithium carbonate wet material obtained in the step S5 with pure water, centrifuging, drying, crushing and packaging to obtain a finished product of battery-grade lithium carbonate.
Example 8
A method for producing battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction adopts the continuous lithium precipitation reaction kettle in the embodiment 4 to prepare, and comprises the following specific steps:
s1, mixing lepidolite and auxiliary materials, forming, roasting, leaching, impurity removal, concentration and ion resin exchange resin treatment to obtain a lithium solution, wherein the concentration of lithium oxide in the lithium solution is controlled to be 25-50 g/L;
s2, dissolving sodium carbonate with water, and performing precision filtration to obtain a sodium carbonate solution, wherein the concentration of sodium carbonate in the sodium carbonate solution is controlled to be 15-30%;
s3, continuously and parallelly flowing the lithium solution of S1 and the sodium carbonate solution of S2 into a lithium precipitation reaction kettle through adjacent pipelines, accurately metering the adding amount and flow rate of the lithium solution and the sodium carbonate solution, and oxidizing lithium according to a substance molar ratio n: n sodium carbonate 1: ratio of 1.05 +/-0.1 and flow rate of 10.0m3Adding the solution for one hour, heating the lithium precipitation reaction kettle to 100 ℃, rapidly stirring and mixing the solution for reaction by a stirring paddle, and controlling the pH value of the reaction solution to be 11-14;
s4, overflowing the solution after the mixed reaction of S3 along an overflow port at the upper part of the lithium precipitation reaction kettle, flowing into an aging kettle for aging, controlling the temperature of the aging kettle at 100 ℃ and the aging time at 20 min;
s5, separating the lithium carbonate slurry in the aging kettle of S4 through a centrifugal machine to obtain a lithium carbonate wet material;
and S6, washing lithium from the lithium carbonate wet material obtained in the step S5 with pure water, centrifuging, drying, crushing and packaging to obtain a finished product of battery-grade lithium carbonate.
The lithium carbonate content of the battery grade lithium carbonate products prepared in examples 5-8 was measured and the results are shown in table 1.
TABLE 1
| Group of | Li2CO3(％) |
| Example 5 | 99.87 |
| Example 6 | 99.91 |
| Example 7 | 99.85 |
| Example 8 | 99.92 |
From the results in table 1, it can be seen that the quality of the battery-grade lithium carbonate obtained by the method for producing the battery-grade lithium carbonate by continuously depositing lithium is good.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (10)
1. A method for producing battery-grade lithium carbonate by continuously precipitating lithium by extracting lithium from lepidolite is characterized by comprising the following specific steps of:
s1, mixing lepidolite and auxiliary materials, forming, roasting, leaching, removing impurities, concentrating, and treating with ion resin exchange resin to obtain a lithium solution;
s2, dissolving sodium carbonate with water, and precisely filtering to obtain a sodium carbonate solution;
s3, continuously and parallelly flowing the lithium solution of S1 and the sodium carbonate solution of S2 into a lithium precipitation reaction kettle through adjacent pipelines, accurately measuring the adding amount and flow rate of the lithium solution and the sodium carbonate solution, then heating the lithium precipitation reaction kettle, controlling the temperature to be 80-100 ℃, and rapidly stirring and mixing through a stirring paddle for reaction;
s4, the solution after the mixed reaction of S3 overflows along an overflow port at the upper part of the lithium precipitation reaction kettle and flows into an aging kettle for aging;
s5, separating the lithium carbonate slurry in the aging kettle of S4 through a centrifugal machine to obtain a lithium carbonate wet material;
and S6, washing lithium from the lithium carbonate wet material obtained in the step S5 with pure water, centrifuging, drying, crushing and packaging to obtain a finished product of battery-grade lithium carbonate.
2. The method for producing the battery-grade lithium carbonate by continuously precipitating the lithium by extracting the lithium from the lepidolite as claimed in claim 1, wherein in S1, the concentration of the lithium oxide in the lithium solution is controlled to be 25-50 g/L.
3. The method for producing the battery-grade lithium carbonate by continuously precipitating the lithium by lepidolite lithium extraction according to claim 1, wherein the concentration of sodium carbonate in the sodium carbonate solution is controlled to be 15-30% in S2.
4. The method for producing battery-grade lithium carbonate through continuous lithium precipitation by lepidolite lithium extraction according to claim 1, wherein in S3, the lithium solution and the sodium carbonate solution are added according to a mass molar ratio of lithium oxide: n sodium carbonate 1: 1.05 plus or minus 0.1; the flow rates of the lithium solution and the sodium carbonate solution are less than or equal to 10.0m3H; and controlling the pH of the reaction liquid to be between 11 and 14 in the mixed reaction.
5. The method for producing the battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction according to claim 4, wherein a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, the middle part and the bottom of the stirring paddle are respectively provided with an upper layer blade and a lower layer blade, pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right below the bottom blades, and the bottom blades are installed to push upwards.
6. The method for producing the battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction according to claim 4, wherein the lithium precipitation reaction kettle is provided with a stirring paddle in the middle, the stirring paddle is provided with an upper layer of blade and a lower layer of blade in the middle and at the bottom, the pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right above the bottom blade, and the bottom blade is installed in a downward pushing mode.
7. The method for producing the battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction according to claim 4, wherein a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, the middle part and the bottom of the stirring paddle are respectively provided with an upper layer blade and a lower layer blade, pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right below the middle blades, and the middle blades are installed to push downwards.
8. The method for producing battery-grade lithium carbonate by continuously precipitating lithium through lepidolite lithium extraction according to claim 4, wherein a stirring paddle is arranged in the middle of the lithium precipitation reaction kettle, the middle part and the bottom of the stirring paddle are respectively provided with an upper layer of blade and a lower layer of blade, an inverted trapezoidal hollow central cylinder is sleeved outside the middle blade, pipeline inlets of the lithium solution and the sodium carbonate solution are adjacently arranged right above the inverted trapezoidal central cylinder, and the middle blade is installed to push downwards.
9. The method for producing battery-grade lithium carbonate through continuous lithium precipitation by lepidolite lithium extraction according to claim 1, wherein in S4, the temperature of the aging kettle is 80-100 ℃, and the aging time is 20-120 min.
10. The continuous lithium precipitation reaction kettle is characterized by comprising a tank body (1), a stirring paddle (2), a heating plate (3) and an overflow port (4), wherein the stirring paddle (2) is arranged in the middle of the tank body (1), the lower part of the stirring paddle extends to the bottom of the tank body (1), a middle blade (5) and a bottom blade (6) are respectively arranged at the middle part and the bottom of the stirring paddle (2), and access ports of a lithium solution pipe (7) and a sodium carbonate solution pipe (8) are respectively adjacently arranged right above or right below the bottom blade (6) or right below the middle blade (5); the heating plate (3) is arranged on the side wall of the tank body (1), and the overflow port (4) is arranged on the upper part of the side wall of the tank body (1) and communicated with an aging tank in the next working procedure.
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