CN106654265A - Method for preparing battery level micrometer lithium carbonate - Google Patents
Method for preparing battery level micrometer lithium carbonate Download PDFInfo
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- CN106654265A CN106654265A CN201710149064.1A CN201710149064A CN106654265A CN 106654265 A CN106654265 A CN 106654265A CN 201710149064 A CN201710149064 A CN 201710149064A CN 106654265 A CN106654265 A CN 106654265A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses a method for preparing battery level micrometer lithium carbonate. The method comprises the following steps: A. preparing an aqueous solution by using a water soluble lithium salt, and obtaining a first solution, wherein the concentration of Li + in the first solution is 0.5-6mo/L; B. preparing an aqueous solution by using water soluble carbonate, and obtaining a second solution, wherein the concentration of CO32- in the second solution is 0.5-3mo/L; C. dissolving a dispersing agent in polyhydric alcohol to obtain a third solution; D. adding the first solution and the second solution to the third solution to obtain a fourth solution; E. mixing the fourth solution at 30-70 DEG C, and reacting for 1-3h to obtain turbid liquid; and F. performing solid-liquid separation on the turbid liquid to obtain filtrate and filter cakes, and washing and drying the filter cakes to obtain the battery level micrometer lithium carbonate. The preparation method according to the invention is simple in process, the obtained battery level micrometer lithium carbonate has good degree of crystallinity, good dispersibility and high purity, and the preparation method is beneficial for the application and promotion of the battery level micrometer lithium carbonate in cutting-edge industries.
Description
Technical field
The invention belongs to battery material technical field, it relates in particular to a kind of preparation side of LITHIUM BATTERY micron lithium carbonate
Method.
Background technology
Lithium carbonate be lithium salts industry basic material, not only can directly use, be also used as raw material prepare it is various attached
Value added high lithium salts and its compound.Colored phosphor powder, medicinal and lithium battery electronic material such as in high-tech application field
Very high Deng field, the i.e. requirement to lithium carbonate quality, industrial level lithium carbonate cannot be directly used to produce lithium battery, it is necessary to by essence
System removes the different quality index request that the impurity such as inorganic salts therein can be only achieved various special products.
With the development of lithium ion battery, market is bigger to the demand of lithium ion battery, according to LITHIUM BATTERY micro mist lithium carbonate
The quality requirement of special product, with reference to the market demand, prepares the high LITHIUM BATTERY micron lithium carbonate of good dispersion, purity and seems more
Come more important.
The content of the invention
To solve the problems, such as above-mentioned prior art, the invention provides a kind of preparation side of LITHIUM BATTERY micron lithium carbonate
Method, the preparation method process is simple, the better crystallinity degree of the LITHIUM BATTERY micron lithium carbonate of acquisition, good dispersion, purity are high.
In order to reach foregoing invention purpose, following technical scheme is present invention employs：
A kind of preparation method of LITHIUM BATTERY micron lithium carbonate, including step：A, water-soluble lithium salts is configured into the aqueous solution, is obtained
The first solution is obtained, wherein, Li in first solution+Concentration is 0.5mol/L～6mol/L；B, water soluble carbonate is prepared
Into the aqueous solution, the second solution is obtained, wherein, CO in second solution3 2-Concentration is 0.5mol/L～3mol/L；C, will dispersion
Agent is dissolved in polyalcohol, obtains the 3rd solution；D, add in the 3rd solution first solution and described second molten
Liquid, obtains the 4th solution；E, the 4th solution mix and react 1h～3h at 30 DEG C～70 DEG C, obtain suspension；F, general
The suspension carries out separation of solid and liquid, obtains filtrate and filter cake, and the filter cake is scrubbed, be dried acquisition LITHIUM BATTERY micron carbonic acid
Lithium.
Further, the dispersant is the polyethylene glycol that the degree of polymerization is 1000～6000, and the quality of the dispersant
For the 1%～7% of the quality of the water-soluble lithium salts.
Further, the polyalcohol is any one in ethylene glycol, propane diols, glycerine, diethylene glycol (DEG).
Further, in the 4th solution, CO3 2-Substance withdrawl syndrome and Li+Substance withdrawl syndrome ratio not
Less than 1:2.
Further, at least one of the water-soluble lithium salts in lithium chloride, lithium nitrate, lithium sulfate.
Further, at least one of the water soluble carbonate in sodium carbonate, ammonium carbonate.
Further, in step F, the filter cake 2 times is first washed with deionized, then uses absolute ethanol washing institute
State filter cake 1 time～2 times.
Further, in step F, at least 12h will be dried at 50 DEG C through the filter cake of washing, obtains the electricity
Pond level micron lithium carbonate.
Further, the volume of the polyalcohol is 1/2～1 times of the volume of first solution.
Further, in step E, the suspension is aged into 1.5h～2.5h.
Beneficial effects of the present invention：
(1) preparation in accordance with the present invention using polyalcohol as solvent, it is to avoid using water as molten in prior art
Existing during agent hydroxyl effect and capillarity and caused agglomeration, the LITHIUM BATTERY micron that the Jing preparation methods are obtained
The dispersiveness of lithium carbonate is more preferably；
(2) preparation in accordance with the present invention is using water-soluble lithium salts as lithium source, using water soluble carbonate as precipitating reagent,
Using polyalcohol-polyethylene glycol as dispersant, using sluggish precipitation, the effective control nucleation of lithium carbonate, crystallization process are carried
The purity and dispersiveness of high LITHIUM BATTERY micron lithium carbonate；
(3) preparation in accordance with the present invention process is simple, the better crystallinity degree of the LITHIUM BATTERY micron lithium carbonate of acquisition, dispersion
The good, purity of property is high, and the preparation method is conducive to LITHIUM BATTERY micron lithium carbonate to sophisticated sector application and popularization.
Description of the drawings
By combining the following description that accompanying drawing is carried out, above and other aspect of embodiments of the invention, feature and advantage
Will become clearer from, in accompanying drawing：
Fig. 1 is the XRD piece of the LITHIUM BATTERY micron lithium carbonate of embodiments in accordance with the present invention 2；
Fig. 2 is the SEM pictures of the LITHIUM BATTERY micron lithium carbonate of embodiments in accordance with the present invention 2；
Fig. 3 is the SEM pictures of the LITHIUM BATTERY micron lithium carbonate of embodiments in accordance with the present invention 3.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to describing embodiments of the invention in detail.However, it is possible to come real in many different forms
Apply the present invention, and the present invention should not be construed as limited to the specific embodiment that illustrates here.On the contrary, there is provided these enforcements
Example is in order to explain the principle and its practical application of the present invention, so that others skilled in the art are it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
It will be appreciated that although here various materials can be described using term " first ", " second " etc., these
Material should not be limited by these terms.These terms are only used for making a distinction a material and another material.
The invention discloses a kind of preparation method of LITHIUM BATTERY micron lithium carbonate, it specifically includes following step：
Step S1, water-soluble lithium salts is configured to the aqueous solution, obtains the first solution, wherein, Li in the first solution+Concentration is
0.5mol/L～6mol/L.
Specifically, water-soluble lithium salts can be at least one in lithium chloride, lithium nitrate, lithium sulfate.
Step S2, water soluble carbonate is configured to the aqueous solution, obtains the second solution, wherein, CO in the second solution3 2-It is dense
Spend for 0.5mol/L～3mol/L.
Specifically, water soluble carbonate can be at least one in sodium carbonate, ammonium carbonate.
Step S3, dispersant is dissolved in polyalcohol, obtains the 3rd solution.
Specifically, dispersant is that the polyethylene glycol that the degree of polymerization is 1000～6000, and the quality of dispersant are water solubility
The 1%～7% of the quality of lithium salts；Polyalcohol can be any one in ethylene glycol, propane diols, glycerine, diethylene glycol (DEG).
Preferably, the volume of polyalcohol is 1/2～1 times of the volume of the first solution.
Step S4, the first solution and the second solution are added in the 3rd solution, obtain the 4th solution.
In order that the Li in the first solution+With the CO in the second solution3 2-Can contact and fully reaction in time, preferably
Simultaneously by the two to add at a slow speed into the 3rd solution, and in view of the fully factor such as reaction and reduces cost, control the 4th is molten
CO in liquid3 2-Substance withdrawl syndrome and Li+Substance withdrawl syndrome ratio be not less than 1:2.
Step S5, the 4th solution mix and react 1h～3h at 30 DEG C～70 DEG C, obtain suspension.
Preferably, in order that LITHIUM BATTERY micron crystallization of lithium carbonate is more intact, by obtain suspension ageing 1.5h～
2.5h。
Step S6, suspension is carried out separation of solid and liquid, obtain filtrate and filter cake, filter cake is scrubbed, be dried and obtain LITHIUM BATTERY
Micron lithium carbonate.
Preferably, first it is washed with deionized filter cake 2 times, then with absolute ethanol washing filter cake 1 time～2 times；Finally by Jing
Cross the filter cake for washing dry at least 12h in vacuum drying chamber at 50 DEG C, you can obtain LITHIUM BATTERY micron lithium carbonate.
The above-mentioned preparation method of the present invention will be embodied by specific embodiment below；In in order to contrast each embodiment not
Same condition, lists in table form the conditional parameter of embodiment 1-5；In embodiment 1-5, the first solution, the second solution are used
Amount is 50mL.
The conditional parameter contrast of embodiment 1-5 of table 1
Chemical analysis is carried out to the LITHIUM BATTERY micron lithium carbonate that embodiment 1 is obtained, it is known that Li in the product2CO3Quality hundred
Fraction is more than 99.5%, and the mass percent of wherein impurity component is listed in Table 2 below.
Impurity component mass percent in the LITHIUM BATTERY micron lithium carbonate that 2 embodiment of table 1 is obtained
| Na | Mg | Ca | K | Fe | Zn | Cu |
| <0.021% | <0.004% | <0.005% | <0.001% | <0.001% | <0.0001% | <0.0001% |
| Pb | Si | Al | Mn | Ni | SO4 2- | Cl- |
| <0.0003% | <0.0003% | <0.0001% | <0.0001% | <0.001% | <0.08% | <0.003% |
X-ray diffraction test (abbreviation XRD) and scanning are carried out respectively to the LITHIUM BATTERY micron lithium carbonate that embodiment 2 is obtained
Electronic Speculum tests (abbreviation SEM), respectively as depicted in figs. 1 and 2.In FIG, the diffraction maximum of product is very sharp, with standard diagram
The goodness of fit is higher, illustrates that the purity of the LITHIUM BATTERY micron lithium carbonate product of acquisition is higher, and the generation without impurities phase；In Fig. 2
In, it can be seen that LITHIUM BATTERY micron crystallization of lithium carbonate degree is higher, and particle diameter is about 8 μm or so, and reaction yield is 23.3%；Consider
Reaction yield is low when reaction time is 1h, and the reaction time when being 3h reaction yield be not improved largely, therefore preferably
2h is used as the reaction time.
Chemical analysis is carried out to the LITHIUM BATTERY micron lithium carbonate that embodiment 2 is obtained, it is known that Li in the product2CO3Quality hundred
Fraction is more than 99.5%, and the mass percent of wherein impurity component is listed in Table 3 below.
Impurity component mass percent in the LITHIUM BATTERY micron lithium carbonate that 3 embodiment of table 2 is obtained
| Na | Mg | Ca | K | Fe | Zn | Cu |
| <0.021% | <0.008% | <0.005% | <0.001% | <0.001% | <0.0002% | <0.0003% |
| Pb | Si | Al | Mn | Ni | SO4 2- | Cl- |
| <0.0003% | <0.003% | <0.001% | <0.0003% | <0.001% | <0.08% | <0.003% |
SEM tests are carried out to the LITHIUM BATTERY micron lithium carbonate that embodiment 3 is obtained, as shown in Figure 3.In figure 3, can see
Go out that LITHIUM BATTERY micron crystallization of lithium carbonate degree is higher, particle diameter is about 4 μm or so, and reaction yield is 25.1%.Due to improve reaction
Temperature and CO3 2-Concentration, reaction yield increases, in actual production can according to production cost select suitable production temperature and
Reactant concentration.Chemical analysis is carried out to the LITHIUM BATTERY micron lithium carbonate that embodiment 3 is obtained, it is known that Li in the product2CO3Matter
Amount percentage is more than 99.5%, and the mass percent of wherein impurity component is listed in Table 4 below.
Impurity component mass percent in the LITHIUM BATTERY micron lithium carbonate that 4 embodiment of table 3 is obtained
| Na | Mg | Ca | K | Fe | Zn | Cu |
| <0.021% | <0.008% | <0.005% | <0.001% | <0.001% | <0.0002% | <0.0003% |
| Pb | Si | Al | Mn | Ni | SO4 2- | Cl- |
| <0.0003% | <0.003% | <0.001% | <0.0003% | <0.001% | <0.08% | <0.003% |
In embodiment 4-5, due to the larger reaction of reactant concentration it is very fast, although play the role of dispersant, but obtain
Certain reunion is still suffered from LITHIUM BATTERY micron lithium carbonate product, therefore suitable reactant concentration is selected in actual production.
Chemical analysis is carried out respectively to the LITHIUM BATTERY micron lithium carbonate that embodiment 4-5 is obtained, it is known that Li in each product2CO3Quality
Percentage is all higher than 99.5%, and the wherein mass percent of impurity component is listed in respectively in table 5-6.
Impurity component mass percent in the LITHIUM BATTERY micron lithium carbonate that 5 embodiment of table 4 is obtained
| Na | Mg | Ca | K | Fe | Zn | Cu |
| <0.021% | <0.008% | <0.005% | <0.001% | <0.001% | <0.0002% | <0.0003% |
| Pb | Si | Al | Mn | Ni | SO4 2- | Cl- |
| <0.0003% | <0.003% | <0.001% | <0.0003% | <0.001% | <0.08% | <0.003% |
Impurity component mass percent in the LITHIUM BATTERY micron lithium carbonate that 6 embodiment of table 5 is obtained
| Na | Mg | Ca | K | Fe | Zn | Cu |
| <0.021% | <0.008% | <0.005% | <0.001% | <0.001% | <0.0002% | <0.0003% |
| Pb | Si | Al | Mn | Ni | SO4 2- | Cl- |
| <0.0003% | <0.003% | <0.001% | <0.0003% | <0.001% | <0.08% | <0.003% |
By embodiment 1-5, it can be seen that when using cetomacrogol 1000 or polyethylene glycol 2000 or polyethylene glycol
3000 or Macrogol 6000 as dispersant when, the species of dispersant to the pattern of LITHIUM BATTERY micron lithium carbonate product and
Grain size affects little, but affects very big to the dispersiveness of LITHIUM BATTERY micron lithium carbonate product.
In order to further verify the preparation method beneficial effect of the LITHIUM BATTERY micron lithium carbonate of the present invention, carry out following
Contrast experiment, comparative example 1 is intended to by being contrasted with above-described embodiment 2-5, to illustrate the necessity that dispersant is used.
Comparative example 1
In the description of comparative example 1, will not be described here with the something in common of embodiment 2-5, only description and embodiment 2-5
Difference.Comparative example 1 is with the difference of embodiment 2-5, in step s3, be not used cetomacrogol 1000 or
Polyethylene glycol 2000 or Macrogol 3000 or Macrogol 6000, that is to say, that the 3rd solution is only including the second two of 25mL
Alcohol.The particle diameter of the final LITHIUM BATTERY micron lithium carbonate for obtaining is about 14 μm, but occurs in that more serious agglomeration.
Although illustrating and describing the present invention with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case of without departing from the spirit and scope of the present invention limited by claim and its equivalent, can here carry out form and
Various change in details.
Claims (10)
1. a kind of preparation method of LITHIUM BATTERY micron lithium carbonate, it is characterised in that including step：
A, water-soluble lithium salts is configured to the aqueous solution, obtains the first solution, wherein, Li in first solution+Concentration is
0.5mol/L～6mol/L；
B, water soluble carbonate is configured to the aqueous solution, obtains the second solution, wherein, CO in second solution3 2-Concentration is
0.5mol/L～3mol/L；
C, dispersant is dissolved in polyalcohol, obtains the 3rd solution；
D, first solution and second solution are added in the 3rd solution, obtain the 4th solution；
E, the 4th solution mix and react 1h～3h at 30 DEG C～70 DEG C, obtain suspension；
F, the suspension is carried out separation of solid and liquid, obtain filtrate and filter cake, the filter cake is scrubbed, be dried that to obtain LITHIUM BATTERY micro-
Rice lithium carbonate.
2. preparation method according to claim 1, it is characterised in that the dispersant is 1000～6000 for the degree of polymerization
Polyethylene glycol, and the quality of the dispersant is the 1%～7% of the quality of the water-soluble lithium salts.
3. preparation method according to claim 1, it is characterised in that the polyalcohol be ethylene glycol, propane diols, the third three
Any one in alcohol, diethylene glycol (DEG).
4. according to the arbitrary described preparation method of claim 1-3, it is characterised in that in the 4th solution, CO3 2-Thing
The amount concentration of matter and Li+Substance withdrawl syndrome ratio be not less than 1:2.
5. according to the arbitrary described preparation method of claim 1-3, it is characterised in that the water-soluble lithium salts selected from lithium chloride,
At least one in lithium nitrate, lithium sulfate.
6. preparation method according to claim 5, it is characterised in that the water soluble carbonate is selected from sodium carbonate, carbonic acid
At least one in ammonium.
7. preparation method according to claim 1, it is characterised in that in step F, be first washed with deionized institute
State filter cake 2 times, then with filter cake described in absolute ethanol washing 1 time～2 times.
8. preparation method according to claim 1, it is characterised in that in step F, will exist through the filter cake of washing
At least 12h is dried at 50 DEG C, the LITHIUM BATTERY micron lithium carbonate is obtained.
9. preparation method according to claim 1, it is characterised in that the volume of the polyalcohol is first solution
1/2～1 times of volume.
10. preparation method according to claim 1, it is characterised in that in step E, by suspension ageing
1.5h～2.5h.
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| CN201710149064.1A CN106654265A (en) | 2017-03-14 | 2017-03-14 | Method for preparing battery level micrometer lithium carbonate |
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| CN201710149064.1A CN106654265A (en) | 2017-03-14 | 2017-03-14 | Method for preparing battery level micrometer lithium carbonate |
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| CN110642273A (en) * | 2018-06-27 | 2020-01-03 | 比亚迪股份有限公司 | Lithium carbonate particles and method for preparing lithium carbonate particles from lithium-containing brine |
| CN113772697A (en) * | 2021-08-24 | 2021-12-10 | 深圳新宸华科技有限公司 | Nano lithium carbonate and preparation method thereof |
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| CN113772697A (en) * | 2021-08-24 | 2021-12-10 | 深圳新宸华科技有限公司 | Nano lithium carbonate and preparation method thereof |
| CN113772697B (en) * | 2021-08-24 | 2024-01-09 | 深圳新宸华科技有限公司 | Nanometer lithium carbonate and preparation method thereof |
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