CN111704144A - Preparation method of lithium tetrafluoroborate, product obtained by preparation method and application of product - Google Patents
Preparation method of lithium tetrafluoroborate, product obtained by preparation method and application of product Download PDFInfo
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- CN111704144A CN111704144A CN202010854017.9A CN202010854017A CN111704144A CN 111704144 A CN111704144 A CN 111704144A CN 202010854017 A CN202010854017 A CN 202010854017A CN 111704144 A CN111704144 A CN 111704144A
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- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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Abstract
The invention discloses a preparation method of lithium tetrafluoroborate, and an obtained product and application thereof, and belongs to the technical field of lithium ion battery electrolytes. The method comprises the following steps: 1) mixing lithium fluoride, a boron trifluoride complex compound and an organic solvent to obtain a mixed material; 2) carrying out microwave treatment on the mixed material obtained in the step 1) to obtain a microwave reaction product; 3) purifying the microwave reaction product obtained in the step 2) to obtain lithium tetrafluoroborate. The preparation method of the lithium tetrafluoroborate provided by the invention has the advantages that the prepared lithium tetrafluoroborate has high purity and high yield, the process flow is short, the operation is simple, and the investment on equipment is less.
Description
Technical Field
The invention relates to the technical field of lithium ion battery electrolyte, in particular to a preparation method of lithium tetrafluoroborate, and an obtained product and application thereof.
Background
Lithium ion batteries have the characteristics of high energy density, long cycle life and no pollution, and are widely applied to various electrical appliances and electric equipment. The electrolyte is one of the main components of the lithium ion battery and is also one of the key materials influencing the performance of the lithium ion battery. At present, the electrolytes of the commonly used lithium ion batteries are mainly lithium hexafluorophosphate (LiPF 6), lithium bis (oxalato) borate (LiBOB) and lithium tetrafluoroborate (LiBF 4). Lithium hexafluorophosphate has poor thermal stability and is easy to deliquesce. Lithium bis (oxalato) borate has a wide electrochemical stability window and good thermal stability, but the low-temperature capacity retention rate and the high-rate discharge capacity of the battery are poor. Compared with lithium hexafluorophosphate and lithium bis (oxalato) borate, the lithium tetrafluoroborate has better low-temperature performance and is not easy to deliquesce.
Patent CN102826563A provides a method for preparing high-purity lithium tetrafluoroborate, which comprises the steps of reacting high-purity lithium fluoride with boron trifluoride complexes in a chain carbonate organic solvent, filtering, concentrating, extracting, crystallizing, washing and drying to obtain lithium tetrafluoroborate. But the time consumption is long, the energy consumption is large, the cost is high, and the product post-treatment is complex. Patent CN104291347B discloses a method for preparing lithium tetrafluoroborate, which uses hydrogen fluoride and boron trifluoride gas as reaction raw materials, and has the disadvantages of difficult operation, high risk, low yield, and unsuitability for large-scale production.
Disclosure of Invention
The invention provides a preparation method of lithium tetrafluoroborate, and an obtained product and application thereof.
In order to solve the technical problems, the invention provides a preparation method of lithium tetrafluoroborate, which comprises the following steps:
1) mixing lithium fluoride, a boron trifluoride complex compound and an organic solvent to obtain a mixed material;
2) carrying out microwave treatment on the mixed material obtained in the step 1) to obtain a microwave reaction product;
3) purifying the microwave reaction product obtained in the step 2) to obtain lithium tetrafluoroborate.
Preferably, the molar ratio of the lithium fluoride to the boron trifluoride complex is (0.9-1.1): (0.9-1.2).
Preferably, the boron trifluoride complex in step 1) includes one or more of boron trifluoride diethyl carbonate, boron trifluoride acetonitrile, boron trifluoride tetrahydrofuran, boron trifluoride dimethyl carbonate, boron trifluoride gamma-butyrolactone, boron trifluoride ethyl acetate, boron trifluoride diethyl ether, boron trifluoride methyl ether, boron trifluoride sulfolane, boron trifluoride butyl acetate, boron trifluoride ethylene glycol dimethyl ether and boron trifluoride phenol.
Preferably, the organic solvent in step 1) is one or more of dimethyl carbonate, dipropyl carbonate, ethyl propyl carbonate, vinylene carbonate, ethyl isopropyl carbonate, methyl butyl carbonate, dibutyl carbonate, ethyl butyl carbonate, propylene carbonate, methyl ethyl carbonate, diethyl carbonate, acetonitrile, propionitrile, butyronitrile, tetrahydrofuran and dimethyl tetrahydrofuran.
Preferably, the temperature during the microwave treatment in the step 2) is 35-70 ℃, the time is 2-30 min, and the power is 100-2000 w.
Preferably, the purification mode in step 3) comprises the following steps:
a. sequentially filtering and/or concentrating, recrystallizing and drying the microwave reaction product to obtain a crude product containing lithium tetrafluoroborate;
b. and d, dissolving the crude product containing the lithium tetrafluoroborate in the step a by using dimethyl carbonate, filtering, concentrating, recrystallizing and drying to obtain the lithium tetrafluoroborate.
Preferably, the drying in step a and/or b is carried out independently by blowing drying and then vacuum drying.
Preferably, the time of the forced air drying is 10-14 h, and the temperature is 80-120 ℃; the vacuum drying time is 12-24 hours, the temperature is 80-120 ℃, and the vacuum degree is-0.09 to-0.1 Mpa.
The invention provides lithium tetrafluoroborate prepared by the method in the scheme.
The invention also provides application of the lithium tetrafluoroborate in the scheme in preparation of lithium ion battery electrolyte.
Compared with the prior art, the invention has the following technical effects:
the preparation method of the lithium tetrafluoroborate provided by the invention adopts the steps of mixing lithium fluoride, boron trifluoride complex and organic solvent to obtain a mixed material, and obtaining the lithium tetrafluoroborate through microwave reaction. The microwave heating is intramolecular heating, and the heating speed is high and the heating is uniform, so the reaction speed is high and the efficiency is high. Meanwhile, as the microwave heating is internal heating generated by intermolecular friction, the reaction degree is higher, the product purity is high, and the yield is higher; and the reaction time is short, the energy consumption is low, and the cost is low. The results of the examples show that the yield of the lithium tetrafluoroborate prepared by the method provided by the invention can reach 98.4%, and the purity can reach 99.89%.
Drawings
FIG. 1 is an XRD pattern of lithium tetrafluoroborate as prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of lithium tetrafluoroborate as prepared in example 2 of the present invention;
FIG. 3 is an XRD pattern of lithium tetrafluoroborate as prepared in example 3 of the present invention.
Detailed Description
The invention provides a preparation method of lithium tetrafluoroborate, which comprises the following steps:
1) mixing lithium fluoride, a boron trifluoride complex compound and an organic solvent to obtain a mixed material;
2) carrying out microwave treatment on the mixed material obtained in the step 1) to obtain a microwave reaction product;
3) purifying the microwave reaction product obtained in the step 2) to obtain lithium tetrafluoroborate.
According to the invention, lithium fluoride, boron trifluoride complex and an organic solvent are mixed to obtain a mixed material. In the present invention, the molar ratio of the lithium fluoride to the boron trifluoride complex is preferably (0.9 to 1.1): (0.9 to 1.2), more preferably 1.0: 1.1.
in the present invention, the boron trifluoride complex preferably includes one or more of boron trifluoride diethyl carbonate, boron trifluoride acetonitrile, boron trifluoride tetrahydrofuran, boron trifluoride dimethyl carbonate, boron trifluoride γ -butyrolactone, boron trifluoride ethyl acetate, boron trifluoride diethyl ether, boron trifluoride methyl ether, boron trifluoride sulfolane, boron trifluoride butyl acetate, boron trifluoride ethylene glycol dimethyl ether, and boron trifluoride phenol, more preferably boron trifluoride diethyl ether or boron trifluoride dimethyl carbonate.
In the present invention, the organic solvent is preferably one or more selected from dimethyl carbonate, dipropyl carbonate, ethyl propyl carbonate, vinylene carbonate, ethyl isopropyl carbonate, methyl butyl carbonate, dibutyl carbonate, ethyl butyl carbonate, propylene carbonate, ethyl methyl carbonate, diethyl carbonate, acetonitrile, propionitrile, butyronitrile, tetrahydrofuran and dimethyltetrahydrofuran, and more preferably dimethyl carbonate or acetonitrile. In the present invention, the organic solvent is a reaction medium. The amount of the organic solvent to be added is not particularly limited in the present invention.
The sources of the lithium fluoride and the boron source and the organic solvent are not particularly limited, and the conventional commercial electronic grade products in the field can be adopted.
After the mixed material is obtained, the microwave treatment is carried out on the mixed material to obtain a microwave reaction product. In the invention, the temperature during microwave treatment is preferably 35-70 ℃, and more preferably 50 ℃; the time is preferably 2-30 min, and more preferably 15 min; the power is preferably 100 to 2000w, and more preferably 200 w.
In the invention, the lithium tetrafluoroborate is prepared by microwave treatment, microwave heating is intramolecular heating, and the heating speed is high and uniform, so the reaction speed is high and the efficiency is high. Meanwhile, as the microwave heating is internal heating generated by intermolecular friction, the reaction degree is higher, the product purity is high, and the yield is higher; and the reaction time is short, the energy consumption is low, and the cost is low.
The microwave equipment used in the microwave treatment is not particularly limited, and the conventional microwave equipment in the field can be adopted.
After the microwave reaction product is obtained, the invention purifies the microwave reaction product to obtain the lithium tetrafluoroborate. In the present invention, the purification method comprises the following steps: a. sequentially filtering and/or concentrating, recrystallizing and drying the microwave reaction product to obtain a crude product containing lithium tetrafluoroborate; b. and d, dissolving the crude product containing the lithium tetrafluoroborate in the step a by using dimethyl carbonate, filtering, concentrating, recrystallizing and drying to obtain the lithium tetrafluoroborate.
According to the invention, the microwave reaction product is preferably sequentially filtered and/or concentrated, recrystallized and dried to obtain a crude product containing lithium tetrafluoroborate. In the present invention, the pore size of the filter screen for filtration is preferably 0.5 to 5 μm. In the present invention, it is preferable that the concentration and recrystallization are carried out by dissolving dimethyl carbonate or diethyl ether. In the invention, the drying mode is to perform forced air drying firstly and then perform vacuum drying. The air-blast drying time is preferably 10-14 h, and more preferably 12 h; the temperature is preferably 80-120 ℃, and more preferably 100 ℃; the vacuum drying time is preferably 12-24 hours, and more preferably 16 hours; the temperature is preferably 80-120 ℃, and more preferably 100 ℃; the degree of vacuum is preferably-0.09 to-0.1 MPa, more preferably-0.095 MPa.
According to the invention, the crude product containing lithium tetrafluoroborate is preferably dissolved by dimethyl carbonate, and is filtered, concentrated, recrystallized and dried to obtain the lithium tetrafluoroborate. In the invention, the drying mode is the same as the drying mode after filtration or concentration recrystallization in the step a, and the drying mode is that air blowing drying is firstly carried out, and then vacuum drying is carried out.
The invention provides lithium tetrafluoroborate prepared by the method in the scheme.
The invention also provides application of the lithium tetrafluoroborate in the scheme in preparation of lithium ion battery electrolyte.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
150ml of acetonitrile was charged into a dry three-necked flask, and then 28.85g of boron trifluoride dimethyl carbonate and 5.18g of lithium fluoride were added thereto and uniformly dispersed with stirring. Placing the three-neck flask into a microwave reactor, starting mechanical stirring, and carrying out condensation reflux. Setting the microwave reaction temperature at 45 ℃, the reaction time at 10min and the power at 300W to obtain a microwave reaction product. And (3) concentrating, recrystallizing and filtering the microwave reaction product, drying by blowing at 80 ℃ for 12h, and then drying in vacuum at-0.1 Mpa and 120 ℃ for 12h to obtain a crude product containing lithium tetrafluoroborate.
Dissolving the crude product containing lithium tetrafluoroborate in dimethyl carbonate, stirring and dissolving for 2h, filtering to remove filter residue, concentrating and recrystallizing the filtrate, drying by blowing at 120 ℃ for 12h, and then drying under vacuum at-0.1 Mpa and 120 ℃ for 24h to obtain lithium tetrafluoroborate.
The obtained lithium tetrafluoroborate is analyzed by XRD, and the specific spectrum is shown in figure 1. From the peak shape and peak position of fig. 1, it can be seen that the product is lithium tetrafluoroborate.
The calculated yield was 96.70% with a purity of 99.89%.
Wherein: yield = actual yield/theoretical yield 100%;
the purity test method comprises the following steps: 10g of lithium tetrafluoroborate was dissolved in 150ml of dimethyl carbonate and then filtered, and the insoluble matter m was weighed to calculate the purity = (1-m/10) × 100%.
Example 2
150ml of dimethyl carbonate was charged into a dry three-necked flask, followed by 28.85g of boron trifluoride ethyl acetate and 5.18g of lithium fluoride, and the mixture was dissolved and dispersed uniformly with stirring. Placing the three-neck flask into a microwave reactor, starting mechanical stirring, and carrying out condensation reflux. Setting the microwave reaction temperature at 70 ℃, the reaction time at 2min and the power at 2000W to obtain a microwave reaction product. And (3) concentrating, recrystallizing and filtering the microwave reaction product, drying by blowing at 120 ℃ for 12h, and then drying under vacuum at-0.09 Mpa and 120 ℃ for 24h to obtain a crude product containing lithium tetrafluoroborate.
Dissolving the crude product containing lithium tetrafluoroborate in dimethyl carbonate, stirring and dissolving for 2h, filtering to remove filter residue, concentrating and recrystallizing the filtrate, drying by blowing at 120 ℃ for 10h, and then drying in vacuum at-0.095 Mpa and 80 ℃ for 16h to obtain the lithium tetrafluoroborate.
The obtained lithium tetrafluoroborate was analyzed by XRD, and the specific spectrum is shown in fig. 2. From the peak shape and peak position of fig. 2, it can be seen that the product is lithium tetrafluoroborate.
The calculated yield was 97.2% with a purity of 98.12%.
Example 3
150ml of diethyl carbonate was charged into a dry three-necked flask, followed by 28.38g of boron trifluoride diethyl ether and 5.18g of lithium fluoride, and the mixture was stirred and dispersed uniformly. Placing the three-neck flask into a microwave reactor, starting mechanical stirring, and carrying out condensation reflux. Setting the microwave reaction temperature at 30 ℃, the reaction time at 35min and the power at 200W to obtain a microwave reaction product. Filtering the microwave reaction product, drying by blowing at 120 ℃ for 12h, and then drying in vacuum at-0.1 Mpa and 100 ℃ for 12h to obtain a crude product containing lithium tetrafluoroborate.
Dissolving the crude product containing lithium tetrafluoroborate in dimethyl carbonate, stirring and dissolving for 2h, filtering to remove filter residue, concentrating and recrystallizing the filtrate, drying by blowing at 100 ℃ for 14h, and then drying under vacuum at-0.09 Mpa and 120 ℃ for 24h to obtain the lithium tetrafluoroborate.
The obtained lithium tetrafluoroborate was analyzed by XRD, and the specific spectrum is shown in fig. 3. From the peak shape and peak position of fig. 3, it can be seen that the product is lithium tetrafluoroborate.
The calculated yield was 98.4% with a purity of 99.68%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the lithium tetrafluoroborate is characterized by comprising the following steps:
1) mixing lithium fluoride, a boron trifluoride complex compound and an organic solvent to obtain a mixed material;
2) carrying out microwave treatment on the mixed material obtained in the step 1) to obtain a microwave reaction product;
3) purifying the microwave reaction product obtained in the step 2) to obtain lithium tetrafluoroborate.
2. The production method according to claim 1, wherein the molar ratio of the lithium fluoride to the boron trifluoride complex is (0.9 to 1.1): (0.9-1.2).
3. The preparation method according to claim 1, wherein the boron trifluoride complex in step 1) comprises one or more of boron trifluoride diethyl carbonate, boron trifluoride acetonitrile, boron trifluoride tetrahydrofuran, boron trifluoride dimethyl carbonate, boron trifluoride γ -butyrolactone, boron trifluoride ethyl acetate, boron trifluoride diethyl ether, boron trifluoride methyl ether, boron trifluoride sulfolane, boron trifluoride butyl acetate, boron trifluoride ethylene glycol dimethyl ether and boron trifluoride phenol.
4. The preparation method according to claim 1, wherein the organic solvent in step 1) is one or more selected from dimethyl carbonate, dipropyl carbonate, ethyl propyl carbonate, vinylene carbonate, ethyl isopropyl carbonate, methyl butyl carbonate, dibutyl carbonate, ethyl butyl carbonate, propylene carbonate, methyl ethyl carbonate, diethyl carbonate, acetonitrile, propionitrile, butyronitrile, tetrahydrofuran and dimethyltetrahydrofuran.
5. The preparation method according to claim 1, wherein the microwave treatment in step 2) is carried out at a temperature of 35 to 70 ℃ for 2 to 30min at a power of 100 to 2000 w.
6. The method according to claim 1, wherein the purification in step 3) comprises the following steps:
a. sequentially filtering and/or concentrating, recrystallizing and drying the microwave reaction product to obtain a crude product containing lithium tetrafluoroborate;
b. and d, dissolving the crude product containing the lithium tetrafluoroborate in the step a by using dimethyl carbonate, filtering, concentrating, recrystallizing and drying to obtain the lithium tetrafluoroborate.
7. The method according to claim 6, wherein the drying in step a and/or step b is carried out by air-blast drying and vacuum drying.
8. The preparation method according to claim 7, wherein the time of the forced air drying is 10-14 h, and the temperature is 80-120 ℃; the vacuum drying time is 12-24 hours, the temperature is 80-120 ℃, and the vacuum degree is-0.09 to-0.1 Mpa.
9. Lithium tetrafluoroborate produced by the process of any of claims 1 to 8.
10. Use of the lithium tetrafluoroborate of claim 9 in the preparation of an electrolyte for a lithium ion battery.
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| CN114477201A (en) * | 2021-12-30 | 2022-05-13 | 石家庄康坦福化工科技有限公司 | Preparation and application of lithium tetrafluoroborate |
| CN116495745A (en) * | 2023-04-28 | 2023-07-28 | 河南省氟基新材料科技有限公司 | Method for preparing tetrafluoroborate |
| CN116947061A (en) * | 2023-08-09 | 2023-10-27 | 兰州理工大学 | Method for preparing lithium tetrafluoroborate from lithium-containing electrolytic aluminum waste residues |
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| CN114477201A (en) * | 2021-12-30 | 2022-05-13 | 石家庄康坦福化工科技有限公司 | Preparation and application of lithium tetrafluoroborate |
| CN116495745A (en) * | 2023-04-28 | 2023-07-28 | 河南省氟基新材料科技有限公司 | Method for preparing tetrafluoroborate |
| CN116947061A (en) * | 2023-08-09 | 2023-10-27 | 兰州理工大学 | Method for preparing lithium tetrafluoroborate from lithium-containing electrolytic aluminum waste residues |
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