CN115321554A - Lithium tetrafluoroborate and preparation method thereof - Google Patents
Lithium tetrafluoroborate and preparation method thereof Download PDFInfo
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- CN115321554A CN115321554A CN202211133561.XA CN202211133561A CN115321554A CN 115321554 A CN115321554 A CN 115321554A CN 202211133561 A CN202211133561 A CN 202211133561A CN 115321554 A CN115321554 A CN 115321554A
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- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
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Abstract
The invention discloses lithium tetrafluoroborate and a preparation method thereof, relating to the technical field of electrolyte lithium salts for lithium ion batteries, wherein the preparation method of the lithium tetrafluoroborate comprises the following steps: dissolving lithium carbonate in water, and introducing carbon dioxide; step two, heating and crystallizing the solution; step three, preparing a fluoboric acid solution; step four, adding the product obtained in the step two into a fluoboric acid solution; step five, concentrating the solution obtained in the step five under reduced pressure, cooling, crystallizing, filtering and drying to obtain a crude product; and step six, dissolving the crude product in a pure propylene carbonate solution, and performing reduced pressure concentration, crystallization, separation and drying to obtain the propylene carbonate. Through the way, the method for preparing the lithium tetrafluoroborate removes soluble impurity ions and insoluble substances in industrial lithium carbonate by a method of hydrogenating and recrystallizing lithium carbonate, and dissolves lithium tetrafluoroborate generated by reaction with a fluoroboric acid solution in an organic solvent to remove crystal water, so that the high-quality lithium tetrafluoroborate with high purity and low water content can be finally obtained.
Description
Technical Field
The invention relates to the technical field of electrolyte lithium salts for lithium ion batteries, in particular to lithium tetrafluoroborate and a preparation method thereof.
Background
Lithium ion batteries have the advantages of high working voltage, high energy density, low self-discharge rate, long cycle life, no memory effect and no pollution, and in recent years, the lithium ion batteries rapidly occupy a plurality of fields with incomparable advantages, and are widely applied to products such as well-known mobile phones, notebook computers, small cameras, electric automobiles and the like. With the continuous expansion of the market, the demand of lithium ion batteries is also continuously expanding.
Lithium hexafluorophosphate is the electrolyte mainly used at present, and has the advantages of being capable of forming a stable solid electrolyte membrane, small in internal resistance, high in charging and discharging speed and the like because lithium hexafluorophosphate has good conductivity, but lithium hexafluorophosphate is too sensitive to moisture, is easily decomposed into phosphorus pentafluoride when heated, and an SEI (solid electrolyte interphase) membrane produced at a low temperature has too high impedance.
In comparison, lithium tetrafluoroborate has better chemical stability and thermal stability, is insensitive to environmental moisture, and is expected to be developed into an excellent electrolyte system widely adopted in the field of energy storage and power lithium ion batteries. At present, lithium tetrafluoroborate is mainly used as an additive of a lithium hexafluorophosphate-based electrolyte system and is used for improving the cycle life and the performance of a lithium ion battery; as a film forming additive, lithium tetrafluoroborate is widely used in the current electrolyte, and after the lithium tetrafluoroborate is added, the working temperature range of the lithium ion battery can be widened, and the high-low temperature discharge performance of the battery can be improved.
At present, the main preparation methods of lithium tetrafluoroborate include an aqueous solution method, a gas-solid reaction method and a non-aqueous solution method, wherein the aqueous solution method is prepared by using hydrofluoric acid, boric acid and lithium carbonate as raw materials, and the generated lithium tetrafluoroborate monohydrate is easy to dissolve in self crystallization water and change into a molten state when being dried, so that the product is difficult to dehydrate, and the content of insoluble substances is high, so that the development of a synthesis method of the lithium tetrafluoroborate with high purity and low water content is urgently needed.
Therefore, in combination with the above problems, it is an urgent need of those skilled in the art to provide a method for preparing lithium tetrafluoroborate.
Disclosure of Invention
The invention aims to provide lithium tetrafluoroborate and a preparation method thereof, which aim to solve the problems that in the background technology, the lithium tetrafluoroborate crystal water is difficult to remove and insoluble substances are high.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of lithium tetrafluoroborate comprises the following steps:
dissolving industrial lithium carbonate in water to prepare a lithium carbonate suspension, introducing carbon dioxide into the lithium carbonate suspension for hydrogenation, obtaining a lithium bicarbonate solution after the reaction is finished, and filtering to obtain the lithium bicarbonate solution;
step two, heating and crystallizing the obtained lithium bicarbonate solution to obtain high-purity lithium carbonate ointment;
step three, adding boric acid into the hydrofluoric acid solution according to the molar ratio of the boric acid to the hydrofluoric acid of 1 to 4 to 5 to prepare the fluoroboric acid solution;
step four, adding the lithium bicarbonate ointment prepared in the step two into a fluoboric acid solution, and obtaining a lithium tetrafluoroborate solution after the reaction is finished;
step five, carrying out reduced pressure concentration on the obtained lithium tetrafluoroborate solution, and then carrying out cooling crystallization, filtration and drying treatment to obtain a crude product of lithium tetrafluoroborate containing a crystal water;
and step six, dissolving the lithium tetrafluorophosphate crude product into a pure propylene carbonate solution, concentrating the solution under reduced pressure, and then crystallizing, separating and drying to obtain the high-purity lithium tetrafluoroborate crystal which can be used for the lithium ion battery.
Furthermore, in the first step, the molar ratio of the lithium carbonate to the water is 1 to 20 to 30.
Further, in the first step, the reaction is carried out under the stirring condition, the reaction temperature is 20-35 ℃, and the reaction time is 2-4 hours.
Further, in the second step, the temperature for heating the lithium bicarbonate is 70 to 100 ℃, and the crystallization time is 1 to 2 hours.
Furthermore, in the third step, the reaction temperature is-10 to 10 ℃, the reaction time is 1 to 5 hours, and the concentration of the hydrofluoric acid solution is 10 to 60 percent.
Furthermore, in the fourth step, the reaction temperature is 50 to 100 ℃, and the reaction time is 1 to 5 hours.
Further, in the fifth step, when the concentration is carried out under reduced pressure, the heating temperature is 70 to 90 ℃, the pressure is-0.05 to-0.09 MPa, the concentration is carried out under reduced pressure to 1/3 to 1/4 of the original volume, then the temperature is reduced to 20 ℃, and lithium tetrafluoroborate crystals are separated out.
Furthermore, in the fifth step, the crude lithium tetrafluoroborate is dried at the temperature of 80 to 90 ℃ for 2 to 8 hours.
And further, in the sixth step, concentrating under reduced pressure at-0.05 to-0.10 MPa to 1/3 to 1/4 of the original volume, then cooling to 20 ℃, performing crystallization separation, and performing vacuum drying at 100 to 120 ℃ for 2 to 8 hours to prepare the high-purity lithium tetrafluoroborate.
The invention also provides lithium tetrafluoroborate prepared by the method according to any one of claims 1 to 9.
Advantageous effects
According to the preparation method of the lithium tetrafluoroborate, the soluble impurity ions and insoluble substances in industrial lithium carbonate are removed by a method of hydrogenating and recrystallizing lithium carbonate, the lithium tetrafluoroborate generated by the reaction of the lithium tetrafluoroborate and a fluoroboric acid solution is dissolved in an organic solvent to remove crystal water, and finally the high-purity and low-water-content high-quality lithium tetrafluoroborate can be obtained.
The invention has the advantages of simple and easily obtained raw materials, no three wastes, environmental affinity and easy industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is an ion chromatogram of lithium tetrafluoroborate prepared in example 1.
Fig. 2 is an ion chromatogram of lithium tetrafluoroborate prepared in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further described with reference to the following examples.
Example 1
The preparation method of lithium tetrafluoroborate of the embodiment comprises the following steps:
(1) Putting 74g of 99% industrial lithium carbonate into ultrapure water, wherein the molar ratio of the lithium carbonate to the water is 1; reacting under the stirring condition, wherein the stirring speed is 100 revolutions per minute, introducing carbon dioxide into the lithium carbonate suspension, carrying out hydrogenation reaction for 3 hours at the reaction temperature of 20 ℃, obtaining a lithium bicarbonate solution after the reaction is finished, and filtering to obtain the lithium bicarbonate solution;
(2) Heating the obtained lithium bicarbonate solution at 90 ℃ for 2 hours to precipitate lithium carbonate, and filtering to obtain 152g of high-purity lithium carbonate ointment;
(3) Under the condition of 10 ℃, adding 132g of boric acid into a hydrofluoric acid solution with the concentration of 50% slowly according to the molar ratio of 1;
(4) Adding the lithium bicarbonate ointment prepared in the step two into a fluoboric acid solution, reacting for 4 hours at the temperature of 50 ℃, and obtaining a lithium tetrafluoroborate solution after the reaction is finished;
(5) Concentrating the obtained lithium tetrafluoroborate solution at 70 ℃ and-0.06 Mpa to 1/3 of the original volume under reduced pressure, then cooling to 20 ℃, crystallizing, filtering, drying at 80 ℃ for 8 hours, and accelerating the drying rate by adopting a nitrogen purging product to obtain 175g of a crude lithium tetrafluoroborate product containing a crystal water;
(6) Dissolving the lithium tetrafluorophosphate crude product in a pure propylene carbonate solution, filtering, concentrating under reduced pressure at 60 ℃ and-0.06 Mpa to 1/3 of the original volume, then cooling to 20 ℃, crystallizing, filtering, and drying in vacuum at 100 ℃ for 5 hours to obtain 168g of lithium tetrafluoroborate crystals with the purity of 99.38%, wherein the yield is 89.4%.
FIG. 1 is an ion chromatogram of lithium tetrafluoroborate prepared in example 1.
Example 2
(1) Putting 148g of 99% industrial lithium carbonate into ultrapure water, wherein the molar ratio of the lithium carbonate to the water is 1; reacting under the stirring condition, wherein the stirring speed is 120 r/min, introducing carbon dioxide into the lithium carbonate suspension for hydrogenation reaction for 4 hours, the reaction temperature is 30 ℃, obtaining a lithium bicarbonate solution after the reaction is finished, and filtering to obtain the lithium bicarbonate solution;
(2) Heating the obtained lithium bicarbonate solution at 80 ℃ for 2 hours to precipitate lithium carbonate, and filtering to obtain 300g of high-purity lithium carbonate ointment;
(3) Under the condition of 0 ℃, slowly adding 264g of boric acid into a hydrofluoric acid solution with the concentration of 55% according to the molar ratio of 1;
(4) Adding the lithium bicarbonate ointment prepared in the step two into a fluoboric acid solution, reacting for 5 hours at the temperature of 50 ℃, and obtaining a lithium tetrafluoroborate solution after the reaction is finished;
(5) Concentrating the obtained lithium tetrafluoroborate solution under the conditions of 80 ℃ and-0.08 Mpa to 1/4 of the original volume under reduced pressure, then cooling to 20 ℃, crystallizing, filtering, drying at 90 ℃ for 2 hours, and accelerating the drying rate by adopting a nitrogen purging product to obtain 347g of crude lithium tetrafluoroborate containing a crystal water;
(6) Dissolving a lithium tetrafluorophosphate crude product in a pure propylene carbonate solution, filtering, concentrating under reduced pressure at 80 ℃ and-0.08 Mpa to 1/4 of the original volume, then cooling to 20 ℃, crystallizing, filtering, and drying in vacuum at 120 ℃ for 6 hours to obtain 320g of lithium tetrafluoroborate crystals with the purity of 99.33%, wherein the yield is 85.10%.
Fig. 2 is an ion chromatogram of lithium tetrafluoroborate prepared in example 2.
Example 3
The present embodiment is different from embodiment 1 in that: in the step (1), the molar ratio of lithium carbonate to water is 1.
Example 4
The present embodiment is different from embodiment 1 in that: in the step (1), carbon dioxide is introduced into the lithium carbonate suspension for hydrogenation reaction for 2 hours, and the reaction temperature is 35 ℃.
Example 5
The present embodiment is different from embodiment 1 in that: in the step (2), the obtained lithium bicarbonate solution is heated at 70 ℃ for 1 hour.
Example 6
The present embodiment is different from embodiment 1 in that: in the step (2), the obtained lithium bicarbonate solution is heated at 100 ℃ for 1 hour.
Example 7
The present embodiment is different from embodiment 1 in that: in the step (3), under the condition of-10 ℃, boric acid and hydrofluoric acid are slowly added into 10% hydrofluoric acid solution according to the molar ratio of 1.
Example 8
The present embodiment is different from embodiment 1 in that: in the step (3), boric acid and hydrofluoric acid are slowly added into a hydrofluoric acid solution with the concentration of 60% according to the molar ratio of 1.
Example 9
The present embodiment is different from embodiment 1 in that: and (4) adding the lithium bicarbonate ointment prepared in the step two into a fluoboric acid solution, reacting for 1 hour at the temperature of 100 ℃, and obtaining a lithium tetrafluoroborate solution after the reaction is finished.
Example 10
The present embodiment is different from embodiment 1 in that: in the step (5), the lithium tetrafluoroborate solution is concentrated under reduced pressure at 90 ℃ and-0.05 Mpa.
Example 11
The present embodiment is different from embodiment 1 in that: in the step (5), the lithium tetrafluoroborate solution is concentrated under reduced pressure at 85 ℃ and-0.09 Mpa.
Example 12
The present embodiment is different from embodiment 1 in that: in the step (6), the parameters of the reduced pressure concentration are replaced by: concentrating under reduced pressure of-0.05 Mpa at 61 deg.C to 1/4 of the original volume. The drying parameters were replaced by: dried under vacuum at 115 ℃ for 8 hours.
Example 13
The present embodiment is different from embodiment 1 in that: in the step (6), the parameters of the reduced pressure concentration are replaced by: concentrating under-0.10 Mpa at 59 deg.C to 1/3 of the original volume. The drying parameters were replaced by: dried under vacuum at 110 ℃ for 2 hours.
Example 14
This example discloses lithium tetrafluoroborate prepared by the above examples (examples 1 to 13).
The preparation method of the lithium tetrafluoroborate adopts a method of hydrogenation and recrystallization of lithium carbonate to remove soluble impurity ions and insoluble substances in industrial lithium carbonate, reacts with a fluoroboric acid solution to generate lithium tetrafluoroborate, and dissolves the lithium tetrafluoroborate in an organic solvent to remove crystal water, thereby finally obtaining the high-quality lithium tetrafluoroborate with high purity and low water content.
The invention has the advantages of simple and easily obtained raw materials, no three wastes, environmental affinity and easy industrial production.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A preparation method of lithium tetrafluoroborate is characterized by comprising the following steps: the preparation method comprises the following steps:
dissolving industrial lithium carbonate in water to prepare a lithium carbonate suspension, introducing carbon dioxide into the lithium carbonate suspension for hydrogenation, obtaining a lithium bicarbonate solution after the reaction is finished, and filtering to obtain the lithium bicarbonate solution;
step two, heating and crystallizing the obtained lithium bicarbonate solution to obtain high-purity lithium carbonate ointment;
step three, adding boric acid into the hydrofluoric acid solution according to the molar ratio of the boric acid to the hydrofluoric acid of 1 to 4 to 5 to prepare the fluoroboric acid solution;
step four, adding the lithium bicarbonate ointment prepared in the step two into a fluoboric acid solution, and obtaining a lithium tetrafluoroborate solution after the reaction is finished;
step five, carrying out reduced pressure concentration on the obtained lithium tetrafluoroborate solution, and then carrying out cooling crystallization, filtration and drying treatment to obtain a crude product of lithium tetrafluoroborate containing a crystal water;
and step six, dissolving the lithium tetrafluorophosphate crude product in a pure propylene carbonate solution, carrying out reduced pressure concentration on the solution, and then carrying out crystallization, separation and drying treatment to obtain the high-purity lithium tetrafluoroborate crystal which can be used for the lithium ion battery.
2. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the first step, the molar ratio of the lithium carbonate to the water is 1 to 20-30.
3. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the first step, the reaction is carried out under the condition of stirring, the reaction temperature is 20-35 ℃, and the reaction time is 2-4 hours.
4. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: and in the second step, the temperature for heating the lithium bicarbonate is 70 to 100 ℃, and the crystallization time is 1 to 2 hours.
5. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the third step, the reaction temperature is-10 to 10 ℃, the reaction time is 1 to 5 hours, and the concentration of the hydrofluoric acid solution is 10 to 60 percent.
6. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the fourth step, the reaction temperature is 50 to 100 ℃, and the reaction time is 1 to 5 hours.
7. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: and fifthly, when concentrating under reduced pressure, heating to 70-90 ℃ and concentrating under-0.05-0.09 MPa under reduced pressure to 1/3-1/4 of the original volume, then cooling to 20 ℃, and crystallizing and precipitating lithium tetrafluoroborate.
8. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: and step five, drying the crude lithium tetrafluoroborate at the temperature of 80 to 90 ℃ for 2 to 8 hours.
9. The method for preparing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: and sixthly, concentrating under reduced pressure under the pressure of-0.05 to-0.10 MPa to 1/3 to 1/4 of the original volume, then cooling to 20 ℃, carrying out crystallization separation, and carrying out vacuum drying at the temperature of 100 to 120 ℃ for 2 to 8 hours to prepare the high-purity lithium tetrafluoroborate.
10. Lithium tetrafluoroborate produced by the method according to any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116462205A (en) * | 2023-03-29 | 2023-07-21 | 宜春国轩电池有限公司 | Synthesis method of lithium tetrafluoroborate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116462205A (en) * | 2023-03-29 | 2023-07-21 | 宜春国轩电池有限公司 | Synthesis method of lithium tetrafluoroborate |
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