CN114181240A - Preparation method of lithium bis (oxalato) borate - Google Patents
Preparation method of lithium bis (oxalato) borate Download PDFInfo
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Abstract
The invention provides a preparation method of lithium bis (oxalato) borate, belonging to the technical field of special chemicals. The method comprises the following steps: 1) mixing a lithium source, boric acid and an oxalic acid compound, and carrying out ball milling to obtain a mixed material; 2) and flatly paving the mixed material in a microwave hot-pressing device, and carrying out microwave hot-pressing reaction to obtain the lithium bis (oxalato) borate. The preparation method provided by the invention has the advantages of high reaction efficiency and high yield, and the prepared lithium bis (oxalato) borate has low water content and high purity.
Description
Technical Field
The invention belongs to the technical field of special chemicals, and particularly relates to a preparation method of lithium bis (oxalato) borate.
Background
The lithium borate complex is a novel lithium ion battery electrolyte, wherein the lithium bis (oxalato) borate LiBOB is the most effectiveIs representative. The lithium bis (oxalato) borate is a coordination chelate, and the formed electrolyte has larger anions and smaller lattice energy, and can obtain more ions in a solvent, so that the conductivity of the electrolyte is improved. Lithium bis (oxalato) borate (LiBOB) has good electrochemical stability and thermal stability, can react with a specific solvent to form a stable SEI film, can not be attenuated after multiple cycles, has higher thermal stability compared with lithium hexafluorophosphate, and a decomposed product B2O3And CO2The electrolyte has little influence on the service performance and the environment of the battery, and is an electrolyte substance with development potential in the lithium battery industry.
The lithium bis (oxalato) borate synthesis methods include an aqueous phase method, a solid phase method and a solvent method. The solvent method adopts an organic solvent as a reaction medium, increases the cost of raw materials and has pollution to the environment. The aqueous phase method needs long time for removing water, and has long reaction time and low efficiency. Patent CN107602603A discloses a solid phase method for synthesizing lithium bis (oxalato) borate, which requires reaction in nitrogen atmosphere, and has high energy consumption and long reaction time. Therefore, how to improve the efficiency of synthesis and reduce the synthesis time is a key challenge in the current work.
Disclosure of Invention
The invention provides a preparation method of lithium bis (oxalato) borate, which has the advantages of high reaction efficiency and high yield, and the prepared lithium bis (oxalato) borate has low water content and high purity.
In order to achieve the above object, the present invention provides a method for preparing lithium bis (oxalato) borate, comprising the steps of:
1) mixing a lithium source, boric acid and an oxalic acid compound, and carrying out ball milling to obtain a mixed material;
2) and flatly paving the mixed material in a microwave hot-pressing device, and carrying out microwave hot-pressing reaction to obtain the lithium bis (oxalato) borate.
Preferably, the molar ratio of the lithium source to the boron source to the oxalic acid compound is 0.8-1.1: 0.8-1.2: 2.0-2.3.
Preferably, the ball milling time is 25-35 min; the rotating speed is 90-110 r/min.
Preferably, the pressure of the microwave hot-pressing reaction is 0.1-20 Mpa.
Preferably, the microwave hot-pressing reaction time is 5-100 min.
Preferably, the microwave power of the microwave hot-pressing reaction is 100-500 w.
Preferably, the temperature of the microwave hot-pressing reaction is 100-240 ℃.
Preferably, the microwave hot-pressing device comprises a pressing sheet upper pressing plate, a pressing sheet lower pressing plate and a microwave transmitting plate; a material groove is arranged in the pressing plate lower pressing plate; the microwave transmitting plate is arranged at the lower part of the pressing plate upper pressing plate, is integrated with the pressing plate upper pressing plate and is matched with the pressing plate lower pressing plate groove.
Preferably, when the microwave hot-pressing reaction is carried out, the pressing rate of the upper pressing plate and the lower pressing plate of the microwave hot-pressing device is 0.1-100 mm/s.
Preferably, the preparation method further comprises the steps of dissolving the lithium bis (oxalato) borate in an organic solvent, filtering, concentrating and drying.
Compared with the prior art, the invention has the advantages and positive effects that:
according to the preparation method of lithium bis (oxalato) borate, provided by the invention, the lithium source, the boron source and the oxalate compound are mixed and subjected to ball milling, and a microwave hot-pressing device is adopted to perform microwave hot-pressing reaction on the mixed material, the microwave hot-pressing can be directly performed in the compacting process, the reaction can be completed by one-step operation, the time and the labor are saved, the preparation process steps are reduced, the operation process is simple, and the preparation method is suitable for industrial production. Meanwhile, in the hot pressing process, the raw material solid particles can be fully contacted, and further the reaction efficiency and the conversion rate are improved.
The microwave hot pressing method combines the compaction and the heating reaction together, can press out water generated by the reaction in time and reduce the water content of the product.
The microwave is adopted, so that the heating can be performed quickly and uniformly, the molecular vibration can be increased by the microwave, the intermolecular friction is increased, and the reaction efficiency is improved. Meanwhile, the microwave can play a magnetic effect to promote the selective reaction among reactant ions without generating side reaction; and the microwave also has the electric effect, so that the activation energy of the reaction is reduced, and the reaction is accelerated.
Meanwhile, the lithium bis (oxalato) borate prepared by the method has high purity and extremely low moisture, and can omit the steps of cooling, crystallizing, filtering and drying, thereby preventing moisture from being introduced in the recrystallization and filtration process.
Drawings
FIG. 1 is a schematic structural diagram of a microwave hot-pressing device used in the present invention;
FIG. 2 is an XRD spectrum of lithium bis (oxalato) borate of examples 1 to 8 and comparative examples 1 to 5;
wherein: 1-base 1, 2-pressing plate lower pressing plate, 3-pressing plate upper pressing plate, 4-material groove, 5-vacuum pipeline, 6-vacuum pump, 7-telescopic rod 7, 8-microwave transmitting plate, 9-microwave emitter, 10-pressure sensor, 11-pressure system, 12-digital display operation screen, 13-pressure system switch, 14-vacuum system switch, 15-microwave heating system switch, 16-emergency stop button, 17-sieve pore base, 18-water outlet and 19-conversion valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be 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 invention provides a preparation method of lithium bis (oxalato) borate, which comprises the following steps:
1) mixing a lithium source, a boron source and an oxalic acid compound, and carrying out ball milling to obtain a mixed material;
2) and flatly paving the mixed material in a microwave hot-pressing device, and carrying out microwave hot-pressing reaction to obtain the lithium bis (oxalato) borate.
According to the invention, a lithium source, boric acid and an oxalic acid compound are mixed and subjected to ball milling to obtain a mixed material. In the invention, the lithium source is preferably one or more of lithium oxalate, lithium carbonate, lithium hydroxide and lithium tetrafluoroborate; more preferably lithium oxalate or lithium hydroxide; most preferred is lithium hydroxide.
In the invention, the boron source is preferably one or more of anhydrous boric acid, boric acid dihydrate, boric acid monohydrate and lithium borate; more preferably anhydrous boric acid.
In the invention, the oxalic acid compound is preferably one or more of lithium oxalate, potassium oxalate, ammonium oxalate, oxamic acid, oxamide, anhydrous oxalic acid, hydrated oxalic acid, rubidium oxalate or cesium oxalate, more preferably anhydrous oxalic acid and hydrated oxalic acid, and most preferably anhydrous oxalic acid.
In the present invention, the molar ratio of the lithium source, the boric acid and the oxalic acid compound is preferably 0.8 to 1.1:0.8 to 1.2:2.0 to 2.3, and more preferably 1:1: 2.1.
The sources of the lithium source, the boron source and the oxalic acid compound are not particularly limited in the present invention, and conventional commercial products in the art can be used.
In the invention, the rotation speed of the ball milling is preferably 90-110 r/min, and more preferably 100 r/min; the ball milling time is preferably 25-35 min, and more preferably 30 min. The invention ball-mills the lithium source, the boron source and the oxalic acid, and can fully mix the materials.
After the mixed material is obtained, the mixed material is flatly paved in a microwave hot-pressing device to carry out microwave hot-pressing reaction, and the lithium bis (oxalato) borate is obtained.
In the invention, the pressure of the microwave hot-pressing reaction is preferably 0.1-20 Mpa, and more preferably 5-15 Mpa.
In the invention, the time of the microwave hot-pressing reaction is preferably 5-100 min, and more preferably 10-15 min.
In the invention, the microwave power of the microwave hot-pressing reaction is preferably 100-500 w, and more preferably 150-200 w.
In the invention, the temperature of the microwave hot-pressing reaction is preferably 100-240 ℃, and more preferably 120-200 ℃.
In the invention, the microwave hot-pressing device preferably comprises a pressing sheet upper pressing plate, a pressing sheet lower pressing plate and a microwave transmitting plate; a material groove is arranged in the pressing plate lower pressing plate; the microwave transmitting plate is arranged at the lower part of the pressing plate upper pressing plate, is integrated with the pressing plate upper pressing plate and is matched with the pressing plate lower pressing plate groove. As shown in particular in figure 1.
In the invention, when the microwave hot-pressing reaction is carried out, the pressing rate of the upper pressing plate and the lower pressing plate of the microwave hot-pressing device is preferably 0.1-100 mm/s, and more preferably 0.5-10 mm/s.
According to the invention, the microwave hot-pressing reaction is carried out on the mixed material by adopting the microwave hot-pressing device, so that solid particles of the raw materials can be fully contacted in the hot-pressing process, and the conversion rate and the reaction efficiency are further improved. The microwave is adopted, so that the heating can be performed rapidly and uniformly, the molecular vibration can be increased by the microwave, the intermolecular friction is increased, and the reaction efficiency is improved. Meanwhile, the microwave can play a magnetic effect to promote the selective reaction among reactant ions without generating side reaction; and the microwave also has the electric effect, so that the activation energy of the reaction is reduced, and the reaction is accelerated. In conclusion, the microwave hot pressing method is adopted, so that the reaction efficiency can be improved, the reaction time can be shortened, and the yield and the purity can be improved. Meanwhile, the method is adopted to simultaneously operate heating and pressurizing, so that the reaction can be completed in one step, and the operation is simpler.
After obtaining lithium bis (oxalato) borate, the present invention preferably further comprises purifying the lithium bis (oxalato) borate. The purification method is preferably dissolution with an organic solvent, filtration, concentration and drying.
In the present invention, the organic solvent is preferably any one or a mixture of several of 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, ethyl acetate, acetonitrile, propionitrile, butyronitrile, tetrahydrofuran and dimethyltetrahydrofuran, and more preferably ethyl acetate and/or acetonitrile.
In the invention, the drying mode is preferably rotary evaporation drying; the specific operation of the rotary evaporation drying is preferably that the concentrated solution is firstly subjected to rotary evaporation at 60 ℃ until no liquid exists, and then the temperature is increased to 180 ℃ for rotary evaporation.
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
Adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a microwave hot-pressing die, heating by microwave with the power of 100W, the hot-pressing pressure of 10MPa, the microwave hot-pressing temperature of 100 ℃, and the hot-pressing time of 10min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Example 2
Adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a hot-pressing mold, heating by using microwave with the power of 200W, and carrying out hot-pressing at the pressure of 10Mpa and the temperature of 100 ℃ for 10min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Example 3
Adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a hot-pressing die, heating by using microwave with the power of 100W, and obtaining a crude product B, wherein the hot-pressing pressure is 10MPa, the hot-pressing temperature is 100 ℃, and the hot-pressing time is 15 min.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Example 4
Adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a hot-pressing mold, heating by using microwave with the power of 100W, and carrying out hot-pressing at the pressure of 5Mpa and the temperature of 100 ℃ for 10min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Example 5
Adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a hot-pressing mold, heating by using microwave with the power of 100W, and carrying out hot-pressing at the pressure of 5Mpa and the temperature of 120 ℃ for 10min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And C, rotationally evaporating the concentrated solution C obtained in the step C at 60 ℃ until no liquid exists, and then rotationally evaporating at 150 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Example 6
Adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a hot-pressing mold, heating by using microwave with the power of 100W, and carrying out hot-pressing at the pressure of 5Mpa and the temperature of 100 ℃ for 5min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at 60 ℃ until no liquid exists, and then carrying out rotary evaporation at 180 ℃ for 3h to obtain the high-purity lithium bis (oxalato) borate.
Example 7
Adding 30.57g of lithium oxalate, 19.2g of lithium borate and 99.72g of potassium oxalate into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly, wherein the ball milling time is 35min, and the ball milling speed is 90r/min, so as to obtain a mixture A;
and flatly paving the mixture A in a microwave hot-pressing die, heating by using microwave with the power of 500W, the hot-pressing pressure of 0.1MPa, the microwave hot-pressing temperature of 240 ℃ and the hot-pressing time of 100min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Example 8
Adding 30.57g of lithium oxalate, 21.6g of boric acid monohydrate and 110.52g of potassium oxalate hydrate into a ball milling tank, and carrying out ball milling for 25min at a ball milling speed of 110r/min to obtain a mixture A;
and flatly paving the mixture A in a microwave hot-pressing die, heating by using microwave at the power of 300W, at the hot-pressing pressure of 20MPa, at the microwave hot-pressing temperature of 100 ℃ and for the hot-pressing time of 50min, and thus obtaining a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Comparative example 1
The procedure is as in example 5, except that: the microwave treatment is not carried out, and the specific operation is as follows:
adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a tablet press die, pressing into tablets under the pressure of 10Mpa, reacting the materials pressed into tablets at 120 ℃ for 6 hours, heating to 240 ℃, and reacting for 6 hours to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at 60 ℃ until no liquid exists, and then carrying out rotary evaporation at 180 ℃ for 3h to obtain the high-purity lithium bis (oxalato) borate.
Comparative example 2
The procedure is as in example 5, except that: the tabletting treatment is not carried out, and the specific operation is as follows:
adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
and flatly paving the mixture A in a tablet press die, setting the pressurizing pressure to be 0MPa, the microwave heating temperature to be 120 ℃, the reaction time to be 10min and the microwave heating power to be 100W, and obtaining a crude product A.
The crude product A was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrated solution B.
And carrying out rotary evaporation on the obtained concentrated solution B at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 3 hours to obtain the high-purity lithium bis (oxalato) borate.
Comparative example 3
The procedure is as in example 5, except that: the grinding treatment is not carried out, and the specific operation is as follows:
spreading 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid in a microwave hot-pressing mold, wherein the microwave heating power is 100W, the hot-pressing pressure is 10MPa, the microwave hot-pressing temperature is 120 ℃, and the hot-pressing time is 10min, so as to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Comparative example 4
The procedure is as in example 5, except that: the grinding and tabletting treatment is not carried out, and the specific operation is as follows:
spreading 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid in a microwave hot-pressing mold, and heating by microwave at the temperature of 120 ℃ for 10min at the power of 100W to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Comparative example 5
The procedure is as in example 5, except that: the tabletting and microwave reaction are separately operated, and the specific operation is as follows:
adding 7.18g of lithium hydroxide, 18.55g of anhydrous boric acid and 56.7g of anhydrous oxalic acid into a ball milling tank, and carrying out ball milling, dispersing and mixing uniformly for 30min at a ball milling speed of 100r/min to obtain a mixture A;
spreading the mixture A in a microwave hot-pressing mold, pressing into tablets under the pressure of 10Mpa, and performing microwave heating reaction on the materials to be pressed into tablets at the microwave heating power of 100W and the microwave heating temperature of 120 ℃ for 10min to obtain a crude product B.
The crude product B was dissolved in 200g of ethyl acetate, and then filtered and concentrated to obtain a concentrate C.
And carrying out rotary evaporation on the obtained concentrated solution C at the temperature of 60 ℃ until no liquid exists, and then carrying out rotary evaporation at the temperature of 180 ℃ for 6 hours to obtain the high-purity lithium bis (oxalato) borate.
Performance testing
The yield, moisture content and purity of lithium bis (oxalato) borate prepared in examples 1 to 8 and comparative examples 1 to 5 were measured, and the specific results are shown in table 1. The XRD patterns of lithium bis (oxalato) borate of examples 1 to 8 and comparative examples 1 to 5 were measured, and are specifically shown in fig. 1.
TABLE 1 test results for yield, moisture, purity of each lithium bis (oxalato) borate
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. A preparation method of lithium bis (oxalato) borate is characterized by comprising the following steps:
1) mixing a lithium source, a boron source and an oxalic acid compound, and carrying out ball milling to obtain a mixed material;
2) and flatly paving the mixed material in a microwave hot-pressing device, and carrying out microwave hot-pressing reaction to obtain the lithium bis (oxalato) borate.
2. The method according to claim 1, wherein the molar ratio of the lithium source, the boric acid, and the oxalic acid compound is 0.8 to 1.1:0.8 to 1.2:2.0 to 2.3.
3. The preparation method according to claim 1, wherein the ball milling time is 25-35 min; the rotating speed is 90-110 r/min.
4. The preparation method according to claim 1, wherein the pressure of the microwave hot-pressing reaction is 0.1 to 20 MPa.
5. The preparation method according to claim 1, wherein the microwave hot-pressing reaction time is 5-100 min.
6. The preparation method according to claim 1, wherein the microwave power of the microwave hot-pressing reaction is 100-500 w.
7. The preparation method according to claim 1, wherein the temperature of the microwave hot-pressing reaction is 100 to 240 ℃.
8. The manufacturing method according to claim 1, wherein the microwave hot-pressing device comprises a tablet upper pressing plate, a tablet lower pressing plate and a microwave transmitting plate; a material groove is arranged in the pressing plate lower pressing plate; the microwave transmitting plate is arranged at the lower part of the pressing plate upper pressing plate, is integrated with the pressing plate upper pressing plate and is matched with the pressing plate lower pressing plate groove.
9. The preparation method according to claim 8, wherein the microwave hot-pressing reaction is carried out at a rate of 0.1 to 100mm/s for the upper and lower pressing plates of the microwave hot-pressing device.
10. The method of claim 1, wherein obtaining the lithium bis (oxalato) borate further comprises dissolving the lithium bis (oxalato) borate in an organic solvent, filtering, concentrating, and drying.
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