CN109851640A - Double oxalic acid lithium phosphates of a kind of difluoro and the preparation method and application thereof - Google Patents
Double oxalic acid lithium phosphates of a kind of difluoro and the preparation method and application thereof Download PDFInfo
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- CN109851640A CN109851640A CN201910042603.0A CN201910042603A CN109851640A CN 109851640 A CN109851640 A CN 109851640A CN 201910042603 A CN201910042603 A CN 201910042603A CN 109851640 A CN109851640 A CN 109851640A
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Abstract
The invention discloses double oxalic acid lithium phosphates of a kind of difluoro and the preparation method and application thereof.The present invention by will be bis- (trimethyl silicane) oxalate and lithium hexafluoro phosphate be miscible in nonaqueous solvents, 12~30h is stirred to react under 70~90 DEG C, atmosphere of inert gases, reaction solution is obtained, the insoluble matter in reaction solution is filtered to remove to obtain the double oxalic acid lithium phosphate solution of difluoro；On this basis, the present invention obtains the double oxalic acid lithium phosphates of difluoro further by the double oxalic acid lithium phosphate solution of the difluoro after reduced pressure, low temperature cosolvent crystallization, ageing, vacuum drying.In terms of the double oxalic acid lithium phosphates of difluoro of the present invention, solution can be applicable to electrolyte addictive with dual functions.The synthetic method of the double oxalic acid lithium phosphates of difluoro of the present invention is very simple, non-environmental-pollution；Meanwhile the purity is high of the double oxalic acid lithium phosphates of the preparation-obtained difluoro of the present invention.
Description
Technical field
The invention belongs to key component in battery electrolytic solution (lithium salts or additive) more particularly to a kind of double oxalic acid of difluoro
The double oxalic acid lithium phosphates of the preparation method and the difluoro of phosphoric acid crystalline lithium and its solution are as electrolyte addictive with dual functions side
The application in face.
Background technique
The double oxalic acid lithium phosphates of difluoro, not only can be effective by being formed in anode as a kind of electrolyte addictive with dual functions
Protective film, improve battery entirety high voltage cycle performance, while will not in the system using carbon-based material as cathode greatly
Volume production gas effectively avoids the problem that battery gas rises, improves security performance.Patent No. CN102216311B discloses a kind of difluoro
Bis- (oxalates) closes the manufacturing method of lithium phosphate solution, and this method synthesizes the double oxalic acid lithium phosphates of difluoro by the introducing of silicon tetrachloride
Solution, but this method complicated condition, can introduce the chloride for being difficult to take out, free acid, and yield is lower, and be difficult industrial metaplasia
It produces.
Summary of the invention
The purpose of the present invention is to provide a kind of double oxalic acid lithium phosphates of difluoro, including its solution, crystal form.
A further object of the present invention is to provide the preparation methods of the double oxalic acid lithium phosphates of above-mentioned difluoro, it is intended to solve existing side
Method complicated condition can introduce the chloride for being difficult to remove, free acid, and yield is lower, and the problem of be difficult industrialized production.
A further object of the present invention is to provide the double oxalic acid lithium phosphates of above-mentioned difluoro as electrolyte addictive with dual functions
The application of aspect
The invention is realized in this way the invention discloses a kind of preparation method of the double oxalic acid lithium phosphates of difluoro, this method
The following steps are included: reaction raw materials are miscible in nonaqueous solvents by (1), it is stirred to react under 70~90 DEG C, atmosphere of inert gases
12~30h obtains reaction solution；The reaction raw materials include in molar ratio be 1:(0.5~3) lithium hexafluoro phosphate and bis- (front threes
Base silicon) oxalate；Insoluble matter in reaction solution is filtered to remove to obtain the double oxalic acid lithium phosphate solution of difluoro.
Preferably, (2) are further comprised the steps of: after step (1) to depressurize the double oxalic acid lithium phosphate solution of the difluoro
- 30~-10 DEG C of cosolvents are added after saturated solution to be generated for concentration, be mixed be precipitated to crystal, ageing 1~for 24 hours, obtain
The double oxalic acid phosphoric acid crystalline lithiums of difluoro.
Preferably, the molar ratio of the lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalates is 1:(1.25~1.9), at this
The double oxalic acid lithium phosphate purity of gained difluoro are higher under ratio.
Preferably, in step (1), mass concentration of the reaction raw materials in nonaqueous solvents is 40~70%；It is described
Nonaqueous solvents is aprotic solvents；In the nonaqueous solvents moisture content within 20ppm, purity be 99.5% or more；Instead
It answers process that moisture should be avoided and enters reaction system, it will cause a large amount of decomposition of the double oxalic acid lithium phosphates of difluoro, reaction should be stringent
Moisture is controlled, therefore, moisture content is less than 1ppm in the atmosphere of inert gases, oxygen content is less than 1ppm；The indifferent gas
Body is at least one of nitrogen, argon gas, helium.
Preferably, the aprotic solvents include cyclic carbonate, linear carbonate, chain nitrile, cyclic sulfones class.
Preferably, in step (2), the cosolvent is the mixed solvent of alkane and ether；Wherein, the ether be ether,
Propyl ether, butyl ether, glycol monomethyl ether, glycol dimethyl ether, ethylene glycol monobutyl ether (EGMBE), ethylene glycol diethyl ether, in petroleum ether at least
It is a kind of；The ethers is that hydrocarbon alkane is at least one of propane, butane, hexane.
The present invention further discloses the double oxalic acid lithium phosphates of difluoro that the above method is prepared, the double oxalic acid phosphoric acid of the difluoro
Lithium can be solution, crystal or Amorphous solids.
The present invention further discloses the double oxalic acid lithium phosphates of above-mentioned difluoro in terms of as electrolyte addictive with dual functions
Using.
The present invention overcomes the deficiencies of the prior art and provide double oxalic acid lithium phosphates of a kind of difluoro and the preparation method and application thereof.
The present invention in nonaqueous solvents by mixing bis- (trimethyl silicane) oxalates and lithium hexafluoro phosphate, in 70~90 DEG C, indifferent gas
It is stirred to react 12~30h under body atmosphere, obtains reaction solution, products therefrom is the double oxalic acid of difluoro after filtering insoluble matter therein
Lithium phosphate solution.The process of each compound reaction is as follows in the reaction solution:
On this basis, the present invention can also by the double oxalic acid lithium phosphate solution of difluoro be concentrated under reduced pressure, low temperature hydrotropy
Agent crystallization, ageing obtain the crystal form of the double oxalic acid lithium phosphates of the difluoro, further, it is also possible to further carry out to the crystal true
After sky is dried, the Amorphous solids form of the double oxalic acid lithium phosphates of the difluoro is obtained.
Compared with the prior art the shortcomings that and deficiency, the invention has the following advantages: the double oxalic acid phosphorus of difluoro of the present invention
The synthetic method of sour lithium is very simple, and reaction product contains only a kind of tail gas, which can be carried out by esters solvent
It absorbs, environmental pollution can be avoided completely；Meanwhile the present invention changes the double oxalic acid lithium phosphates of difluoro by the method for low temperature cosolvent and exists
The principle of different solvents different solubility improves the purity of the double oxalic acid lithium phosphate solids of preparation-obtained difluoro.
Detailed description of the invention
Fig. 1 is the 19F nuclear magnetic spectrogram of the double oxalic acid lithium phosphates of difluoro of the present invention；
Fig. 2 is the infrared comparison diagram of Fourier of difluoro of the present invention double oxalic acid lithium phosphate solution and sample solution.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 60.0g electricity is added in 500mL two mouth flask
Sub- grade methyl ethyl carbonate dissolves hexafluorophosphoric acid 13.0g, bis- (trimethyl silicane) oxalate 21.0g thereto, in 60 after stirring and dissolving
~90 DEG C of confined reactions.It is provided with bubbler and sufficiently reacts 20h until excluding gas (CH3)3SiF.Gained after reaction is muddy
The colorless and transparent extraction raffinate of about 78g (the double oxalic acid lithium phosphate solution of difluoro, similarly hereinafter) are obtained after liquid cold filtration, take a small amount of test atom
It absorbs, wherein lithium salt content is about 15.3%.
Embodiment 2
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 50.0g electricity is added in 500mL two mouth flask
The mixture of sub- grade dimethyl carbonate and ethylene carbonate is being charged with 7.0g lithium hexafluoro phosphate and the bis- (trimethyls of 25.0g
Silicon) oxalate, in 60~90 DEG C of confined reactions after stirring and dissolving.Bubbler is provided with sufficiently to react for 24 hours until excluding gas
(CH3)3SiF.The colorless and transparent extraction raffinate of about 88g is obtained after gained troubled liquor cold filtration after reaction, a small amount of test atom is taken to inhale
It receives, wherein lithium salt content is about 21.7%.
Embodiment 3
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 95.0g electricity is added in 500mL two mouth flask
The mixture of sub- grade methyl ethyl carbonate and ethylene carbonate is being charged with 35.0g lithium hexafluoro phosphate and the bis- (trimethyls of 108g
Silicon) oxalate, in 60~90 DEG C of confined reactions after stirring and dissolving.Bubbler is provided with sufficiently to react for 24 hours until excluding gas
(CH3)3SiF.The colorless and transparent extraction raffinate of about 160g is obtained after gained troubled liquor cold filtration after reaction, a small amount of test atom is taken
It absorbs, wherein lithium salt content is about 21.7%.
Embodiment 4
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 95.0g electricity is added in 500mL two mouth flask
Sub- grade methyl ethyl carbonate ester solvent is being charged with 35.0g lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalates of 108g, is stirring molten
In 60~80 DEG C of confined reactions after solution.It is provided with bubbler and sufficiently reacts 30h until excluding gas (CH3)3SiF.After reaction
The colorless and transparent extraction raffinate of about 160g is obtained after gained troubled liquor cold filtration, the solution is concentrated makes its concentration reach 75% left side
Then the right side is charged with cold hexamethylene/ether mixed solvent.After ageing for 24 hours, filters and produced after crystal is precipitated completely
Product are dried in -20 DEG C of vacuum ovens.
Embodiment 5
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 200.0g is added in 500mL two mouth flask
Electron level methyl ethyl carbonate ester solvent is being charged with 70.0g lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalates of 216g, stirring
In 60~80 DEG C of confined reactions after dissolution.It is provided with bubbler and sufficiently reacts 30h until excluding gas (CH3)3SiF.Reaction
The colorless and transparent extraction raffinate of about 280.0g is obtained after gained troubled liquor cold filtration afterwards, the solution is concentrated reaches its concentration
50% or so, then it is charged with cold butane/petroleum ether mixed solvent.After ageing for 24 hours, filtered after crystal is precipitated completely
Product is obtained, is dried in -20 DEG C of vacuum ovens.
Embodiment 6
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 200.0g is added in 500mL two mouth flask
Electron level methyl ethyl carbonate ester solvent is being charged with 1mmol lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalates of 0.5mmol,
In 60~80 DEG C of confined reactions after stirring and dissolving.It is provided with bubbler and sufficiently reacts 30h until excluding gas (CH3)3SiF.?
The colorless and transparent extraction raffinate of about 280.0g is obtained after gained troubled liquor cold filtration after reaction, the solution is concentrated reaches its concentration
To 50% or so, it is then charged with cold butane/petroleum ether mixed solvent.After ageing for 24 hours, taken out after crystal is precipitated completely
Filter obtains product, dries in -20 DEG C of vacuum ovens.
Embodiment 7
In the glove box that moisture content and oxygen content are respectively less than 1ppm, 200.0g is added in 500mL two mouth flask
Electron level methyl ethyl carbonate ester solvent is being charged with 1mmol lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalates of 3mmol, is stirring
It mixes after dissolving in 60~80 DEG C of confined reactions.It is provided with bubbler and sufficiently reacts 30h until excluding gas (CH3)3SiF.Anti-
The colorless and transparent extraction raffinate of about 280.0g should be obtained after rear gained troubled liquor cold filtration, the solution is concentrated reaches its concentration
50% or so, then it is charged with cold butane/petroleum ether mixed solvent.After ageing for 24 hours, filtered after crystal is precipitated completely
Product is obtained, is dried in -20 DEG C of vacuum ovens.
Effect example
Nuclear-magnetism 19F analysis is carried out to solution obtained in embodiment 2, it as a result as shown in Figure 1, can after analyzing Fig. 1
To find out, the corresponding spectrogram of the double oxalic acid lithium phosphates of the difluoro within the scope of this, can analyze the double grass of difluoro of synthesis from figure
Acid phosphoric acid lithium solution impurity content is low, purity is high.
The methyl ethyl carbonate ester solution of the double oxalic acid lithium phosphates of the difluoro that embodiment 2 is obtained and sample solution are red by Fourier
External spectrum figure compares, as a result as shown in Fig. 2, gone out peak position can analyze product synthesized by the present invention and sample peak from Fig. 2
Position is basic to be corresponded, and also illustrates that products obtained therefrom purity is higher.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of preparation method of the double oxalic acid lithium phosphates of difluoro, which is characterized in that method includes the following steps:
(1) reaction raw materials are miscible in nonaqueous solvents, are stirred to react 12~30h under 70~90 DEG C, atmosphere of inert gases, obtain
To reaction solution；The reaction raw materials include in molar ratio be 1:(0.5~3) lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalic acid
Ester；Insoluble matter in reaction solution is filtered to remove to obtain the double oxalic acid lithium phosphate solution of difluoro.
2. the preparation method of the double oxalic acid lithium phosphates of difluoro as described in claim 1, which is characterized in that after step (1) also
Comprising steps of
(2) the double oxalic acid lithium phosphate solution of the difluoro are concentrated under reduced pressure, -30~-10 DEG C is added after saturated solution to be generated
Cosolvent, be mixed be precipitated to crystal, ageing 1~for 24 hours, obtain the double oxalic acid phosphoric acid crystalline lithiums of difluoro.
3. the preparation method of the double oxalic acid lithium phosphates of difluoro as described in claim 1, which is characterized in that described in step (1)
The molar ratio of lithium hexafluoro phosphate and bis- (trimethyl silicane) oxalates is 1:(1.25~1.9).
4. the preparation method of the double oxalic acid lithium phosphates of difluoro as described in claim 1, which is characterized in that described in step (1)
Mass concentration of the reaction raw materials in nonaqueous solvents is 40~70%；The nonaqueous solvents is aprotic solvents；It is described non-aqueous
In solvent moisture content within 20ppm, purity be 99.5% or more；Moisture content is less than in the atmosphere of inert gases
1ppm, oxygen content are less than 1ppm；The inert gas is at least one of nitrogen, argon gas, helium.
5. the preparation method of the double oxalic acid lithium phosphates of difluoro as claimed in claim 4, which is characterized in that the aprotic solvents
Including cyclic carbonate, linear carbonate, chain nitrile, cyclic sulfones class.
6. the preparation method of the double oxalic acid lithium phosphates of difluoro as claimed in claim 2, which is characterized in that described in step (2)
Cosolvent is the mixed solvent of alkane and ether；Wherein, the ether is ether, propyl ether, butyl ether, glycol monomethyl ether, ethylene glycol two
At least one of methyl ether, ethylene glycol monobutyl ether (EGMBE), ethylene glycol diethyl ether, petroleum ether；The ethers be hydrocarbon alkane be propane, butane,
At least one of hexane.
7. the double oxalic acid lithium phosphates of the difluoro that the described in any item methods of claim 1~6 are prepared.
8. double applications of the oxalic acid lithium phosphate in terms of as electrolyte addictive with dual functions of difluoro as claimed in claim 7.
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Cited By (8)
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| CN110204576A (en) * | 2019-07-18 | 2019-09-06 | 东莞东阳光科研发有限公司 | A kind of preparation method of the double oxalic acid lithium phosphate solution of difluoro |
| CN110240617A (en) * | 2019-06-19 | 2019-09-17 | 上海如鲲新材料有限公司 | A kind of preparation method of difluoro dioxalic acid lithium phosphate |
| CN110845539A (en) * | 2019-11-26 | 2020-02-28 | 九江天赐高新材料有限公司 | Preparation method and application of battery-grade lithium difluorobis (oxalato) phosphate solid |
| CN111606952A (en) * | 2020-05-14 | 2020-09-01 | 东莞东阳光科研发有限公司 | Preparation method of lithium tetrafluorooxalate phosphate, nonaqueous electrolyte and battery |
| CN111943984A (en) * | 2020-08-17 | 2020-11-17 | 常德市大度新材料有限公司 | Difluorodioxalato phosphate, preparation method thereof and application thereof in non-aqueous electrolyte |
| CN113717227A (en) * | 2020-05-26 | 2021-11-30 | 恒大新能源技术(深圳)有限公司 | Preparation method of lithium difluorobis (oxalato) phosphate and derivatives thereof, electrolyte and secondary battery |
| CN113793975A (en) * | 2021-08-31 | 2021-12-14 | 湖南法恩莱特新能源科技有限公司 | Preparation method of fluorine-containing electrolyte |
| CN115583974A (en) * | 2022-01-13 | 2023-01-10 | 安徽新宸新材料有限公司 | Preparation method of lithium difluorobis (oxalate) phosphate |
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| CN111606952A (en) * | 2020-05-14 | 2020-09-01 | 东莞东阳光科研发有限公司 | Preparation method of lithium tetrafluorooxalate phosphate, nonaqueous electrolyte and battery |
| CN111606952B (en) * | 2020-05-14 | 2022-04-29 | 东莞东阳光科研发有限公司 | Preparation method of lithium tetrafluorooxalate phosphate, nonaqueous electrolyte and battery |
| CN113717227A (en) * | 2020-05-26 | 2021-11-30 | 恒大新能源技术(深圳)有限公司 | Preparation method of lithium difluorobis (oxalato) phosphate and derivatives thereof, electrolyte and secondary battery |
| CN111943984A (en) * | 2020-08-17 | 2020-11-17 | 常德市大度新材料有限公司 | Difluorodioxalato phosphate, preparation method thereof and application thereof in non-aqueous electrolyte |
| CN113793975A (en) * | 2021-08-31 | 2021-12-14 | 湖南法恩莱特新能源科技有限公司 | Preparation method of fluorine-containing electrolyte |
| CN115583974A (en) * | 2022-01-13 | 2023-01-10 | 安徽新宸新材料有限公司 | Preparation method of lithium difluorobis (oxalate) phosphate |
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