CN112002943B - Electrolyte and preparation method and application thereof - Google Patents

Electrolyte and preparation method and application thereof Download PDF

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CN112002943B
CN112002943B CN202010947298.2A CN202010947298A CN112002943B CN 112002943 B CN112002943 B CN 112002943B CN 202010947298 A CN202010947298 A CN 202010947298A CN 112002943 B CN112002943 B CN 112002943B
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electrolyte
polyfluoroether
lithium
carbonate
solvent
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CN112002943A (en
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谭强强
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Institute of Process Engineering of CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • 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
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to an electrolyte, a preparation method and an application thereof, wherein the electrolyte contains polyfluoroether, lithium salt and a solvent. The electrolyte is added with the polyfluoroether, the molecular structure of the polyfluoroether additive is similar to that of hydrocarbons, but fluorine atoms in molecules replace hydrogen atoms, and because the fluorine atoms have strong electronegativity and the bond energy is as high as 418kJ/mol to 502.08kJ/mol, the polyfluoroether has higher thermal stability and oxidation stability as well as good chemical inertness and insulating property. Thereby improving the high pressure resistance and high temperature resistance of the electrolyte and ensuring good electrochemical performance.

Description

Electrolyte and preparation method and application thereof
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to an electrolyte and a preparation method and application thereof.
Background
Lithium ion batteries are an energy storage device that plays a major role in modern society because of their large energy density. At present, most of portable devices used in life and work of people, such as personal computers, smart phones, ipads and the like, adopt lithium ion batteries for power supply. The electrolyte is used as an important component of the battery, plays a role in charge transfer between a positive electrode and a negative electrode in the battery, and has important influence on the specific capacity, the working temperature range, the cycle efficiency, the safety performance and the like of the battery. The electrolyte of the lithium battery consists of an organic solvent, an electrolyte lithium salt and necessary additives.
Safety is a key issue that restricts the development of high-capacity and high-power lithium ion batteries. At present, the electrolyte of the lithium ion battery mainly takes organic carbonate as a solvent, and the electrolyte has excellent electrochemical performance, but has the characteristics of low lightning, flammability and the like, so that the battery is extremely easy to catch fire and even explode under the conditions of overcharge and overheating.
Currently, liquid electrolytes, gel state and solid electrolytes present a number of challenges. More improvements are needed to be studied to balance the differences between different electrolytes, achieving high energy density and higher safety.
CN107069094A discloses an ultralow temperature discharge lithium ion battery electrolyte. The electrolyte consists of electrolyte lithium salt, cyclic ether compounds, organic carbonate, ethylene glycol dimethyl ether and N, N-dimethyl trifluoroacetamide; the electrolyte lithium salt is lithium hexafluorophosphate and lithium bis (oxalato) borate, and the lithium bis (oxalato) borate is mixed according to the mass ratio of 3:1: 1. According to the invention, the organic additive N, N-dimethyl trifluoroacetamide is mixed with organic carbonate, so that the freezing point of a mixed solvent can be obviously reduced, the low-temperature electrolyte is formed, and the electrolyte prepared by reasonably proportioning three lithium salts, namely lithium hexafluorophosphate, lithium bis (oxalato) borate and lithium oxalato difluoro borate overcomes the defect of lack of temperature stability when the lithium hexafluorophosphate is singly used, and has better low-temperature performance and high-rate discharge performance. However, the solvent used in the invention is flammable and explosive, and has potential safety hazard.
CN103762382A discloses an electrolyte of a lithium ion battery and a lithium battery containing the electrolyte, wherein the electrolyte consists of organic carbonates and hydroxybenzene carbonate, the hydroxybenzene carbonate is dissolved in the organic carbonates, and the mass of the hydroxybenzene carbonate accounts for 0.1-2% of the total mass of the electrolyte. The invention improves the thermal stability of the passive film of the solid electrolyte interface of the negative electrode of the lithium battery and prolongs the charge-discharge cycle service life of the lithium battery at high temperature. Meanwhile, the electrolyte does not generate gases such as ethylene or propylene during charging and discharging, so that the battery does not swell and the safety of the battery is improved. Although the present invention solves the problem of the generation of gases such as ethylene and propylene, organic carbonates themselves have a low flash point and are liable to be burned and exploded when the temperature is too high.
CN107154510A discloses a lithium ion battery electrolyte and a lithium ion battery. A lithium ion battery electrolyte includes a solvent and a lithium salt; the solvent comprises ethylene carbonate, 2-butanone and dichloromethane; the mass ratio of the ethylene carbonate to the 2-butanone to the dichloromethane is 1-2: 1-7: 1-7. The lithium ion battery electrolyte and the lithium ion battery take ethylene carbonate, 2-butanone and dichloromethane as solvents, and the ethylene carbonate can form a stable SEI film in the using process; the 2-butanone and the dichloromethane both have lower melting points, have better chemical stability at low temperature and normal temperature, and still show better solubility at lower temperature. The three solvents are matched for use and are reasonably proportioned, so that the lithium ion battery electrolyte and the lithium ion battery can have better electrochemical performance and stability at low temperature. However, the lithium ion battery of the invention still has certain potential safety hazard in practical application, especially under the conditions of high temperature and high pressure.
Therefore, the development of a novel electrolyte or a lithium ion battery is urgently needed in the field, and the problem that a common product is poor in high-pressure resistance and high-temperature resistance is solved, so that the problem that the common product is flammable and explosive is solved, and the safety is improved.
Disclosure of Invention
An object of the present invention is to provide an electrolyte which has excellent high-pressure and high-temperature resistance, is less likely to cause combustion and explosion, and is highly safe.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an electrolyte, which contains polyfluoroether, lithium salt and a solvent.
The electrolyte is added with the polyfluoroether, the molecular structure of the polyfluoroether additive is similar to that of hydrocarbons, but fluorine atoms in molecules replace hydrogen atoms, and because the fluorine atoms have strong electronegativity and the bond energy is as high as 418kJ/mol to 502.08kJ/mol, the polyfluoroether has higher thermal stability and oxidation stability as well as good chemical inertness and insulating property. Thereby improving the high pressure resistance and high temperature resistance of the electrolyte and ensuring good electrochemical performance.
In the present invention, the preparation method of the polyfluoroether is common knowledge in the art, and those skilled in the art can select an appropriate preparation method according to actual circumstances or can obtain the polyfluoroether commercially (for example, perfluoropolyether Krytox157-FSH from dupont), and the present invention is not limited thereto.
Preferably, the polyfluoroether is a perfluoropolyether.
Preferably, the polyfluoroether has a number average molecular weight of 6X 102～6×104E.g. 7X 102、8×102、 9×102、1×103、2×103、3×103、4×103、5×103、6×103、7×103、8×103、 9×103、1×104、2×104、3×104、4×104、5×104And the like.
Preferably, the polyfluoroether contains 0 to 2 end-capping functional groups, such as 1, including any one or a combination of at least two of carboxyl, hydroxyl, or vinyl groups.
Preferably, the polyfluoroether does not contain end-capping functional groups.
The invention further prefers polyfluoroether without end-capping functional groups, because the active end groups can react with lithium sheets in lithium batteries, thereby influencing the electrochemical performance and the high-temperature and high-pressure resistance.
Preferably, the lithium salt comprises any one or a combination of at least two of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium hexafluoroarsenate, lithium trifluoromethanesulfonate or lithium bis (trifluoromethylsulfonyl) imide.
Preferably, the solvent includes any one or a combination of at least two of ethylene carbonate, ethyl methyl carbonate, propylene carbonate, diethyl carbonate, dimethyl carbonate, propylene carbonate, acetate, propionate, butyrate, perfluorohexane, perfluorodecalin, tetrahydrofuran, fluoroethylene carbonate, vinylene carbonate, nonafluoromethoxybutane, nonafluoroethoxybutane, 1, 2-trifluorotrichloroethane, pentafluoromonochloroethane, perfluoroheptane, decafluoropentane, hexafluorobenzene, acetone, dimethylformamide, or dimethylacetamide.
Preferably, the mass fraction of the polyfluoroether in the electrolyte is 1% to 7%, for example 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, etc., preferably 2% to 4%.
Preferably, the mass ratio of the polyfluoroether to the solvent to the lithium salt is (1-5): 2-8): 2-6, for example, (1-5) includes 2, 3 or 4, etc., (2-8) includes 3, 4, 5, 6 or 7, etc., (2-6) includes 3, 4 or 5, etc., and further preferably (2-4): 4-7): 3-5.
Another object of the present invention is to provide a method for preparing the electrolyte solution according to the first object, the method comprising: and mixing polyfluoroether, lithium salt and a solvent, and stirring to obtain the electrolyte.
Preferably, the mixing and stirring are both performed in a glove box.
Preferably, the glove box is filled with an inert gas, preferably argon.
Preferably, the glove box has a water oxygen value of < 1ppm, such as 0.1ppm, 0.2ppm, 0.3ppm, 0.4ppm, 0.5ppm, 0.6ppm, 0.7ppm, 0.8ppm, 0.9ppm, and the like.
The invention also provides a lithium ion battery, which comprises the electrolyte for one purpose.
The lithium ion battery provided by the invention has excellent high-pressure resistance and high-temperature resistance, is not easy to combust and explode, and has high safety and good electrochemical performance.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, polyfluoroether is added into the electrolyte, fluorine atoms in molecules of the additive replace hydrogen atoms, and because the fluorine atoms have strong electronegativity and the bond energy is as high as 418kJ/mol to 502.08kJ/mol, the polyfluoroether has higher thermal stability and oxidation stability and good chemical inertness and insulating property, so that the high-pressure resistance and high-temperature resistance of the electrolyte can be improved, and meanwhile, good electrochemical performance is ensured.
The lithium ion battery provided by the invention has the high-pressure cycle capacity retention rate of 86-94%, the high-temperature cycle capacity retention rate of 84-93%, and the first-cycle capacity of 191-220mAh g-1The first week efficiency is 83-90%.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
Mixing ethylene carbonate and fluoroethylene carbonate according to the mass fraction of 30 wt% and 70 wt% to obtain a solvent, adding lithium trifluoromethanesulfonate with the lithium ion concentration of 0.5mol/L, and adding 2 wt% of perfluoropolyether (hydroxyl terminated, molecular weight of 6 x 10) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 2
Mixing ethylene ester and fluoroethylene carbonate according to the mass fraction of 40 wt% and 60 wt% to obtain a solvent, adding lithium bis (trifluoromethylsulfonyl) imide with the lithium ion concentration of 1mol/L, and adding 1 wt% of perfluoropolyether (inactive end group, molecular weight of 6 x 10) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 3
Fluoroethylene carbonate and perfluorohexane are mixed according to the mass fraction of 35 wt% to 75 wt%Mixing the components in proportion as a solvent, adding lithium tetrafluoroborate, adding 5 wt% of perfluoropolyether (hydroxyl end capping, molecular weight of 8 multiplied by 10) according to the total mass of the electrolyte, wherein the lithium ion concentration is 1.5mol/L3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 4
Perfluorodecalin as solvent, lithium hexafluorophosphate in the concentration of 0.5mol/L and perfluoropolyether in the amount of 8 wt% based on the total electrolyte mass (hydroxyl end capped and molecular weight of 6X 10)3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 5
Mixing vinyl ester and perfluorodecalin according to the mass fraction of 30 wt% and 70 wt% to obtain a solvent, adding lithium tetrafluoroborate, wherein the lithium ion concentration is 1.5mol/L, and adding 4 wt% of perfluoropolyether (vinyl-terminated, molecular weight is 5 multiplied by 10) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 6
Mixing ethylene carbonate and fluoroethylene carbonate according to the mass fraction of 35 wt% and 65 wt% to obtain a solvent, adding lithium trifluoromethanesulfonate with a lithium ion concentration of 0.5mol/L, and adding 3 wt% of perfluoropolyether (hydroxyl-terminated, molecular weight of 4 x 10) according to the total mass of the electrolyte4) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 7
Mixing dimethyl carbonate and perfluorohexane ester according to the mass fraction of 30 wt% and 70 wt% to obtain a solvent, adding lithium bis (trifluoromethylsulfonyl) imide with the lithium ion concentration of 2mol/L, and adding 5 wt% of perfluoropolyether (double-bond end-capped, molecular weight of 8 x 10 and the like) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 8
Mixing ethylene carbonate and fluoroethylene carbonate according to the mass fraction of 30 wt% and 70 wt% to obtain a solvent, adding lithium hexafluorophosphate, wherein the lithium ion concentration is 1.5mol/L, and adding 2 wt% of perfluoropolyether according to the total mass of the electrolyte(hydroxyl terminated, molecular weight 7X 102) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 9
Mixing ethylene carbonate and fluoroethylene carbonate according to the mass fraction of 30 wt% and 70 wt% to obtain a solvent, adding lithium trifluoromethanesulfonate with the lithium ion concentration of 0.5mol/L, and adding 10 wt% of perfluoropolyether (inactive end group, molecular weight of 6 x 10) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 10
Mixing ethylene carbonate and fluoroethylene carbonate according to the mass fraction of 20 wt% and 80 wt% to obtain a solvent, adding lithium hexafluoroarsenate, wherein the lithium ion concentration is 1.5mol/L, and adding 2 wt% of perfluoropolyether (inactive end group, molecular weight is 5 multiplied by 10) according to the total mass of the electrolyte4) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 11
Mixing propyl carbonate and perfluorodecalin according to the mass fraction of 50 wt% and 50 wt% to obtain a solvent, adding lithium trifluoromethanesulfonate with the lithium ion concentration of 2.5mol/L, and adding 20 wt% of perfluoropolyether (hydroxyl terminated, molecular weight of 3 x 10) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Example 12
Mixing ethylene carbonate and fluoroethylene carbonate according to the mass fraction of 10 wt% and 90 wt% to obtain a solvent, adding lithium trifluoromethanesulfonate with the lithium ion concentration of 1.5mol/L, and adding 3 wt% of perfluoropolyether (carboxyl-terminated, molecular weight of 5 × 10) according to the total mass of the electrolyte3) And fully stirring at 25 ℃ to obtain the electrolyte of the lithium ion battery.
Comparative example 1
The difference from example 1 is that the perfluoropolyether is replaced with an equal mass of 4 methyl N tosylbenzenesulfonamide.
Comparative example 2
The difference from example 1 is that perfluoropolyether is replaced by an equal mass of trispyrrole phosphate
Comparative example 3
The difference from example 1 is that perfluoropolyether is replaced with an equal mass of polyetheretherketone.
Performance testing
The electrolytes obtained in the above examples and comparative examples are respectively prepared into lithium ion batteries, and the preparation method is as follows:
and sequentially stacking the positive plate (lithium plate), the diaphragm, the prepared electrolyte and the negative lithium plate, pressing at room temperature of 20MPa, assembling into the lithium battery, and then carrying out performance test.
The following tests were carried out for the lithium ion batteries prepared in examples and comparative examples:
(1) high pressure resistance test: and standing the prepared lithium battery for 24 hours, performing 100 charge-discharge cycle tests in a voltage range of 4V-4.8V and under a current of 1C, and recording the capacity retention rate of the battery after 200 cycles.
(2) And (3) high temperature resistance test: and standing the prepared lithium battery in a constant temperature box at 60 ℃ for 8 hours, carrying out 100 charge-discharge cycle tests in a voltage range of 3.0V-4.3V and under a current of 1C, and recording the capacity retention rate of the battery after 100 cycles.
(3) And (3) electrochemical performance testing: and standing the prepared lithium battery for 24 hours, performing charge-discharge test in a voltage interval of 3.0V-4.8V and under a current of 0.2C, and recording the first-week discharge capacity and the first-week efficiency.
The results of the above tests are shown in table 1.
TABLE 1
Figure BDA0002675730400000081
Figure BDA0002675730400000091
As can be seen from Table 1, the electrolyte provided by the invention has excellent high pressure resistance and high temperature resistance, is not easy to combust and explode, has high safety and good electrochemical performance. Comparative examples 1-3 the polyfluoroether was replaced with other additives and the high pressure and high temperature resistance properties were inferior to those of the examples.
It is understood from the comparison between example 1 and example 2 that the polyfluoroether containing no functional group end-capping (example 2) can further improve the high pressure and high temperature resistance and the electrochemical performance as compared with the polyfluoroether containing a functional group end-capping (example 1).
The present invention is illustrated in detail by the examples described above, but the present invention is not limited to the details described above, i.e., it is not intended that the present invention be implemented by relying on the details described above. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (14)

1. An electrolyte, characterized in that the electrolyte consists of polyfluoroether, lithium salt and a solvent;
the number average molecular weight of the polyfluoroether is 3 multiplied by 103～6×104；
The mass fraction of the polyfluoroether in the electrolyte is 1-7%.
2. The electrolyte of claim 1, wherein the polyfluoroether contains 0 to 2 end-capping functional groups comprising any one or a combination of at least two of carboxyl, hydroxyl, or vinyl groups.
3. The electrolyte of claim 2, wherein the polyfluoroether does not contain end-capping functional groups.
4. The electrolyte of claim 1, wherein the lithium salt comprises any one or a combination of at least two of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium hexafluoroarsenate, lithium trifluoromethanesulfonate, or lithium bis (trifluoromethylsulfonyl) imide.
5. The electrolyte of claim 1, wherein the solvent comprises any one or a combination of at least two of ethylene carbonate, ethyl methyl carbonate, propylene carbonate, diethyl carbonate, dimethyl carbonate, propylene carbonate, acetate, propionate, butyrate, perfluorohexane, perfluorodecalin, tetrahydrofuran, fluoroethylene carbonate, vinylene carbonate, nonafluoromethoxybutane, nonafluoroethoxybutane, 1, 2-trifluorotrichloroethane, pentafluoromonochloroethane, perfluoroheptane, decafluoropentane, hexafluorobenzene, acetone, dimethylformamide, or dimethylacetamide.
6. The electrolyte of claim 1, wherein the mass fraction of polyfluoroether in the electrolyte is between 2% and 4%.
7. The electrolyte of claim 1, wherein the mass ratio of the polyfluoroether to the solvent to the lithium salt is (1-5): (2-8): (2-6).
8. The electrolyte of claim 7, wherein the mass ratio of the polyfluoroether to the solvent to the lithium salt is (2-4) to (4-7) to (3-5).
9. A method of preparing the electrolyte of any of claims 1-8, comprising: and mixing polyfluoroether, lithium salt and a solvent, and stirring to obtain the electrolyte.
10. The method of claim 9, wherein the mixing and agitating are both performed in a glove box.
11. The method of claim 10, wherein the glove box is filled with an inert gas.
12. The method of claim 11, wherein the inert gas is argon.
13. The method of claim 10, wherein the glove box has a water oxygen value of < 1 ppm.
14. A lithium ion battery comprising the electrolyte of any one of claims 1-8.
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Inventor before: Lou Pingping

Inventor before: Ji Xueqian

Inventor before: Wang Pengfei

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