CN108878978A - A kind of anti-overcharge lithium battery electrolytes containing silicone additives - Google Patents
A kind of anti-overcharge lithium battery electrolytes containing silicone additives Download PDFInfo
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- CN108878978A CN108878978A CN201810699962.9A CN201810699962A CN108878978A CN 108878978 A CN108878978 A CN 108878978A CN 201810699962 A CN201810699962 A CN 201810699962A CN 108878978 A CN108878978 A CN 108878978A
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- lithium
- overcharge
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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
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/42—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
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- 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
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- General Physics & Mathematics (AREA)
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Abstract
The present invention provides a kind of anti-overcharge lithium-ion battery electrolytes containing silicone additives, the electrolyte include lithium salts, double solvents and additive A, and the additive A is a kind of organosilicon derivates, and general structure is：It is using silicon oxygen bond as main chain, wherein n1For the natural number in 2-20, when biphenyl class formation is containing there are four to overcharge in the main structure of molecule, the electrochemical polymer of formation crosslinking, preferably protects battery.
Description
Technical field
The present invention relates to lithium ion battery preparation technical field more particularly to a kind of anti-overcharge lithiums containing silicone additives
Battery electrolyte.
Background technique
With the development of economy with the progress of science and technology, portable electronic device, hybrid electric vehicle, electric car etc. are increasingly
It is widely deep into the production and living of people, in these equipment, lithium ion battery is very widely used.However, safety
Problem but emerges one after another, and process is one of most incident safety problem in lithium ion battery use.Due to current lithium ion
For battery mostly using the carbonates organic electrolyte extremely to burn, battery very likely causes battery in super-charge super-discharge and overheat
Burning even explode, thus very big security risk is caused to battery, particularly power battery.By improving the steady of electrolyte
Qualitative, such as adding anti-overcharge compound is an important method for reinforcing lithium ion battery security.
There are mainly of two types for Overcharge prevention electrolyte at present：Oxidation-reduction type and voltolisation mould assembly.Oxidation-reduction type such as benzene first
Ether and its derivative can be repeated as many times its main feature is that it is reversible to overcharge protection mechanism and overcharge protection, but methyl phenyl ethers anisole class oxygen
Electrochemical potential is lower, is beginning to that redox reaction occurs lower than lithium ion normal working voltage (4.2V), is being not suitable for certain
It is used in high-voltage lithium ion batteries.And voltolisation mould assembly is mainly simple cyclohexylbenzene, dimethylbenzene, biphenyl compound chemical combination
Object, this kind of compound can occur polymerization reaction when battery is more than certain voltage, be capped electrode surface to increase battery
Internal resistance clamps down on charging current to protect battery.But this kind of compound, is easy burning, and the protective film formed when overcharging is not enough
Speed is slower, inadequate to battery protection, and influences the cycle performance of battery.
Patent document CN107946648A is disclosed adds 1,1 '-biphenyl additive, additive in lithium battery electrolytes
Oxygenolysis can occur prior to electrolyte when lithium battery is overcharged, separate contact of the electrolyte with electrode surface, promote peace
Full performance, but the anti-overcharge effect of this additive is unobvious, and can seriously affect the cycle performance and cryogenic property of battery.
Summary of the invention
It is an object of the invention to：A kind of anti-overcharge lithium battery electrolytes are provided, the Overcharge prevention electrolyte can be in electricity
More the efficient point chemistry polymer for forming fine and close crosslinking net is covered in pole piece rapidly when pond overcharges, more preferably
Battery is protected on ground, does not smolder, is not on fire, not exploding, hence it is evident that improving the security performance of battery, and do not influence the cycle performance of battery
And cryogenic property.
To achieve the above object, the present invention provides the following technical solutions：
A kind of anti-overcharge lithium-ion battery electrolytes containing silicone additives, it is characterised in that：The electrolyte includes
Lithium salts, double solvents and additive A, the additive A are a kind of organosilicon derivates, have special molecular structure, knot
Structure general formula is as follows：
It is using silicon oxygen bond as main chain, containing there are four biphenyl class formation in the main structure of molecule, wherein n1For in 1-100
Natural number.Additive A forms the electrochemical polymer of crosslinking when overcharging, and can preferably protect battery.
Wherein n2、n3、n4、n5Natural number independent in 2-5.
n2、n3、n4、n5It may be the same or different.
R1, R2, R3, R4 are independent in methyl, ethyl, n-propyl, isopropyl, methoxyl group, ethyoxyl, phenyl
It is a kind of.
R1, R2, R3, R4 can be identical group, can also be respectively different groups.
R5, R6, R7, R8 independent are fluorine, chlorine, bromine, cyano, carboxyl, trifluoroacetyl group, carboxyl, carboxylic acid lithium salt, sulphur
One of acidic group, sulfonic acid lithium salts.
R5, R6, R7, R8 can be identical group, can also be respectively different groups.
It is preferred that its additional amount is the 0.5%-10% of the lithium-ion battery electrolytes gross mass.
The lithium salts is at least one of inorganic lithium salt, organic boronic lithium, lithium salts of sulfonimide；The double solvents
For in carbonate-based solvent such as ethylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate or polycarbonate at least
Two kinds of solvents.
The present invention further provides a kind of lithium batteries, use electrolyte as described above.Electrolyte of the invention is suitable
For conventional lithium-ion battery and power lithium-ion battery.
Compared with prior art, the beneficial effects of the invention are as follows：
1, the present invention is by being added anti-overcharge additive, and further changes to existing anti-overcharge additive
Property, in conjunction with some characteristics of organosilicon, a kind of Overcharge prevention electrolyte for containing silicone additives (additive A) has been invented, by
Contain multiple biphenyl class groups in the additive molecule structure, more can efficiently form densification rapidly when overcharging
The electrochemical polymer of crosslinking net, more common monomer biphenyl compound can form finer and close electrochemical polymer covering
In pole piece, in this way to the more abundant of battery protection, to have better anti-overcharge ability, safety is higher.
2, since organosilicon compound has excellent thermal stability, low combustible, low volatility, low viscosity, temperature viscous
The advantages that coefficient is small, surface tension is small, migration is good, high-low temperature resistant, high de-agglomeration voltage, so the more general anti-mistake when overcharging
It is more nonflammable to fill electrolyte, is not easily decomposed more resistant to high voltage.
3, since organosilicon compound viscosity is low, and the viscous coefficient of temperature is small, when additive A is added, will not influence electrolyte
Cryogenic property and cycle performance.
Specific embodiment
In order to be more clear goal of the invention of the invention, technical solution and advantageous effects, with reference to embodiments,
The present invention will be described in further detail.It should be understood that embodiment described in this specification is just for the sake of explanation
The present invention, be not intended to limit the present invention, formula, ratio of embodiment etc. can adaptation to local conditions make a choice and reality had no to result
Matter influences.
Below with the n2=n3=n4=n5=2 in additive A general formula, R1, R2, R3, R4=CH3, R5, R6, R7, R8=
For Cl, the present invention will be described in further detail.
The synthetic method of additive A is as follows：
1, the synthesis of dimethyl four (3 '-chlorine) xenyl disiloxane
By (3 '-chlorine) the xenyl Ethoxysilane of 450g methyl two and 450mL LiOH aqueous solution (about 5% mass fraction)
It is sequentially added into reaction kettle, 100 DEG C is to slowly warm up in 1h, then insulation reaction 15-20h, when distillate refractive index is close
1.333 when, reaction was completed.Cooled to room temperature, filtering, is repeatedly washed to neutrality, then filter, finally by gains in 95 DEG C
It is dried in vacuo 10h, obtains dimethyl four (3 '-chlorine) xenyl disiloxane.Reaction equation is as follows：
2, the A synthesis of compound
By (3 '-chlorine) the xenyl disiloxane of 96g dimethyl four and 228g octamethylcy-clotetrasiloxane and the dense sulphur of 7.3g
Acid is added in reaction kettle, fills N2It protects, polymerization reaction 12h at 60-65 DEG C is cooled to room temperature, is washed till with saturated sodium carbonate solution
Neutrality then collects oily phase again with deionization washing twice, after water-oil separating, and then vacuum distillation goes in oil removing phase to remain moisture content
Obtain compound A.Reaction equation is as follows：
Embodiment 1：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Methyl ethyl carbonate rouge：Carbonic acid
Vinyl acetate：Propene carbonate=1:2:2:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned mixed liquor, and six
Lithium fluophosphate substance withdrawl syndrome is 1.0mol/L；The above compound A that mass percentage is 2% is finally added again and is used as adds
Agent is added to obtain required electrolyte.
Embodiment 2：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Methyl ethyl carbonate rouge：Carbonic acid
Vinyl acetate：Propene carbonate=1:2:3:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned mixed liquor, and six
Lithium fluophosphate substance withdrawl syndrome is 1.0mol/L；The above compound A that mass percentage is 2% is finally added again and is used as adds
Agent is added to obtain required electrolyte.
Embodiment 3：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Carbonic acid diethyl ester：Carbonic acid
Vinyl acetate：Propene carbonate=1:2:2:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned mixed liquor, and six
Lithium fluophosphate substance withdrawl syndrome is 1.1mol/L；The above compound A that mass percentage is 2% is finally added again and is used as adds
Agent is added to obtain required electrolyte.
Embodiment 4：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Carbonic acid diethyl ester：Carbonic acid
Vinyl acetate：Propene carbonate=1:2:3:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned mixed liquor, and six
Lithium fluophosphate substance withdrawl syndrome is 1.1mol/L；The above compound A that mass percentage is 2% is finally added again and is used as adds
Agent is added to obtain required electrolyte.
Embodiment 5：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Methyl ethyl carbonate rouge：Carbonic acid
Vinyl acetate：Propene carbonate：Methyl formate=1:2:2:2:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned
In mixed liquor, lithium hexafluoro phosphate substance withdrawl syndrome is 1.2mol/L；Above-mentionedization that mass percentage is 3% is finally added again
Object A is closed as additive and obtains required electrolyte.
Comparative example 1：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Methyl ethyl carbonate rouge：Carbonic acid
Vinyl acetate：Propene carbonate=1:2:2:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned mixed liquor, and six
Lithium fluophosphate substance withdrawl syndrome is 1.0mol/L, electrolyte needed for obtaining comparative example 1.
Comparative example 2：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Methyl ethyl carbonate rouge：Carbonic acid
Vinyl acetate：Propene carbonate=1:2:3:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned mixed liquor, and six
Lithium fluophosphate substance withdrawl syndrome is 1.0mol/L, finally adds 1, the 1 '-biphenyl that mass percentage is 2% again and is used as addition
Agent obtains electrolyte needed for required electrolyte obtains comparative example 2.
Comparative example 3：
(the H2O in the glove box full of argon gas<15ppm), using mass ratio as dimethyl carbonate：Methyl ethyl carbonate rouge：Carbonic acid
Vinyl acetate：Propene carbonate：Methyl formate=1:2:2:2:1 is uniformly mixed, and then dissolves lithium hexafluoro phosphate (LiPF6) in above-mentioned
In mixed liquor, lithium hexafluoro phosphate substance withdrawl syndrome is 1.2mol/L, finally adds 1,1 '-that mass percentage is 3% again
Biphenyl obtains electrolyte needed for required electrolyte obtains comparative example 3 as additive.
Test data of experiment project：
1, all embodiment and comparative examples are matched to the electrolyte injection postponed with batch in the power battery of model, are tested
Battery normal temperature environment at 3-4.2V carries out the cycle performance of 1C charging and discharging.
2, all embodiment and comparative examples are matched to the electrolyte injection postponed with batch in the power battery of model, are tested
Battery low temperature performance at -20 DEG C.
3, all embodiment and comparative examples are matched to the electrolyte injection postponed with batch in the power battery of model, are tested
Anti-overcharge performance of the battery under 10V charging voltage.
Test data such as the following table 1：
From the electrolyte of embodiment and comparative example in table in the battery equally with batch test effect：Common
It does not generate adverse effect to battery room temperature 1C cycle performance after additive A is added in electrolyte, and commonly anti-overcharge adds
The addition of agent (such as 1,1 '-biphenyl) is added but to lead to the decline of battery core cycle performance；Likewise, since organo-silicon compound are with low
Viscosity, temperature be viscous, and coefficient is small, surface tension is small, migration is good, high-low temperature resistant, the advantages of, so the electrolyte containing additive A,
There is better cryogenic property；It is prior due to organosilicon compound have excellent thermal stability, low combustible, low volatilization
Degree, high de-agglomeration voltage the advantages that, the electrolyte containing additive A when charging voltage reaches 10V still non-flatulence, do not explode,
With excellent anti-overcharge performance, and general electrolytic liquid has occurred and that flatulence is exploded, and is added to 1 when charging voltage does not arrive 10V,
Although the electrolyte of 1 '-biphenyl does not explode at additional amount larger (mass fraction for being added 3%), battery is had occurred sternly
The flatulence of weight, when additional amount is less (be added 2% mass fraction) an explosion occurred, anti-overcharge ability is poor.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
It makes a variety of changes.
Claims (10)
1. a kind of anti-overcharge lithium-ion battery electrolytes containing silicone additives, it is characterised in that：The electrolyte includes lithium
Salt, double solvents and additive A, the additive A are a kind of organosilicon derivates, and general structure is as follows：
It is using silicon oxygen bond as main chain, containing there are four biphenyl class formations in the main structure of molecule.
2. the anti-overcharge lithium-ion battery electrolytes according to claim 1 containing silicone additives, which is characterized in that its
In, n1For the natural number in 1-100, n2、n3、n4、n5Natural number independent in 2-5.
3. the anti-overcharge lithium-ion battery electrolytes according to claim 1 containing silicone additives, which is characterized in that
R1, R2, R3, R4 independent are one of methyl, ethyl, n-propyl, isopropyl, methoxyl group, ethyoxyl, phenyl.
4. the anti-overcharge lithium-ion battery electrolytes according to claim 1 containing silicone additives, which is characterized in that
R5, R6, R7, R8 independent are fluorine, chlorine, bromine, cyano, carboxyl, trifluoroacetyl group, carboxyl, carboxylic acid lithium salt, sulfonic group, sulphur
One of sour lithium salts.
5. the anti-overcharge lithium-ion battery electrolytes according to claim 1 containing silicone additives, which is characterized in that add
Add the additional amount of agent A for the 0.5%-10% of the lithium-ion battery electrolytes gross mass.
6. the anti-overcharge lithium-ion battery electrolytes according to claim 1 containing silicone additives, which is characterized in that institute
Stating lithium salts is at least one of inorganic lithium salt, organic boronic lithium, lithium salts of sulfonimide.
7. the anti-overcharge lithium-ion battery electrolytes according to claim 1 containing silicone additives, which is characterized in that institute
Stating double solvents is carbonate-based solvent such as ethylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate or poly- carbonic acid
At least two solvents in ester.
8. a kind of lithium battery, which is characterized in that use the described in any item electrolyte of claim 1-7.
9. a kind of compound A, which is characterized in that the compound A is a kind of organosilicon derivates, and general structure is：
Wherein n1For the natural number in 1-100, n2、n3、n4、n5Natural number independent in 2-5, R1, R2, R3, R4 are each
From being independently one of methyl, ethyl, n-propyl, isopropyl, methoxyl group, ethyoxyl, phenyl, R5, R6, R7, R8 are respectively
It is independently one of fluorine, chlorine, bromine, cyano, carboxyl, trifluoroacetyl group, carboxyl, carboxylic acid lithium salt, sulfonic group, sulfonic acid lithium salts.
10. the purposes that a kind of compound as claimed in claim 9 is used for lithium-ion battery electrolytes.
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| CN1267304A (en) * | 1997-07-14 | 2000-09-20 | 心脏临床研究中心有限公司 | Silicon-contg. chain extenders |
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