CN109786837A - A kind of anti-overcharge lithium battery electrolytes and preparation method thereof - Google Patents
A kind of anti-overcharge lithium battery electrolytes and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of anti-overcharge lithium battery electrolytes and preparation method thereof, and the electrolyte is made of electrolyte lithium salt, non-aqueous organic solvent, anti-overcharge additive, functional additive, fire retardant；The quality of the anti-overcharge additive is the 0.5-7% of electrolyte gross mass, is at least made of one of aromatic compound with formula (I) structure and one of connection benzene and its derivative；
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of anti-overcharge lithium battery electrolytes and its preparation side
Method.
Background technique
As the charging voltage > 4.3V of lithium ion battery, over-charging of battery phenomenon will be caused, since cell voltage is with pole
To change and increase and rise rapidly, the overloading problem of positive and negative electrode will necessarily be caused, irreversible change occurs for positive electrode active materials, and
Rapid oxidation decomposes the organic solvent in electrolyte, and then makes aggregation bulk gas and heat in battery, cause inner pressure of battery and
Temperature abruptly increase drops lithium battery security performance in addition, lithium metal can be deposited on negative electrode material surface when overcharging to a certain extent
It is low, cause the diffusion of heat large area, the problems such as internal short-circuit of battery, increases battery spontaneous combustion, risk of explosion.
The prior art mainly improves overcharge safety by the way that anti-overcharge additive is added in lithium battery electrolytes, reduces electricity
Thermal runaway problem of the pond under overcharge conditions, but existing anti-overcharge additive is limited primarily to redox shuttle additives, electropolymerization
Additive occurs for additive and gas, as the halide, Metallocenic compound (Ferrocene and its derivative), polypyridine of lithium are complexed
Object (phenanthroline and biphenyl complex compound and its derivative of such as Fe, Ru, Ir and Ce), thianthrene, anisole, biphenyl and its derivative
Object, hexamethylene benzene and its derivative, 3- chlorothiophene etc., when blocking over-charging of battery happens is that irreversible decomposition reaction or voltolisation
Reaction is closed, cyclical stability is poor, and with the increase of over-charging of battery number, the performance of additive is constantly reduced, and also easily causes battery
Internal resistance increases problem.Such as application No. is the patents of CN201710015032.2, disclose a kind of ternary battery Overcharge prevention electrolyte
And preparation method thereof, using biphenyl and/or cyclohexylbenzene as anti-overcharge additive, utilize the voltolisation of biphenyl and cyclohexylbenzene
It closes reaction and blocks over-charging of battery, but the cyclical stability of additive itself is not good enough；As application No. is CN201810577367.8
Patent discloses a kind of anti-overcharge lithium battery electrolytes and lithium battery, lithium battery preparation method, using benzene derivate as anti-overcharge
Additive, the equally problem there is also cyclical stability difference.
Therefore, the present invention propose a kind of cyclical stability it is high, with the novel anti-overcharge additive for shunting pressure limiting performance, and
It is applied particularly in lithium battery electrolytes.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of anti-overcharge lithium battery electrolytes and its
Preparation method.
Technical solution of the present invention is summarized as follows:
A kind of anti-overcharge lithium battery electrolytes, the electrolyte is by electrolyte lithium salt, non-aqueous organic solvent, anti-overcharge addition
Agent, functional additive, fire retardant composition；
Wherein, the molar concentration of the electrolyte lithium salt in the electrolytic solution is 0.8-2mol/L；
The quality of the anti-overcharge additive is the 0.5-7% of electrolyte gross mass, at least by the virtue with formula (I) structure
One of fragrant compounds of group and one of connection benzene and its derivative composition；
In formula: X represents H atom, halogen atom, alkyl, alkoxy or halogenated alkyl, and R1-R10 respectively represents H atom, halogen
Plain atom, alkyl, naphthenic base, alkoxy, halogenated alkyl, alkylene or haloalkene alkyl；
The quality of the functional additive be electrolyte gross mass 0.5-3%, by 5- hydroxyl -6- methyl-1 H- indazole,
Bismaleimide, sulfuric acid vinyl ester, n-butanol, glass powder are formed by the mass ratio of 1:4:2:1:2.
Preferably, the electrolyte lithium salt includes at least difluorine oxalic acid boracic acid lithium, di-oxalate lithium borate, hexafluorophosphoric acid
One of lithium, hexafluoro methane sulfonic acid lithium, two (trimethyl fluoride sulfonyl) imine lithiums, LiBF4.
Preferably, the non-aqueous organic solvent is ethyl acetate, methyl propionate, gamma-valerolactone, δ-valerolactone, carbonic acid
Vinylene, propene carbonate, methyl ethyl carbonate, two or more in diethyl carbonate compare mixed liquor in equal volume.
Preferably, the mass ratio of the aromatic compound with formula (I) structure and connection benzene and its derivative is 1:
(0.5-2)。
Preferably, the quality of the fire retardant is the 0.1-1% of electrolyte gross mass, includes at least di(2-ethylhexyl)phosphate benzene toluene
One of ester, three phosphonitrile of hexakis-methoxy basic ring, three (2,2,2- trifluoroethyl) phosphates.
A kind of preparation method of anti-overcharge lithium battery electrolytes: 10 DEG C, each component is sequentially added poly- four according to the above ratio
It in the reaction kettle of vinyl fluoride liner, stirs evenly, filling storage.
Beneficial effects of the present invention:
(1) the anti-overcharge additive of the present invention is made of the aromatic compound of special construction with connection benzene and its derivative, and two
Person's collaboration is anti-overcharge, can effectively avoid lithium battery that spontaneous combustion and explosion issues occur, compared to simple electropolymerization additive (biphenyl and
Its derivative, hexamethylene benzene and its derivative, phenyl ring derivative, thiophene etc.), the cyclical stability of additive is significantly changed
It is kind, it lets off and fills that effect is more preferable, and lithium battery electrode resistance reduces, and electrical efficiency is higher, the aromatic compound with formula (I) structure
Any reaction does not occur at normal battery operation voltage (3.0-4.35V), it, will be in electricity as battery charging voltage >=4.5V
Redox reaction occurs for pole surface, quickly shunts pressure limiting, prevents that the decomposition reaction of electrolyte occurs because of overtension.
(2) present invention utilizes 5- hydroxyl -6- methyl-1 H- indazole and bismaleimide in functional additive can be just
Pole material surface forms excellent interface passivation film, effectively inhibits electrolyte in the oxygenolysis of electrode material surface, reduces anti-
Activity is answered, lithium battery high voltage cycle performance is promoted and high-temperature behavior, sulfuric acid vinyl ester is film for additive, cathode can be improved
The stability of SEI film, and then inhibit the interfacial reaction of negative electrode material and electrolyte, n-butanol is antifreezing agent, improves electrolyte
Low temperature flow, glass powder effectively eliminate the HF in electrolyte, free F for regulating and controlling water and HF content in electrolyte-Attachment
On electrodeless glass granules surface, have the function that permanently to be passivated, prevents corrosion of the HF to positive and negative pole material, the electrolyte of raising
Stability.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
The present invention provides the anti-overcharge lithium battery electrolytes of an embodiment, by electrolyte lithium salt, non-aqueous organic solvent, anti-mistake
Fill additive, functional additive, fire retardant composition；Preparation method: 10 DEG C, each component is sequentially added poly- four in the following proportions
It in the reaction kettle of vinyl fluoride liner, stirs evenly, filling storage；
Wherein, the molar concentration of the electrolyte lithium salt in the electrolytic solution is 0.8-2mol/L, includes at least difluoro oxalate
Lithium borate, di-oxalate lithium borate, lithium hexafluoro phosphate, hexafluoro methane sulfonic acid lithium, two (trimethyl fluoride sulfonyl) imine lithiums, tetrafluoro boric acid
One of lithium；
The quality of the anti-overcharge additive is the 0.5-7% of electrolyte gross mass, at least by the virtue with formula (I) structure
One of fragrant compounds of group and one of connection benzene and its derivative composition, and the two mass ratio is 1:(0.5-2)；
In formula: X represents H atom, halogen atom, alkyl, alkoxy or halogenated alkyl, and R1-R10 respectively represents H atom, halogen
Plain atom, alkyl, naphthenic base, alkoxy, halogenated alkyl, alkylene or haloalkene alkyl；
The quality of the functional additive be electrolyte gross mass 0.5-3%, by 5- hydroxyl -6- methyl-1 H- indazole,
Bismaleimide, sulfuric acid vinyl ester, n-butanol, glass powder are formed by the mass ratio of 1:4:2:1:2；
The non-aqueous organic solvent be ethyl acetate, methyl propionate, gamma-valerolactone, δ-valerolactone, vinylene carbonate,
Propene carbonate, methyl ethyl carbonate, two or more in diethyl carbonate compare mixed liquor in equal volume；
The quality of the fire retardant is the 0.1-1% of electrolyte gross mass, includes at least di(2-ethylhexyl)phosphate benzene toluene ester, hexakis-methoxy
One of three phosphonitrile of basic ring, three (2,2,2- trifluoroethyl) phosphates.
Embodiment 1
Anti-overcharge lithium battery electrolytes, by electrolyte lithium salt, non-aqueous organic solvent, anti-overcharge additive, functional additive,
Fire retardant composition；
Wherein, the electrolyte lithium salt is difluorine oxalic acid boracic acid lithium, and molar concentration in the electrolytic solution is 0.8mol/L；
The quality of the anti-overcharge additive is the 0.5% of electrolyte gross mass, by the aromatic series with formula (I) structure
Object and biphenyl composition are closed, and the two mass ratio is 1:0.5；
In formula: X represents F atom, and R1-R10 respectively represents a methyl fluoride；
The quality of the functional additive is the 0.5% of electrolyte gross mass, by 5- hydroxyl -6- methyl-1 H- indazole, double
Maleimide, sulfuric acid vinyl ester, n-butanol, glass powder are formed by the mass ratio of 1:4:2:1:2；
The non-aqueous organic solvent is ethyl acetate gamma-valerolactone, the isometric of vinylene carbonate compares mixed liquor；
The fire retardant is di(2-ethylhexyl)phosphate benzene toluene ester, and quality is the 0.1% of electrolyte gross mass.
Embodiment 2
Anti-overcharge lithium battery electrolytes, by electrolyte lithium salt, non-aqueous organic solvent, anti-overcharge additive, functional additive,
Fire retardant composition；
Wherein, the electrolyte lithium salt is lithium hexafluoro phosphate, and molar concentration in the electrolytic solution is 1mol/L；
The quality of the anti-overcharge additive is the 1% of electrolyte gross mass, by the aromatic compound with formula (I) structure
Object and dimethyl diphenyl composition, and the two mass ratio is 1:0.8；
In formula: X represents H atom, and R1-R10 respectively represents methyl；
The quality of the functional additive is the 1% of electrolyte gross mass, by 5- hydroxyl -6- methyl-1 H- indazole, span
Come acid imide, sulfuric acid vinyl ester, n-butanol, glass powder to form by the mass ratio of 1:4:2:1:2；
The non-aqueous organic solvent is methyl propionate, the isometric of δ-valerolactone, propene carbonate compares mixed liquor；
The fire retardant is three phosphonitrile of hexakis-methoxy basic ring, and quality is the 0.2% of electrolyte gross mass.
Embodiment 3
Anti-overcharge lithium battery electrolytes, by electrolyte lithium salt, non-aqueous organic solvent, anti-overcharge additive, functional additive,
Fire retardant composition；
Wherein, the electrolyte lithium salt be di-oxalate lithium borate and hexafluoro methane sulfonic acid lithium equimolar than salt-mixture,
Molar concentration in electrolyte is 1.5mol/L；
The quality of the anti-overcharge additive is the 2% of electrolyte gross mass, by the aromatic compound with formula (I) structure
Object and 2, the fluoro- 4'- methyl biphenyl of 3- bis- composition, and the two mass ratio is 1:1；
In formula: X represents Cl atom, and R1-R10 respectively represents difluoroethylene base；
The quality of the functional additive is the 1.8% of electrolyte gross mass, by 5- hydroxyl -6- methyl-1 H- indazole, double
Maleimide, sulfuric acid vinyl ester, n-butanol, glass powder are formed by the mass ratio of 1:4:2:1:2；
The non-aqueous organic solvent is methyl propionate, the isometric of vinylene carbonate, propene carbonate compares mixed liquor；
The fire retardant is three (2,2,2- trifluoroethyl) phosphates, and quality is the 0.3% of electrolyte gross mass.
Embodiment 4
With embodiment 3, difference is:
The molar concentration of electrolyte lithium salt in the electrolytic solution is 2mol/L；
The quality of anti-overcharge additive is the 3% of electrolyte gross mass, has the aromatic compound and 2 of formula (I) structure,
The mass ratio of the fluoro- 4'- methyl biphenyl of 3- bis- is 1:1.2；
In formula (I): X represents methyl, and R1-R5 respectively represents methoxyl group, and R6-R10 respectively represents difluoroethylene base；
The quality of the functional additive is the 2.5% of electrolyte gross mass；
The fire retardant quality is the 0.5% of electrolyte gross mass.
Embodiment 5
With embodiment 4, difference is:
The quality of anti-overcharge additive is the 5% of electrolyte gross mass, has the aromatic compound and 2 of formula (I) structure,
The mass ratio of the fluoro- 4'- methyl biphenyl of 3- bis- is 1:1.5；
In formula (I): X represents a methyl fluoride, and R1-R5 respectively represents methoxyl group, and R6-R8 respectively represents difluoroethylene base, R9-
R10 respectively represents cyclohexyl；
The quality of the functional additive is the 3% of electrolyte gross mass；
The fire retardant quality is the 0.8% of electrolyte gross mass.
Embodiment 6
With embodiment 5, difference is:
The quality of anti-overcharge additive is the 6% of electrolyte gross mass, has the aromatic compound and 2 of formula (I) structure,
The mass ratio of the fluoro- 4'- methyl biphenyl of 3- bis- is 1:1.7；
In formula (I): X represents a methyl fluoride, and R1-R5 respectively represents difluoroethylene base, and R6-R8 respectively represents methyl, R9-
R10 respectively represents cyclohexyl；
The fire retardant quality is the 1% of electrolyte gross mass.
Embodiment 7
With embodiment 6, difference is:
The quality of anti-overcharge additive is the 7% of electrolyte gross mass, has the aromatic compound and 2 of formula (I) structure,
The mass ratio of the fluoro- 4'- methyl biphenyl of 3- bis- is 1:2；
,
In formula (I): X represents Br atom, and R1-R5 respectively represents difluoroethylene base, and R6-R8 respectively represents a methyl fluoride, R9-
R10 respectively represents cyclopenta.
In formula: X represents H atom, halogen atom, alkyl, alkoxy or halogenated alkyl, and R1-R10 respectively represents H atom, halogen
Plain atom, alkyl, naphthenic base, alkoxy, halogenated alkyl, alkylene or haloalkene alkyl；
The quality of the functional additive be electrolyte gross mass 0.5-3%, by 5- hydroxyl -6- methyl-1 H- indazole,
Bismaleimide, sulfuric acid vinyl ester, n-butanol, glass powder are formed by the mass ratio of 1:4:2:1:2；
The non-aqueous organic solvent be ethyl acetate, methyl propionate, gamma-valerolactone, δ-valerolactone, vinylene carbonate,
Propene carbonate, methyl ethyl carbonate, two or more in diethyl carbonate compare mixed liquor in equal volume；
The quality of the fire retardant is the 0.1-1% of electrolyte gross mass, includes at least di(2-ethylhexyl)phosphate benzene toluene ester, hexakis-methoxy
One of three phosphonitrile of basic ring, three (2,2,2- trifluoroethyl) phosphates.
Comparative example 1
With embodiment 1, difference is: anti-overcharge additive is free of in electrolyte.
Comparative example 2
With embodiment 2, difference is: anti-overcharge additive contains only dimethyl diphenyl, without the fragrance with formula (I) structure
Compounds of group；
In formula: X represents H atom, halogen atom, alkyl, alkoxy or halogenated alkyl, and R1-R10 respectively represents H atom, halogen
Plain atom, alkyl, naphthenic base, alkoxy, halogenated alkyl, alkylene or haloalkene alkyl.
Embodiment 1-7 and comparative example 1-2 are tested for the property:
Select aluminum-shell lithium battery, in positive plate, m [Li (Ni1/3Co1/3Mn1/3)O2]: m (acetylene black): m (PVDF)=90:
5:5, artificial graphite are cathode, and PET micro-pore septum, electrolyte is the electrolyte that embodiment 1-7 and comparative example 1-2 are produced, assembling
At test lithium battery, is tested using cyclic voltammetry method in 3.0-5.4V voltage range, carried out when blanking voltage is 5V
100% overcharges experiment, carries out charge and discharge with 0.5C multiplying power, and 25 DEG C under the conditions of, utilizes conductivity measurement test electrolysis
The conductivity of liquid, test result is as follows shown in table:
As seen from the above table, the electrolyte that the present invention produces is anti-overcharge highly-safe, all can overcharge examination by the high pressure of 5V
It tests, the stability height of circulating battery.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (6)
1. a kind of anti-overcharge lithium battery electrolytes, which is characterized in that the electrolyte by electrolyte lithium salt, non-aqueous organic solvent,
Anti-overcharge additive, functional additive, fire retardant composition；
Wherein, the molar concentration of the electrolyte lithium salt in the electrolytic solution is 0.8-2mol/L；
The quality of the anti-overcharge additive is the 0.5-7% of electrolyte gross mass, at least by the aromatic series with formula (I) structure
One of compound and one of connection benzene and its derivative composition；
In formula: X represents H atom, halogen atom, alkyl, alkoxy or halogenated alkyl, and it is former that R1-R10 respectively represents H atom, halogen
Son, alkyl, naphthenic base, alkoxy, halogenated alkyl, alkylene or haloalkene alkyl；
The quality of the functional additive is the 0.5-3% of electrolyte gross mass, by 5- hydroxyl -6- methyl-1 H- indazole, span
Come acid imide, sulfuric acid vinyl ester, n-butanol, glass powder to form by the mass ratio of 1:4:2:1:2.
2. a kind of anti-overcharge lithium battery electrolytes according to claim 1, which is characterized in that the electrolyte lithium salt at least wraps
Include difluorine oxalic acid boracic acid lithium, di-oxalate lithium borate, lithium hexafluoro phosphate, hexafluoro methane sulfonic acid lithium, two (trimethyl fluoride sulfonyl) imines
One of lithium, LiBF4.
3. a kind of anti-overcharge lithium battery electrolytes according to claim 1, which is characterized in that the non-aqueous organic solvent is by second
Acetoacetic ester, methyl propionate, gamma-valerolactone, δ-valerolactone, vinylene carbonate, propene carbonate, methyl ethyl carbonate, carbonic acid two
Two or more isometric ratio in ethyl ester mixes.
4. a kind of anti-overcharge lithium battery electrolytes according to claim 1, which is characterized in that described with formula (I) structure
The mass ratio of aromatic compound and connection benzene and its derivative is 1:(0.5-2).
5. a kind of anti-overcharge antifreeze lithium battery electrolytes according to claim 1, which is characterized in that the quality of the fire retardant
For the 0.1-1% of electrolyte gross mass, di(2-ethylhexyl)phosphate benzene toluene ester, three phosphonitrile of hexakis-methoxy basic ring, three (2,2,2- trifluoros are included at least
One of ethyl) phosphate.
6. a kind of preparation method of anti-overcharge lithium battery electrolytes, it is characterised in that: 10 DEG C, successively by each component according to the above ratio
It is added in the reaction kettle of polytetrafluoroethyllining lining, stirs evenly, filling storage.
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| CN111153897A (en) * | 2020-02-16 | 2020-05-15 | 成都其其小数科技有限公司 | Overcharge-preventing additive for lithium battery electrolyte and preparation method thereof |
| WO2021128228A1 (en) * | 2019-12-27 | 2021-07-01 | 微宏动力系统（湖州）有限公司 | Electrolyte containing solid particles and lithium ion secondary battery |
| CN113851717A (en) * | 2021-10-14 | 2021-12-28 | 湖南法恩莱特新能源科技有限公司 | Electrolyte additive for lithium ion battery, electrolyte and application of electrolyte |
| WO2023279953A1 (en) * | 2021-07-09 | 2023-01-12 | 深圳新宙邦科技股份有限公司 | Non-aqueous electrolyte and battery |
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