CN109461968A - A kind of flame retardant type calcium ion battery electrolyte and its preparation method and application - Google Patents
A kind of flame retardant type calcium ion battery electrolyte and its preparation method and application Download PDFInfo
- Publication number
- CN109461968A CN109461968A CN201811318289.6A CN201811318289A CN109461968A CN 109461968 A CN109461968 A CN 109461968A CN 201811318289 A CN201811318289 A CN 201811318289A CN 109461968 A CN109461968 A CN 109461968A
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- Prior art keywords
- ion battery
- calcium ion
- flame retardant
- electrolyte
- flame
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Classifications
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
-
- 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
-
- 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 present invention provides flame retardant type calcium ion battery electrolytes and its preparation method and application.The electrolyte is composed of the following components: electrolytic salt, organic solvent, flame-retardant additive, functional additive.The preparation method of the flame retardant type calcium ion battery electrolyte obtains mixed liquor the following steps are included: (1) is dissolved after removing water fire retardant in organic solvent, and then functional additive is added in above-mentioned mixed liquor, obtains solution A；(2) calcium salt is added in the solution A in step (1) in the environment of anhydrous and oxygen-free, is made into electrolyte to get flame retardant type calcium ion battery electrolytic solution for super capacitor of the present invention.Electrolyte prepared by the present invention has low toxicity, low viscosity and wider electrochemical window and temperature range, while having efficient flame retardant effect, increases substantially the security performance of lithium battery, therefore has good industrial applications prospect.
Description
Technical field
The invention belongs to chemical cell technical fields, and in particular to a kind of flame retardant type calcium ion battery electrolyte and its preparation
Methods and applications.
Background technique
In alkali earth metal, calcium has the low, standard electrode EMF of polarization and lithium close to (Ca2+/ Ca:-2.868V
It is vs.SHE, only 170mV higher than lithium), ion be+divalent (electrically charged number be lithium ion twice), rich reserves, cost is relatively low
The advantages of, therefore, calcium ion battery has the potentiality as high efficiency, low cost energy-storage battery.
However, the safety problem of calcium ion battery is the matter of utmost importance that we are concerned about.The electricity used due to calcium ion battery
Solution liquid is inflammable organic electrolyte system, when overcharge, short circuit or under the conditions ofs heated etc., on fire, combustion may occur for battery
It burns or explodes, and then cause safety accident.
It is most of although flame-retardant additive in the prior art can reduce the combustibility of electrolyte to a certain extent
Flame-retardant additive has biggish negative effect to calcium ion battery performance, and to sum up, calcium ion battery commonly used at present is being pacified
Many hidden danger are still had in all directions, easily cause safety accident, therefore, need to develop a kind of flame retardant type calcium ion battery electrolysis
Liquid.
Summary of the invention
In view of the above shortcomings of the prior art, the purpose of the present invention is to provide a kind of flame retardant type calcium ion battery electrolytes
And its preparation method and application, flame-retardant additive of the invention can be under the premise of guaranteeing excellent flame effect, not only to calcium
The chemical property of ion battery has no adverse effect, and the cyclical stability and battery capacity that battery can be improved instead are kept
Rate, therefore there is good industrial applications prospect.
An object of the present invention is to provide a kind of flame retardant type calcium ion battery electrolyte.
The second object of the present invention is to provide the preparation method of above-mentioned flame retardant type calcium ion battery electrolyte.
The third object of the present invention is to provide the application of above-mentioned flame retardant type battery electrolyte.
To achieve the above object, the present invention relates to following technical schemes:
The first aspect of the invention provides a kind of calcium ion battery electrolyte, and the electrolyte is composed of the following components:
Electrolytic salt, organic solvent, flame-retardant additive, functional additive.
The general structure of the fire retardant are as follows:
Wherein, R1-R6It all can be alkyl, halogenated alkyl, halogenated alkoxy, halogenated biphenyl, alkoxy, alkyl silicon, halogenated
Alkylene, xenyl, phenyl, halogenophenyl, alkyl phosphate, alkoxyl silicone, boron alkoxide or amide groups, in which: halogenated to be
Part replaces or full substitution.
The content of the electrolytic salt is 0.001~5mol/L.
The content of the organic solvent are as follows: 0.1%~50% (mass fraction).
The flame retardant agent content are as follows: 0.1%~50% (mass fraction).
The functional additive content are as follows: 0.1~0.5mol/L.
The halogen of substituent group is F in the general structure of the flame-retardant additive.
Preferably, the flame-retardant additive are as follows: five fluorine ring triphosphine nitrile of ethyoxyl, five fluorine ring triphosphine nitrile of phenoxy group, siloxy
Five fluorine ring triphosphine nitriles, siloxy ptfe ring triphosphine nitrile (disubstituted), phenoxy group ptfe ring triphosphine nitrile (disubstituted), trifluoro propyl first
The mixture of one or more of basic ring trisiloxanes, hexaphenoxycyclotriphosphazene.
The electrolytic salt is hexafluorophosphoric acid calcium, hexafluoroarsenate calcium, Calcium perchlorate, tetrafluoro boric acid calcium, calcium methanesulfonate, three
The mixture of one or more of methyl fluoride sulfoacid calcium, bis trifluoromethyl sulfimide calcium.
The organic solvent be acetonitrile, propionitrile, ethylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate,
The mixture of one or more of gamma-butyrolacton, propene carbonate, dimethyl carbonate.
The functional additive is biphenyl (BP), vinylethylene carbonate (VEC), vinylene carbonate (VC), fluoro carbon
Vinyl acetate (FEC), 1,4- butyl sultone (BS), 1,3-N-morpholinopropanesulfonic acid lactone (PS), ethylene sulfite (ESI), 1,3- (1-
Propylene) sultone (PST), sulfuric acid vinyl ester (ESA), tert-butyl benzene (TBB), tert-amyl benzene (TPB), cyclohexyl benzene (CHB) or
The mixture of one or more of fourth dicyan (SN).
The effect of functional additive is: (1) promoting the formation of SEI film；(2) protection anode and negative electrode material；(3) conduct
LiPF6Stabilizer；(4) as the protective agent of overshoot voltage；(5) increase the conductivity of electrolyte；(6) the low of electrolyte is improved
Warm nature energy；(7) thermal stability of electrolyte is improved；(8) combustibility of electrolyte is reduced.
The second aspect of the invention discloses the preparation method of above-mentioned flame retardant type calcium ion battery electrolyte, specific to wrap
Include following steps:
(1) it is dissolved after removing water fire retardant and obtains mixed liquor in organic solvent, then functional additive is added above-mentioned mixed
It closes in liquid, obtains solution A；
(2) calcium salt is added in the solution A in step (1) in the environment of anhydrous and oxygen-free, is made into electrolyte to get this hair
The bright flame retardant type calcium ion battery electrolyte.
Wherein, in step (1), the water removal refers to: screening out water 36-96h with 4A sodium molecule.
In step (2), the calcium salt should be slowly added into solution A, prevent solution A overheat from solvent being made to boil.
The third aspect of the invention, provides the application of above-mentioned flame retardant type calcium ion battery electrolyte, and the application includes
Application of the flame retardant type calcium ion battery electrolyte in calcium ion battery, electric vehicle, electric car.
Compared with prior art, a kind of flame retardant type calcium ion battery electrolyte disclosed by the invention achieves following beneficial to effect
Fruit:
(1) fire retardant containing phosphazenium groups compound has good flame retardant property, and to Electrochemical Performances
Very little improves its chemical property sometimes, therefore can be used as novel electrolyte flame-retardant additive；
(2) by adding flame-retardant additive in electrolyte solution, the flammable performance of electrolyte can be reduced.It will be of the invention
After electrolyte is applied to calcium ion battery, the burning possibility of electrolyte can be reduced to zero, improve the safety of calcium ion battery
Property.
(3) this electrolyte has low toxicity, low viscosity and wider electrochemical window and temperature range, while having efficiently
Flame retardant effect；Not only there is good chemical property using the calcium ion of this electrolyte, and security performance can be substantially
It improves, there is wider array of application market.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the electrolyte flame-retardant performance map of the fire retardant prepared containing embodiment 1.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As previously mentioned, although flame-retardant additive in the prior art can reduce the flammable of electrolyte to a certain extent
Property, but most of flame-retardant additives have biggish negative effect to calcium ion battery performance.
In view of this, providing a kind of calcium ion battery electrolyte, the electrolysis in a kind of specific embodiment of the invention
Liquid is composed of the following components: electrolytic salt, organic solvent, flame-retardant additive, functional additive.
The general structure of the fire retardant are as follows:
In still another embodiment of the invention, R1-R6It all can be alkyl, halogenated alkyl, halogenated alkoxy, halogenated
Biphenyl, alkoxy, alkyl silicon, haloalkene alkyl, xenyl, phenyl, halogenophenyl, alkyl phosphate, alkoxyl silicone, alkoxy
Boron or amide groups, in which: halogenated to replace for part or replace entirely.
In still another embodiment of the invention, the content of the electrolytic salt is 0.001~5mol/L.
In still another embodiment of the invention, the content of the organic solvent are as follows: 0.1%~50% (mass fraction)
In still another embodiment of the invention, the flame retardant agent content are as follows: 0.1%~50% (mass fraction).
In still another embodiment of the invention, the functional additive content are as follows: 0.1~0.5mol/L.
In still another embodiment of the invention, the halogen of substituent group is F in the general structure of the flame-retardant additive.
In still another embodiment of the invention, the flame-retardant additive are as follows: five fluorine ring triphosphine nitrile of ethyoxyl, phenoxy group
Five fluorine ring triphosphine nitriles, five fluorine ring triphosphine nitrile of siloxy, siloxy ptfe ring triphosphine nitrile (disubstituted), phenoxy group ptfe ring triphosphine nitrile
The mixture of one or more of (disubstituted), trifluoro propyl methyl cyclotrisiloxane, hexaphenoxycyclotriphosphazene.
In still another embodiment of the invention, the electrolytic salt is hexafluorophosphoric acid calcium, hexafluoroarsenate calcium, perchloric acid
One or both of calcium, tetrafluoro boric acid calcium, calcium methanesulfonate, trifluoromethane sulfonic acid calcium, bis trifluoromethyl sulfimide calcium with
On mixture.
In still another embodiment of the invention, the organic solvent is acetonitrile, propionitrile, ethylene carbonate, carbonic acid two
One or more of methyl esters, diethyl carbonate, methyl ethyl carbonate, gamma-butyrolacton, propene carbonate, dimethyl carbonate
Mixture.
In still another embodiment of the invention, the functional additive is biphenyl (BP), vinylethylene carbonate
(VEC), vinylene carbonate (VC), fluorinated ethylene carbonate (FEC), 1,4- butyl sultone (BS), 1,3-N-morpholinopropanesulfonic acid lactone
(PS), ethylene sulfite (ESI), 1,3- (1- propylene) sultone (PST), sulfuric acid vinyl ester (ESA), tert-butyl benzene (TBB),
The mixture of one or more of tert-amyl benzene (TPB), cyclohexyl benzene (CHB) or fourth dicyan (SN).
In still another embodiment of the invention, the preparation side of above-mentioned flame retardant type calcium ion battery electrolyte is disclosed
Method, specifically includes the following steps:
(1) it is dissolved after removing water fire retardant and obtains mixed liquor in organic solvent, then functional additive is added above-mentioned mixed
It closes in liquid, obtains solution A；
(2) calcium salt is added in the solution A in step (1) in the environment of anhydrous and oxygen-free, is made into electrolyte to get this hair
The bright flame retardant type calcium ion battery electrolyte.
In still another embodiment of the invention, in step (1), the water removal refers to: screening out water 36- with 4A sodium molecule
96h。
In step (2), the calcium salt should be slowly added into solution A, prevent solution A overheat from solvent being made to boil.
In still another embodiment of the invention, the application of above-mentioned flame retardant type calcium ion battery electrolyte is provided, it is described
Using the application including flame retardant type calcium ion battery electrolyte in calcium ion battery, electric vehicle, electric car.
Explanation is further explained to the present invention by the following examples, but is not construed as limiting the invention.It should be understood that
These examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.Actual conditions are not specified in the following example
Test method, carry out usually according to normal condition.
Embodiment 1
The preparation of five fluorine ring of ethyoxyl, three phosphonitrile: three phosphonitrile of ethyoxyl pentachloro- ring is stirred continuously down and adds in 100g acetonitrile
Enter 50g NaF, under the conditions of 70 DEG C of temperature, after carrying out 4 hours fluorination reactions, distillation obtains five fluorine ring of ethyoxyl, three phosphonitrile.
Above-mentioned five fluorine ring of ethyoxyl, three phosphonitrile is prepared into electrolyte, tests its flame retardant property, as a result as shown in Figure 1.
Embodiment 2
The preparation process of five fluorine ring of silicon, three phosphonitrile: it by three phosphonitrile of 15g siloxy pentachloro- ring in 180ml chlorobenzene, constantly stirs
Lower addition catalyst iron chloride, 3.2 grams of sodium ethoxides are mixed, under the conditions of 80 DEG C of temperature, 5h is reacted, is evaporated under reduced pressure, after purification
Obtain phosphazene derivative: five fluorine ring of siloxy, three phosphonitrile.
Embodiment 3
The preparation process of hexaphenoxycyclotriphosphazene: by 20g hexachlorocyclotriph,sphazene crystal, hexane be placed in blender,
Thermometer returns in the 500ml three-necked bottle for evaporating condenser pipe, stirs to being uniformly dissolved, reacts under the conditions of 80 DEG C of temperature with 30g sodium phenate
It 10 hours, is distilled, is refining to obtain phosphazene derivative: hexaphenoxycyclotriphosphazene.
Embodiment 4
Triacetyl butanol-three phosphonitrile of triethoxy ring preparation process: by 40g hexachlorocyclotriph,sphazene crystal, hexane is placed in
With blender, thermometer, return and evaporate in the 500ml three-necked bottle of condenser pipe, stirring to being uniformly dissolved, under the conditions of 70 DEG C of temperature with
200g acetobutyl alcohol sodium reacts 10 hours, then reacts 5 hours, is distilled in 200ml ethane with 40g sodium ethoxide, refines
Obtain phosphazene derivative: triacetyl butanol-three phosphonitrile of triethoxy ring.
Embodiment 5
The preparation method of flame retardant type calcium ion battery electrolyte, specifically includes the following steps:
(1) it is dissolved after removing water fire retardant and obtains mixed liquor in organic solvent, then functional additive is added above-mentioned
In mixed liquor, solution A is obtained；
(2) calcium salt is added in the solution A in step (1) in the environment of anhydrous and oxygen-free, is made into electrolyte to get this hair
The electrolyte of the bright flame retardant type calcium ion battery.
In step (1), the water removal refers to: screening out water 36-96h with 4A sodium molecule.
In step (2), the calcium salt should be slowly added into solution A, prevent solution A overheat from solvent being made to boil.
It can be obtained by Fig. 1, five fluorine ring of ethyoxyl base, three phosphonitrile flame-retardant additive is added in the electrolyte in the present invention, can significantly mention
The flame retardant property of high electrolyte, 5% five fluorine ring of ethyoxyl, three phosphonitrile flame-retardant additive can achieve complete non-flammable effect
(self-extinguishing time 0s), the mass fraction of flame-retardant additive in the prior art in the electrolytic solution commonly reach 10~40% ability
With preferable non-flammable effect, but the viscosity of electrolyte that the flame-retardant additive of better quality score can make increases, shadow
The electric conductivity of electrolyte is rung, and then influences the performance of calcium ion battery.
Flame-retardant additive in the prior art can reduce the combustibility of electrolyte, but most of flame-retardant additives are to calcium
Ion battery performance has a biggish negative effect, a small number of flame-retardant additives can also make the battery performance of calcium ion battery under
Drop.And after the flame-retardant additive in the application is added, under the premise of guaranteeing excellent flame effect, a small amount of fire-retardant addition is added
Agent, not only has no adverse effect the chemical property of calcium ion battery, can be improved instead battery cyclical stability and
Battery capacity conservation rate can be used as safety additives and apply in actual battery, this is the super of routine in the prior art
The inaccessiable technical effect of capacitor electrolyte flame-retardant additive institute.When the content of flame-retardant additive is higher, electricity will affect
Solve the electric conductivity of liquid and the cyclical stability and battery capacity conservation rate of battery.
It should be noted that above example is only used to illustrate the technical scheme of the present invention rather than is limited.Although ginseng
It is described the invention in detail according to given example, but those skilled in the art can be as needed to this hair
Bright technical solution is modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. a kind of flame retardant type calcium ion battery electrolyte, which is characterized in that the electrolyte is composed of the following components: electrolyte
Salt, organic solvent, flame-retardant additive, functional additive；
The general structure of the fire retardant are as follows:
Wherein, R1-R6It all can be alkyl, halogenated alkyl, halogenated alkoxy, halogenated biphenyl, alkoxy, alkyl silicon, alkenyl halide
Base, xenyl, phenyl, halogenophenyl, alkyl phosphate, alkoxyl silicone, boron alkoxide or amide groups, in which: halogenated is part
Replace or replaces entirely.
2. a kind of flame retardant type calcium ion battery electrolyte as described in claim 1, which is characterized in that
The content of the electrolytic salt is 0.001~5mol/L；
The content of the organic solvent are as follows: 0.1%~50% (mass fraction)；
The flame retardant agent content are as follows: 0.1%~50% (mass fraction)；
The functional additive content are as follows: 0.1~0.5mol/L；
The halogen of substituent group is F in the general structure of the flame-retardant additive.
3. a kind of flame retardant type calcium ion battery electrolyte as described in claim 1, which is characterized in that the flame-retardant additive
Are as follows: five fluorine ring triphosphine nitrile of ethyoxyl, five fluorine ring triphosphine nitrile of phenoxy group, five fluorine ring triphosphine nitrile of siloxy, siloxy ptfe ring triphosphine
Nitrile (disubstituted), phenoxy group ptfe ring triphosphine nitrile (disubstituted), trifluoro propyl methyl cyclotrisiloxane, hexaphenoxycyclotriphosphazene
One or more of mixture.
4. a kind of flame retardant type calcium ion battery electrolyte as described in claim 1, which is characterized in that the electrolytic salt is six
Fluorapatite, hexafluoroarsenate calcium, Calcium perchlorate, tetrafluoro boric acid calcium, calcium methanesulfonate, trifluoromethane sulfonic acid calcium, bis trifluoromethyl
The mixture of one or more of sulfimide calcium.
5. a kind of flame retardant type calcium ion battery electrolyte as described in claim 1, which is characterized in that the organic solvent is second
Nitrile, propionitrile, ethylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, gamma-butyrolacton, propene carbonate, carbonic acid
The mixture of one or more of dimethyl ester.
6. a kind of flame retardant type calcium ion battery electrolyte as described in claim 1, which is characterized in that the functional additive is
Biphenyl (BP), vinylethylene carbonate (VEC), vinylene carbonate (VC), fluorinated ethylene carbonate (FEC), 1,4- fourth sulfonic acid
Lactone (BS), 1,3-N-morpholinopropanesulfonic acid lactone (PS), ethylene sulfite (ESI), 1,3- (1- propylene) sultone (PST), sulfuric acid second
One of enester (ESA), tert-butyl benzene (TBB), tert-amyl benzene (TPB), cyclohexyl benzene (CHB) or fourth dicyan (SN) or two
Kind or more mixture.
7. the preparation method of any one of the claim 1-6 anti-flammability calcium ion battery electrolyte, specifically includes the following steps:
(1) it is dissolved after removing water fire retardant and obtains mixed liquor in organic solvent, then above-mentioned mixed liquor is added in functional additive
In, obtain solution A；
(2) calcium salt is added in the solution A in step (1) in the environment of anhydrous and oxygen-free, is made into electrolyte to get institute of the present invention
The flame retardant type calcium ion battery electrolyte stated.
8. preparation method as claimed in claim 7, which is characterized in that in step (1), the water removal refers to: being sieved with 4A sodium molecule
Remove water 36-96h.
9. preparation method as claimed in claim 7, which is characterized in that in step (2), the calcium salt is slowly added into solution A.
10. any one of the claim 1-6 flame retardant type calcium ion battery electrolyte is in calcium ion battery, electric vehicle, electronic vapour
Application in vehicle.
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| CN201811318289.6A CN109461968A (en) | 2018-11-07 | 2018-11-07 | A kind of flame retardant type calcium ion battery electrolyte and its preparation method and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113851715A (en) * | 2021-09-23 | 2021-12-28 | 山东大学深圳研究院 | High-safety electrolyte for phosphazene-based lithium battery and preparation method and application thereof |
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Application publication date: 20190312 |