CN107195970A - A kind of high pressure, function electrolyte and preparation method and application is filled soon - Google Patents
A kind of high pressure, function electrolyte and preparation method and application is filled soon Download PDFInfo
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- CN107195970A CN107195970A CN201710606850.XA CN201710606850A CN107195970A CN 107195970 A CN107195970 A CN 107195970A CN 201710606850 A CN201710606850 A CN 201710606850A CN 107195970 A CN107195970 A CN 107195970A
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- electrolyte
- high pressure
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
- H01M2300/004—Three solvents
-
- 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 discloses a kind of high pressure, fills function electrolyte and preparation method and application soon, belongs to technical field of lithium ion.The electrolyte is that the functional additive added in general electrolytic liquid equivalent to general electrolytic liquid quality 1%~5% is prepared；Described functional additive is benzal fluoride sulfone.The present invention functional additive benzal fluoride sulfone can as lithium-ion electrolyte high pressure, fill film for additive soon, because the additive has relatively low oxidizing potential, can be in one layer of densification of positive electrode surface formation, stable interfacial film during first charge-discharge, optimize positive electrode surface film, suppress the surface-active of electrode, so as to suppress the further contact and HF formation of electrolyte and electrode active material, oxidation Decomposition of the electrolyte bulk solvent in electrode surface is reduced.Room temperature cycles performance and high rate performance of the lithium ion battery containing the functional additive under 3~4.35V are improved, and application prospect is good.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of high pressure, fill function electrolyte and its preparation soon
Method and application.
Background technology
At present, in commercialization secondary cell, the specific energy highest of lithium ion battery, cycle performance are best, and because of its electricity
The diversity of pole material selection, has vast potential for future development as energy-storage battery.Current power lithium battery positive electrode both at home and abroad
Technology path mainly has 3 schools：LiFePO4 group, LiMn2O4 group, ternary send (nickel cobalt lithium aluminate (NCA) and nickle cobalt lithium manganate
(NCM)〕.Wherein LiFePO4 has extended cycle life as the battery charging and discharging of positive electrode, but it has the disadvantage energy density, height
There is larger gap in warm nature energy, charge/discharge rate property, and production cost is higher, and ferric phosphate lithium cell technology and application are
Run into the bottleneck of development；Cyclical stability and storage performance under lithium manganate battery energy density low and high temperature is poor, thus mangaic acid
Lithium is only capable of the positive electrode as international 1st generation power lithium battery；And multicomponent material is because dual excellent with combination property and cost
Gesture is increasingly by industry is of interest and approval, and progressively surmounting LiFePO4 and LiMn2O4 turns into the technology path of main flow, especially with
Using prominent tesla's (Tesla) electric automobile as representative, the TeslaModel S course continuation mileages that it is released are reachable within 2013
480km.From the point of view of battery energy density and electric car course continuation mileage, the ternary system of nickeliferous (Ni) is with the obvious advantage, particularly high Ni
The battery that ternary based material makes.
In ternary material, with the raising of nickel element ratio, bigger advantage is had on specific energy.Including 333,532,
622nd, 711,811 (nickel, cobalt, the ratios of manganese three) and nickel cobalt aluminium.The high nickel oxide of layer structure has height ratio capacity, relative
The advantages of low cost, inherently one of important candidate's positive electrode as lithium ion battery of future generation.
However, with the fast development and the continuous quickening of people's rhythm of life of science and technology, people are to lithium ion battery energy
It is enough fully charged within the most short time, and the long period can be used, it is proposed that more and more urgent serious hope.At present by nickelic
NCM (811) materials as electrode battery, although can realize that specific capacity is big, but its charging voltage and rate of charge all compare
It is smaller, cause the practical efficiency of its capacity not high, and the charging interval is long, far can not meet the demand of people.Other NCM
(811) charging voltage is higher, Ni4+More serious is decomposed to the catalytic electrolysis liquid of electrolyte, and the decomposition of electrolyte, the HF of generation is not
Certain corrosion can be only caused to collector, certain destruction can be also caused to electrode material, such as positive electrode pattern changes,
The pernicious reaction such as structure collapses, this phenomenon is particularly evident in the case of being charged to battery using big multiplying power.If one can be developed
Battery high pressure can be realized simultaneously, fill the electrolyte of function soon by planting, and then make NCM (811) electrical as the lithium battery of positive electrode
The excellent performance of energy, improves cycle life, meets production and daily life demand, it will simplified apparatus and process, greatlys save into
This, and reduce the gap of domestic battery production and process of industrialization.It is few by being added in conventional lithium-ion battery electrolytes
The electrolysis additive of amount is the most convenient for improving performance of lithium ion battery, most economical method.
The content of the invention
In order to overcome the shortcoming and deficiency of prior art, primary and foremost purpose of the invention is to provide a kind of high pressure, fills work(soon
Can electrolyte.The electrolyte can be obviously improved cycle performance of the material under the conditions of high pressure, high rate charge-discharge.
Another object of the present invention is to the preparation method for providing a kind of above-mentioned high pressure, filling function electrolyte soon.
It is still another object of the present invention to provide above-mentioned high pressure, application of the function electrolyte in lithium ion battery is filled soon.
The purpose of the present invention is achieved through the following technical solutions：
A kind of high pressure, function electrolyte is filled soon, the electrolyte is added in general electrolytic liquid equivalent to general electrolytic liquid
The functional additive of quality 1%~5% is prepared；Described functional additive is benzal fluoride sulfone (DPS), its structural formula
As shown in formula (1)：
Described general electrolytic liquid is made up of cyclic carbonate solvents, linear carbonate solvent and electric conducting lithium salt.
Described cyclic carbonate solvents are preferably ethylene carbonate (EC).
Described linear carbonate solvent includes dimethyl carbonate (DMC), methyl ethyl carbonate (EMC), diethyl carbonate
(DEC) and more than one or both of methyl propyl carbonate (MPC).
Described electric conducting lithium salt is selected from lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), dioxalic acid lithium borate
(LiBOB), difluorine oxalic acid boracic acid lithium (LiDFOB), trifluoromethyl sulfonic acid lithium (LiSO3CF3), lithium perchlorate (LiClO4), hexafluoro
Arsenic acid lithium (LiAsF6) and bis trifluoromethyl sulfimide lithium (Li (CF3SO2)2One or both of) N more than.
Preferably, the mass ratio of described cyclic carbonate solvents and linear carbonate solvent is 1：(2~3), it is described
Concentration of the electric conducting lithium salt in general electrolytic liquid is 0.8~1.0mol/L.
Above-mentioned high pressure, the preparation method for filling function electrolyte soon, comprise the following steps：
(1) cyclic carbonate solvents and linear carbonate solvent are mixed, clarification, water removal are commonly mixed molten
Agent；
(2) at ambient temperature, in the mixed solvent electric conducting lithium salt added obtained by step (1), obtains general electrolytic
Liquid；
(3) function of being added in the general electrolytic liquid that step (2) is obtained equivalent to general electrolytic liquid quality 1~5% adds
Plus agent benzal fluoride sulfone (DPS), obtain the high pressure, fill function electrolyte soon.
Clarification described in step (1), water removal preferably refer to by molecular sieve, activated carbon, calcium hydride, lithium hydride,
In anhydrous calcium oxide, calcium chloride, phosphorus pentoxide, alkali metal or alkaline-earth metal any one or two or more handled.
Described molecular sieve can be usedType,Type orType, is preferably selectedType orType.
Above-mentioned high pressure, application of the function electrolyte in manufacture lithium ion battery is filled soon, obtained battery has good
Cycle performance and high rate performance.
The present invention has the following advantages and effect relative to prior art：
(1) present invention uses the organic matter benzal fluoride sulfone of sulfur-bearing element additive as the height of lithium-ion electrolyte
Press, fill film for additive soon, can be in positive pole during first charge-discharge because the additive has relatively low oxidizing potential
Surface forms one layer of densification, stable interfacial film, optimizes positive electrode surface film, suppresses the surface-active of electrode, so as to suppress electricity
The further contact and HF formation of liquid and electrode active material are solved, oxidation point of the electrolyte bulk solvent in electrode surface is reduced
Solution.Room temperature cycles performance and high rate performance of the lithium ion battery containing this functional additive under 3~4.35V are changed
Kind, application prospect is good.
(2) present invention uses the organic matter benzal fluoride sulfone of sulfur-bearing element additive as the height of lithium-ion electrolyte
Press, fill additive soon, be due to that the sulfone group in the additive can effectively improve the electrical conductance of carbonates electrolyte, it is fluorine-based
Functional group can participate in the formation of the compositions such as skin covering of the surface LiF, and phenyl can improve the stability of electrolyte.
Brief description of the drawings
Fig. 1 is the high pressure of the preparation of embodiment 2, fills function electrolyte soon and the contrasts of the circle of general electrolytic solution battery circulation 70
Figure；Wherein, A：0.5C discharge and recharges；B：3C discharge and recharges.
Fig. 2 is multiplying power figure of the pole piece of embodiment 2 under the conditions of high pressure, different multiplying discharge and recharge；Wherein, A：Slow play is filled soon；
B：Fast charging and discharging；C：Trickle charge is put soon.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Embodiment 1
(1) by cyclic carbonate solvents ethylene carbonate (EC), linear carbonate solvent methyl ethyl carbonate (EMC) and carbonic acid
Diethylester (DEC), in mass ratio EC: EMC：DEC=3: 5：2 mixing, and using molecular sieve, calcium hydride, lithium hydride clarification,
Water removal, obtains mixed solvent；
(2) at ambient temperature, by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) is obtained is dissolved in, it is final concentration of
1.0mol/L, stirs, and obtains general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2) addition benzal fluoride sulfone (reagent is bought in Adamas, purity
More than 98%, without further purifying when using), the consumption of benzal fluoride sulfone is the 1% of electrolyte quality, is used
High pressure in lithium ion battery, function electrolyte is filled soon.
Embodiment 2
(1) by cyclic carbonate solvents ethylene carbonate (EC), linear carbonate solvent methyl ethyl carbonate (EMC) and carbonic acid
Diethylester (DEC), by mass ratio EC: EMC：DEC=3: 5：2 mixing, and removed using molecular sieve, calcium hydride, lithium hydride purifying
Miscellaneous, water removal, obtains mixed solvent；
(2) at ambient temperature, by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) is obtained is dissolved in, it is final concentration of
1.0mol/L, stirs, and obtains general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2) addition benzal fluoride sulfone (reagent is bought in Adamas, purity
More than 98%, without further purifying when using), the consumption of benzal fluoride sulfone is the 2% of electrolyte quality, is used
High pressure in lithium ion battery, function electrolyte is filled soon.
Embodiment 3
(1) by cyclic carbonate solvents ethylene carbonate (EC), linear carbonate solvent methyl ethyl carbonate (EMC) and carbonic acid
Diethylester (DEC), by mass ratio EC: EMC：DEC=3: 5：2 mixing, and removed using molecular sieve, calcium hydride, lithium hydride purifying
Miscellaneous, water removal, obtains mixed solvent；
(2) at ambient temperature, by electric conducting lithium salt LiPF6The in the mixed solvent that step (1) is obtained is dissolved in, it is final concentration of
1.0mol/L, stirs, and obtains general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2) addition benzal fluoride sulfone (reagent is bought in Adamas, purity
More than 98%, without further purifying when using), the consumption of benzal fluoride sulfone is the 5% of electrolyte quality, is used
High pressure in lithium ion battery, function electrolyte is filled soon.
Embodiment 4
(1) by cyclic carbonate solvents ethylene carbonate (EC), linear carbonate solvent methyl ethyl carbonate (EMC) and carbonic acid
Diethylester (DEC), by mass ratio EC: EMC：DEC=3: 5：2 mixing, and removed using molecular sieve, calcium hydride, lithium hydride purifying
Miscellaneous, water removal, obtains mixed solvent；
(2) at ambient temperature, by electric conducting lithium salt LiAsF6It is dissolved in the in the mixed solvent that step (1) is obtained, final concentration
For 1.0mol/L, stir, obtain general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2) addition benzal fluoride sulfone (reagent is bought in Adamas, purity
More than 98%, without further purifying when using), the consumption of phenylphosphonous acid diethylester is the 2% of electrolyte quality, is obtained
To the high pressure for lithium ion battery, function electrolyte is filled soon.
Embodiment 5
(1) by cyclic carbonate solvents ethylene carbonate (EC), linear carbonate solvent methyl ethyl carbonate (EMC) and carbonic acid
Diethylester (DEC), by mass ratio EC: EMC：DEC=3: 5：2 mixing, and removed using molecular sieve, calcium hydride, lithium hydride purifying
Miscellaneous, water removal, obtains mixed solvent；
(2) at ambient temperature, by electric conducting lithium salt LiSO3CF3It is dissolved in the in the mixed solvent that step (1) is obtained, final concentration
For 1.0mol/L, stir, obtain general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2) addition benzal fluoride sulfone (reagent is bought in Adamas, purity
More than 98%, without further purifying when using), the consumption of benzal fluoride sulfone is the 2% of electrolyte quality, is used
High pressure in lithium ion battery, function electrolyte is filled soon.
Embodiment 6
(1) by cyclic carbonate solvents ethylene carbonate (EC), linear carbonate solvent methyl ethyl carbonate (EMC) and carbonic acid
Diethylester (DEC), by mass ratio EC: EMC：DEC=3: 5：2 mixing, and removed using molecular sieve, calcium hydride, lithium hydride purifying
Miscellaneous, water removal, obtains mixed solvent；
(2) at ambient temperature, by electric conducting lithium salt Li (CF3SO2)2N is dissolved in the in the mixed solvent that step (1) is obtained, eventually
Concentration is 1.0mol/L, is stirred, and obtains general electrolytic liquid；
(3) in general electrolytic liquid prepared by step (2) addition benzal fluoride sulfone (reagent is bought in Adamas, purity
More than 98%, without further purifying when using), the consumption of benzal fluoride sulfone is the 2% of electrolyte quality, is used
High pressure in lithium ion battery, function electrolyte is filled soon.
Effect compares：
By embodiment 2 prepare for lithium ion battery high pressure, fill function electrolyte (that is to say 2%DPS) soon
It is compared with contrast general electrolytic liquid (that is to say STD)：
(1) Fig. 1 be embodiment 2 prepare the high pressure for being used for lithium ion battery, fill function electrolyte soon, carry out 70 height enclosed
Press after (4.35V) circulation, in small multiplying power 0.5C charge-discharge magnification (figure A), moreover it is possible to keep 95% capability retention, it is and general
Logical electrolyte carries out that close to after 70 circles 70% capability retention can only be kept.In addition, be can be seen that from figure B in big multiplying power 3C
Charge and discharge cycles after, battery is still significantly higher than in prepared high pressure, the capability retention (80%) for filling function electrolyte soon
General electrolytic liquid (63%).From the results, it was seen that the electrolyte of benzal fluoride sulfone is added in electrolyte is used for lithium-ion electric
Pond can improve its in high pressure, fill soon under the conditions of cycle performance, have relatively good application prospect in high-tension battery system.
(2) Fig. 2 be embodiment 2 prepare for lithium ion battery high pressure, fill function electrolyte, Li/NCM (811) soon
Battery carries out multiplying power test in the electrolyte that benzal fluoride sulfone is included, from the results, it was seen that finding either to fill slow soon
Put (Fig. 2A), (Fig. 2 C) is put in fast charging and discharging (Fig. 2 B) or trickle charge soon, benzal fluoride sulfone is added in the electrolytic solution and occupies this
Very big high-quality, before realizing that NCM (811) has preferably application as the excellent performance of the lithium battery performance of positive electrode
Scape.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of high pressure, function electrolyte is filled soon, it is characterised in that：The electrolyte is to be added in general electrolytic liquid equivalent to general
The functional additive of logical electrolyte quality 1%~5% is prepared；Described functional additive is benzal fluoride sulfone.
2. high pressure according to claim 1, function electrolyte is filled soon, it is characterised in that：
Described general electrolytic liquid is made up of cyclic carbonate solvents, linear carbonate solvent and electric conducting lithium salt.
3. high pressure according to claim 2, function electrolyte is filled soon, it is characterised in that：
Described cyclic carbonate solvents are ethylene carbonate.
4. high pressure according to claim 2, function electrolyte is filled soon, it is characterised in that：
Described linear carbonate solvent is included in dimethyl carbonate, methyl ethyl carbonate, diethyl carbonate and methyl propyl carbonate
It is one or more kinds of.
5. high pressure according to claim 2, function electrolyte is filled soon, it is characterised in that：
Described electric conducting lithium salt is selected from lithium hexafluoro phosphate, LiBF4, dioxalic acid lithium borate, difluorine oxalic acid boracic acid lithium, trifluoro
It is more than one or both of pyrovinic acid lithium, lithium perchlorate, hexafluoroarsenate lithium and bis trifluoromethyl sulfimide lithium.
6. high pressure according to claim 2, function electrolyte is filled soon, it is characterised in that：
Described cyclic carbonate solvents and the mass ratio of linear carbonate solvent are 1：(2~3), described electric conducting lithium salt is general
Concentration in logical electrolyte is 0.8~1.0mol/L.
7. high pressure described in any one of claim 1~6, the preparation method for filling function electrolyte soon, it is characterised in that including such as
Lower step：
(1) cyclic carbonate solvents and linear carbonate solvent are mixed, clarification, water removal obtain common mixed solvent；
(2) at ambient temperature, in the mixed solvent electric conducting lithium salt added obtained by step (1), obtains general electrolytic liquid；
(3) functional additive equivalent to general electrolytic liquid quality 1~5% is added in the general electrolytic liquid that step (2) is obtained
Benzal fluoride sulfone, obtains the high pressure, fills function electrolyte soon.
8. high pressure according to claim 7, the preparation method for filling function electrolyte soon, it is characterised in that：
Clarification, water removal described in step (1) refer to by molecular sieve, activated carbon, calcium hydride, lithium hydride, dry oxidation
In calcium, calcium chloride, phosphorus pentoxide, alkali metal or alkaline-earth metal any one or two or more handled.
9. high pressure according to claim 8, the preparation method for filling function electrolyte soon, it is characterised in that：
Described molecular sieve is usedType,Type orType.
10. high pressure described in any one of claim 1~6, application of the function electrolyte in manufacture lithium ion battery is filled soon.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107799823A (en) * | 2017-10-23 | 2018-03-13 | 华南师范大学 | A kind of electrolysis additive and electrolyte and lithium secondary battery containing the additive |
| WO2019156539A1 (en) * | 2018-02-12 | 2019-08-15 | 주식회사 엘지화학 | Non-aqueous electrolyte solution for lithium secondary battery and lithium secondary battery comprising same |
| WO2022197094A1 (en) * | 2021-03-16 | 2022-09-22 | 주식회사 엘지에너지솔루션 | Non-aqueous electrolyte for lithium secondary battery and lithium secondary battery comprising same |
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| CN101771167A (en) * | 2010-02-05 | 2010-07-07 | 九江天赐高新材料有限公司 | High-capacity lithium-ion electrolyte, battery and preparation method of battery |
| CN103493277A (en) * | 2011-04-22 | 2014-01-01 | 宇部兴产株式会社 | Nonaqueous electrolyte solution, electricity storage device using same, and trifluoromethylbenzene compound |
| CN105870501A (en) * | 2016-04-12 | 2016-08-17 | 华南师范大学 | High-voltage functional electrolyte and preparation method and application therefor |
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| CN103493277A (en) * | 2011-04-22 | 2014-01-01 | 宇部兴产株式会社 | Nonaqueous electrolyte solution, electricity storage device using same, and trifluoromethylbenzene compound |
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Application publication date: 20170922 |