CN102637901B - Electrolyte for lithium ion battery and preparation method thereof - Google Patents
Electrolyte for lithium ion battery and preparation method thereof Download PDFInfo
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- CN102637901B CN102637901B CN201210123080.0A CN201210123080A CN102637901B CN 102637901 B CN102637901 B CN 102637901B CN 201210123080 A CN201210123080 A CN 201210123080A CN 102637901 B CN102637901 B CN 102637901B
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Abstract
The invention discloses an electrolyte for a lithium ion battery and a preparation method thereof. The electrolyte consists of a main electrolyte, an electrolyte additive, a main solvent and a solvent additive. The preparation method comprises the following steps of: A. under the condition of vacuum or inert gas protection, respectively mixing the main solvent and the solvent additive with a drying agent (lithium oxide) which is dried to be at constant weight in advance, and mixing and filtering to remove the lithium oxide and lithium hydroxide sediment; B. uniformly mixing the dried main solvent and the dried solvent additive from the step A; and C. adding a main electrolyte mixture and an electrolyte additive into the solvent mixed in the step B, and agitating and dissolving under the vacuum and inert gas protection to prepare a solution with the mass mol concentration of the main electrolyte of 0.5-1.5 M. The electrolyte has the advantages of abundant resources, low price and no toxin, effectively improves the work temperature range of the battery and effectively prolongs the circulating service life of the battery, so that various types of the lithium ion batteries are manufactured; and the electrolyte is particularly suitable for manufacturing a lithium ion power battery with high power capacity and high multiplying power charging and discharging capacity.
Description
Technical field
The present invention relates to technical field of chemical power, be specifically related to again a kind of lithium-ion battery electrolytes, also relate to a kind of preparation method of lithium-ion battery electrolytes simultaneously, can be used for manufacturing the lithium ion battery of various models, be also applicable to manufacture the lithium-ion-power cell for high power charging-discharging.
Background technology
At present, existing industrial manufacturing lithium ion battery electrolyte used is mainly LiPF
6, LiBF
4deng being that electrolytical, electrolyte concentration is at 0.1～2.0M (mol/L, hereinafter to be referred as M) EC-EMC, EC-EMC-EMC, (wherein EC is ethylene carbonate for EC-EMC-DEC, EC-DMC-DEC-PC, EMC is methyl ethyl carbonate, DEC is diethyl carbonate, DMC is dimethyl carbonate, PC is propene carbonate, as follows) etc. the organic substance solution that is solvent.Electrolyte is very large on performance of lithium ion battery impact, this be due to bath composition and concentration and its conductivity and electrode reaction closely related, the conductivity of electrolyte and the invertibity of electrode reaction directly affect discharge capacity of lithium ion battery, the stability of electrolyte directly and electrolyte effect, can affect the security performance (Guo Yingjun etc. of lithium ion battery, lithium-ion battery electrolytes progress [J]. new material industry, 2007,8:60-64).Specific capacity, operating temperature range, charge and discharge cycles efficiency and the security performance of lithium-ion battery electrolytes to lithium ion battery is most important.And EC, DEC, DMC, EMC equal solvent be mainly used in lithium rechargeable battery, and PC and DME (1,2-dimethoxy-ethane/glycol dimethyl ether) are mainly used in disposable lithium-battery.Because PC is for secondary cell, very poor with the graphite cathode compatibility of lithium ion battery, in charge and discharge process, PC decomposes at graphite electrode surface, can cause coming off of graphite linings, (the Liao Hongying etc. thereby the charge/discharge capacity of reduction battery and cycle performance significantly decline, lithium-ion battery electrolytes [J]. industry forum, 2003,9:34-37.).Crown ether and cryptate can form clad type chelate with lithium ion, can improve the solubility of lithium salts in organic solvent, realize anion and cationic effective separation and the separating of lithium ion and solvent, and improve the conductance of electrolyte; Some fluoro chain ethers are as C
4f
9oCH
3etc. recommended for secondary lithium ion cell electrolyte solution, can improve the thermal stability (He Zhengzhen etc. of organic electrolyte, the progress [J] of lithium-ion battery electrolytes and functional additive thereof. contemporary chemical industry, 2011,40 (9): 928-930.); Trialkyl aryl-silane joins in the conventional electrolyte of lithium ion battery by 3～8% mass ratio, can improve the security performance of electrolyte, battery do not smolder in the time overcharging, not on fire, do not explode that (bear beautiful jade is strong etc., lithium ion battery is clicked right anti-overcharge additive progress [J]. chemical industry progress, 2011,30 (6): 1198-1204).Research shows: trace (0.5%) HMDS (HMDS) can suppress lithium-ion battery electrolytes LiPF in storage process
6hydrolysis and pyrolysis, reduce water and hydrofluoric content in electrolyte, improve storage stability and the thermal stability (Hu Lixin etc. of lithium-ion battery electrolytes, HMDS is as the research [J] of lithium-ion battery electrolytes stabilizer. chemistry and bioengineering, 2011,28 (2): 24-26.).
In addition, 200710143920.9 number Chinese invention patent application discloses a kind of " constituent of electrolyte of low temp lithium ion battery ", consisting of of this electrolyte: EC (ethylene carbonate), PC (propene carbonate), DME (1,2-dimethoxy-ethane/glycol dimethyl ether), EMC (methyl ethyl carbonate), DEC (diethyl carbonate), 1,3-PS (1,3-propane sultone), LiPF
6.This patent is disclosed is a kind of low temperature functional electrolyte, can improve battery electrical property at low temperatures.200810087478.7 disclose a kind of " lithium-ion battery electrolytes ", and the disclosed electrolyte of this patent comprises primary solvent: at least one in gamma-valerolactone, acetic acid methyl isobutyryl ester, 2-Methoxyethyl acetate, 2-ethoxyethyl acetate and diethy-aceto oxalate and lithium salts.200710123621.9 number Chinese invention patent application discloses " a kind of lithium-ion battery electrolytes ".The technology of this Patent Application Publication is: a kind of lithium-ion battery electrolytes contains electrolyte and organic solvent, organic solvent is EC, PC, DMC, EMC, DEC, biphenyl goods cyclohexyl benzene, and a kind of goods in additive vinylene carbonate, polypropylene carbonate alkene ester, gamma-butyrolacton, PS, butyl sultone is multiple.The click right side of this disclosure of the invention conducts electricity very well, internal resistance is little, can long-time heavy-current discharge, have stable high-temperature performance.201110243969.8 number Chinese patent application discloses " a kind of lithium-ion battery electrolytes ", its electrolyte is selected the mixture of di-oxalate lithium borate, difluorine oxalic acid boracic acid lithium, two fluoroform sulfimide lithiums, nonaqueous solvents is 1, one in 4-butane sultones, benzyltrimethyl ketone, DMF, methyl ethyl carbonate, methyl-sulfoxide, oxolane, acetone, ethyl acetate, propylene sulfite.It is said: the disclosed electrolyte of this invention technology has good stability, high low temperature serviceability, high conductivity, high rate performance excellence, energy density advantages of higher.But the technology of this Patent Application Publication is not used the data of the correlated performance of the battery of this technology electrolyte manufacture.
Correlative study and the disclosed Patents technology of comprehensive above-mentioned existing lithium-ion battery electrolytes are visible, prior art taking lithium salts as electrolyte, common are machine solvent as solution and some functional additive etc., the lithium ion battery of the lithium-ion battery electrolytes manufacturing of manufacturing obviously exists following not enough: 1) high temperature or low-temperature working poor performance, even higher (more than 55 DEG C) or lower (below 30 DEG C) battery cannot work completely or service behaviour very poor; 2) power-type lithium ion battery high current charge-discharge weak effect, affects the normal work of lithium ion battery group, has seriously limited the range of application of lithium-ion-power cell; 3) battery storage capacity decay is serious, directly affects capacity and the service life cycle of lithium ion battery; 4) anti-over-charging poor performance, affects lithium ion battery efficiency for charge-discharge, battery capacity and service life cycle; 5) poor safety performance, normally discharge and recharge and battery classification partial volume process in and in the course of work, all there is actual potential safety hazard; 6) many electrolyte solvents, as furans, pyridine and acetone etc. have larger toxicity, more or less can cause pollution to a certain degree in the production of lithium ion battery and the process of use and old and useless battery.Although above-mentioned deficiency is not exclusively due to lithium-ion battery electrolytes, all deficiencies all with electrolyte conductivity energy, with the compatibility of electrode, the fail safe of electrode charge and discharge performance and cycle life, battery is had to direct impact.Therefore, it is all within reason how lithium ion battery is emphasized the high request of electrolyte, solves prior art deficiency, and electrolyte is also one of very important factor.
Summary of the invention
In order to solve prior art above shortcomings, the object of the invention is to be to provide a kind of lithium-ion battery electrolytes, lithium ion battery prepared by the present invention, under-40～65 DEG C of temperature range working environments, can normally work, lithium ion battery efficiency for charge-discharge, heavy-current discharge effect, discharge capacity obviously improve, charge and discharge cycles significant prolongation in useful life, and lithium ion battery comprehensive electrochemical significantly improves.
Another object of the present invention is the preparation method who has been to provide a kind of lithium-ion battery electrolytes, and technique is simple, additive amount is few, price is low, remarkable to improving lithium ion battery comprehensive electrochemical effect.Not changing under existing electrolyte production equipment condition, can realize the manufacture of all kinds lithium ion battery, be specially adapted to manufacture the lithium-ion-power cell of high power capacity, high power charging-discharging.
The present invention is achieved by following technical proposals:
A kind of lithium-ion battery electrolytes, is made up of main electrolyte, additive agent electrolyte, organic solvent (or claiming main solvent) and solvent additive; Wherein, main electrolyte mol ratio is respectively 0.5～1: 0.1～0.3: 0.01～0.05: 0.01～0.05 lithium hexafluoro phosphate (LiPF
6), LiBF4 (LiBF
4), lithium fluorosilicate (Li
2siF
6) and lithium perchlorate (LiClO
4) four mixture; Additive agent electrolyte is that mol ratio is three perfluor ethyl three lithium fluophosphate (LiPF of main electrolyte molal quantity 0.1～0.5%
3(C
2f
5)
3), trifluoromethyl sulfonic acid lithium (LiCF
3sO
3), lithium carbonate (Li
2cO
3) and lithium acetate (LiAc) in three kinds or the mixtures that mass ratio mixes such as four kinds; Main solvent is that equal-volume is than the ethylene carbonate (EC), diethyl carbonate (DEC), the dimethyl carbonate (DMC), 1 that mix, 2-dimethoxy-ethane/glycol dimethyl ether (DME), methyl ethyl carbonate (EMC), 1, three kinds or the mixture of four kinds in 3-propane sultone (1.3-PS), sulfurous acid glycol ester (ES/DTO), dicyclohexyl carbon dimethylamine (DCC), butylene sulfite (BS), vinylethylene carbonate (VEC); Solvent additive is the mixture of any three kinds that equal-volume is seen in acid esters (DECP), sulfuric acid propylene (TS), methane-disulfonic acid methylene ester (CDE) than the HMDS (HMDS), the diethyl (cyano methyl) that mix, account for main solvent volume ratio 0.1～0.5%.
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; at vacuum (1～10kpa; following vacuum is this vacuum ranges) or the condition of inert gas shielding under, be that the prior vacuumize of solvent 1～5% is to the drier lithia (Li of constant weight with mass ratio respectively by main solvent, solvent additive (being referred to as " solvent ")
2o) mix, stir 4～12 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step; dried first step equal-volume is mixed with solvent additive dried, that account for main solvent volume ratio 0.1～0.5% than the main solvent mixing; under the condition of vacuum (1～10kpa) or inert gas shielding, mix, obtain electrolyte solvent.
The 3rd step, by under vacuum (1～10kpa) condition, be dried to constant weight, mol ratio is 0.5～1: 0.1～0.3: 0.01～0.05: 0.01～0.05 lithium hexafluoro phosphate (LiPF
6), LiBF4 (LiBF
4), lithium fluorosilicate (Li
2siF
6) and lithium perchlorate (LiClO
4) main electrolyte mixture and be dried to constant weight etc. mole mixing, total mole number accounts for the additive agent electrolyte of main electrolyte mixture total mole number 0.1～0.5%; join in the solvent that second step mixes; under vacuum or inert gas shielding, stir 4～8 hours; be made into main electrolyte molality (note: additive agent electrolyte concentration is not counted in; identical below) be the solution of 0.5～1.5M (M=mol/L, below identical).
Described main solvent is ethylene carbonate (EC), diethyl carbonate (DEC), the dimethyl carbonate (DMC), 1 that volume ratio is mixed, 2-dimethoxy-ethane/glycol dimethyl ether (DME), methyl ethyl carbonate (EMC), 1, the mixture of any three kinds or four kinds in 3-propane sultone (1.3-PS), sulfurous acid glycol ester (ES/DTO), dicyclohexyl carbon dimethylamine (DCC), butylene sulfite (BS), vinylethylene carbonate (VEC).
Described solvent additive is the mixture of any three kinds that equal-volume is seen in acid esters (DECP), sulfuric acid propylene (TS), methane-disulfonic acid methylene ester (CDE) than the HMDS (HMDS), the diethyl (cyano methyl) that mix.
Described main electrolyte is that mol ratio is respectively 0.5～1: 0.1～0.3: 0.01～0.05: 0.01～0.05 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixture.
Described electrolysis additive be mol ratio be main electrolyte molal quantity 0.1～0.5%, etc. mass ratio mix LiPF
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3, and LiAc in three kinds or the mixture of four kinds.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
Adopt technical scheme of the present invention, can obtain following significantly effect:
The lithium ion battery that the lithium-ion battery electrolytes of preparing by the technology of the present invention is produced, can improve existing conventional positive active material (cobalt acid lithium owing to having used simultaneously, lithium nickelate, LiMn2O4 or cobalt nickel LiMn2O4 ternary material and LiFePO4 etc.), the compound additive combination of negative electrode active material (lithium ion battery negative pole active materials material " Activated Graphite ") and electrolyte property, make the lithium ion battery of manufacturing can obtain following effect: first, the utilance of positive active material and negative electrode active material improves greatly, thereby can effectively improve the efficiency for charge-discharge of battery, and then the discharge capacity of raising lithium ion battery, the second, the effective utilization that has improved positive active material, reduced positive active material and negative electrode active material crystal habit in use change, come off etc., high current charge-discharge effect, electrode and the discharge capacity of the cell of electrode are significantly improved, the 3rd, effectively raise the operating temperature range of lithium ion battery, battery can more efficiently be worked in-45～65 DEG C of temperature ranges, and the discharge capacity first under-45～65 DEG C of conditions reaches the more than 70% of design capacity theoretical value, the 4th, effectively extend the service life cycle of battery, compared with prior art, the lithium ion battery service life cycle of manufacture of the present invention extends and reaches 132～253 charge and discharge cycles, the 5th, there is good overcharge resistant ability, overcharge in experimentation, overcharge capacity exceed design capacity 50% battery not significantly in the security incident such as high, the burning of voltage rise, blast occur.
The present invention is applicable to manufacture the lithium rechargeable battery of various models, also can be used for manufacturing cylindrical, the lithium-ion-power cell of all kinds, various models.
Compared with prior art, the present invention has following advantage and useful effect:
The first, a kind of lithium-ion battery electrolytes that prepared by the present invention, the electrolyte primary raw material used of preparing due to the present invention is all more common raw material, abundant, cheap, the nontoxic or low toxicity of originating, therefore low production cost, be specially adapted to the application of the lithium-ion-power cell production field that electrolyte consumption is larger, and can not increase more production cost; Can not cause problem of environmental pollution;
The second, a kind of lithium-ion electrolyte that prepared by the present invention, owing to having used relatively abundant multiple additive agent electrolyte, the solvent additive in relative low price, source, and the relatively main electrolyte of the consumption of additive and main solvent less, significantly improving on the basis of lithium ion battery comprehensive electrochemical, can't significantly increase extra production cost;
Three, a kind of lithium-ion battery electrolytes that prepared by the present invention, owing to having used multiple, the multi-functional compound additive combination that can improve positive active material, negative electrode active material and electrolyte property simultaneously, the utilance of positive active material and negative electrode active material is improved greatly, thereby can effectively improve the efficiency for charge-discharge of battery, and then the discharge capacity of raising battery, more than same model capacity of lithium ion battery has increased 100mAh than prior art;
The 4th, a kind of lithium-ion battery electrolytes prepared by the present invention, can improve positive active material owing to having used simultaneously, the little molecule lithium carbonate of negative electrode active material and electrolyte property, improving effective utilization of positive active material, reduce the change of positive active material and negative electrode active material crystal habit in use, electrolytic conductivity improves, when the high current charge-discharge effect of electrode is significantly improved, the solidifying point of electrolyte is reduced, the elevation of boiling point, lithium ion battery can more effectively be worked in wider temperature range,
The 5th, a kind of lithium ion battery special electrolysis liquid prepared by the present invention, can improve positive active material owing to having used simultaneously, the composite electrolyte additive of negative electrode active material and electrolyte property and double solvents additive, make electrolyte solution with can be at lithium ion cell positive, compatibility between negative pole improves, make effectively to form between electrolyte and both positive and negative polarity solid solid/electrolyte interface film (SEI), embedding/the eliminating efficiency of lithium ion is improved, the efficiency for charge-discharge that is lithium ion battery is able to obvious improvement, improved effective utilization of positive active material simultaneously, reduce the change of positive active material and negative electrode active material crystal habit in use, the high current charge-discharge successful of electrode and battery is improved, efficiency for charge-discharge has increased more than 10% than prior art,
Six, the lithium-ion battery electrolytes that prepared by the present invention, can improve the compound additive combination of positive active material, negative electrode active material and electrolyte property, multiple additive agent electrolyte, electrolysis additive owing to having used simultaneously, effectively raise the operating temperature range of battery, battery can effectively be worked in-45～65 DEG C of temperature ranges;
The 7th, a kind of lithium-ion battery electrolytes prepared by the present invention, can improve positive active material owing to having used simultaneously, the compound additive combination of negative electrode active material and electrolyte property, effectively extend the service life cycle of battery, compared with the battery that the electrolyte of producing with prior art is assembled, because the electrolyte of this technology can improve electrode active material utilance, improve the SEI film between electrolyte and electrode, improve the electricity of electrolyte and lead efficiency, the lithium ion battery of manufacturing is being improved greatly compared with the charge-discharge performance under high magnification, 2C multiplying power service life cycle all exceedes control cell performance.
Eight, a kind of lithium-ion battery electrolytes that prepared by the present invention, owing to having used the compound additive combination that can improve positive active material, negative electrode active material and electrolyte property simultaneously, effectively extend the service life cycle of battery, compared with the battery that the electrolyte of producing with prior art is assembled, 2C multiplying power service life cycle has increased by 132～253 charge and discharge cycles than control cell.
Brief description of the drawings
Fig. 1 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of-45 DEG C;
Fig. 2 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of-30 DEG C;
Fig. 3 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of-15 DEG C;
Fig. 4 is the lithium ion battery of a kind of electrolyte assembling discharging efficiency curve in the time of 0 DEG C;
Fig. 5 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of 15 DEG C;
Fig. 6 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of 25 DEG C;
Fig. 7 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of 35 DEG C;
Fig. 8 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of 45 DEG C;
Fig. 9 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of 55 DEG C;
Figure 10 is the lithium ion battery of a kind of electrolyte assembling discharge capacity curve in the time of 65 DEG C;
Wherein: A～2000mAh18650 type lithium ion battery of the present invention, B～same model contrast lithium ion battery; Discharge and recharge is all to complete under 2C multiplying power, constant current charge-discharge test condition.
Embodiment
Below in conjunction with embodiment and Figure of description, the present invention is done to further detailed description.
Embodiment 1:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; than the mixture of three kinds of the solvent additive HMDS (HMDS), the DECP that mix (diethyl (cyano methyl) see acid esters), TS (sulfuric acid propylene), be that the prior vacuumize of solvent 5% is to the drier lithia (Li of constant weight with mass ratio by main solvent EC, the DEC, VEC (vinylethylene carbonate) three's that mix for volume ratio mixture, equal-volume respectively
2o) mix, stir 4 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.1%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.5: 0.1: 0.01: 0.01 main electrolyte LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixture, and be dried to constant weight etc. mole mixing, total mole number accounts for the additive agent electrolyte LiPF of main electrolyte mixture total mole number 0.1%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3three kinds of mixtures, join in the electrolyte solvent that second step mixes, and stir 4 hours under vacuum or inert gas shielding, and being made into main electrolyte molality (note: additive agent electrolyte concentration is not counted in, below identical) is the solution of 0.5M.
Described a kind of nickel-base alkaline electrokinetic cell special electrolysis liquid is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, discharge and recharge under-45 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 1.
Embodiment 2:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; solvent additive HMDS (HMDS), the TS (sulfuric acid propylene) that equal-volume is mixed than the mixture of three kinds of main solvent EC, the DEC, the BS (butylene sulfite) that mix, equal-volume ratio, CDE (methane-disulfonic acid methylene ester) three's mixture are that the prior vacuumize of solvent 5% is to the drier lithia (Li of constant weight with mass ratio respectively
2o) mix, stir 4 hours, remove by filter lithia and lithium hydroxide precipitation.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.1%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.6: 0.1: 0.02: 0.02 the electrolytical LiPF of master
6, LiBF
4, Li
2siF
6and LiClO
4four mixture, and be dried to constant weight etc. mole mixing, total mole number account for main electrolyte mixture total mole number 0.15%, equimolar ratio mix LiCF
3sO
3, Li
2cO
3, and LiAc (lithium acetate) additive agent electrolyte, join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 4 hours, be made into the solution that main electrolyte molality is 0.65M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, discharge and recharge under-30 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 2.
Embodiment 3:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than DMC, the 1.3-PS, BS (butylene sulfite) three's that mix mixture main solvent, equal-volume than the admixture solvent additive of the DECP mixing (diethyl (cyano methyl) see acid esters), TS (sulfuric acid propylene), CDE (methane-disulfonic acid methylene ester), with mass ratio be that the prior vacuumize of solvent 4% is to the drier lithia (Li of constant weight
2o) mix, stir 10 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.2%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.7: 0.2: 0.03: 0.03 main electrolyte LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixture, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiCF of main electrolyte mixture total mole number 0.2%
3sO
3, Li
2cO
3, and the mixture additive agent electrolyte of LiAc (lithium acetate), join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 5 hours, be made into the solution that main electrolyte molality is 0.8M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, discharge and recharge under-15 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 3.
Embodiment 4:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than EC, the EMC, DCC (dicyclohexyl carbon dimethylamine) the mixture main solvent that mix, equal-volume than the admixture solvent additive that mixes DECP (diethyl (cyano methyl) see acid esters), TS (sulfuric acid propylene), CDE (methane-disulfonic acid methylene ester), with mass ratio be that the prior vacuumize of solvent 4% is to the drier lithia (Li of constant weight
2o) mix, stir 10 hours, dry except the water in desolventizing, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.2%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.75: 0.2: 0.03: 0.03 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.25%
3(C
2f
5)
3, Li
2cO
3and LiAc (lithium acetate) three's mixture additive agent electrolyte, join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 5 hours, be made into the solution that main electrolyte molality is 0.9M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, are to discharge and recharge under 0 DEG C of condition 2C rate charge-discharge condition in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 4.
Embodiment 5:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than EMC, the ES/DTO (sulfurous acid glycol ester), DCC (the dicyclohexyl carbon dimethylamine) three's that mix mixture main solvent, equal-volume than the HMDS (HMDS), the DECP that mix (diethyl (cyano methyl) see acid esters), CDE (methane-disulfonic acid methylene ester) three's admixture solvent additive, with mass ratio be that the prior vacuumize of solvent 3% is to the drier lithia (Li of constant weight
2o) mix, stir 8 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.3%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.8: 0.25: 0.035: 0.035 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.3%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3three's mixture additive agent electrolyte, joins in the solvent that second step mixes, and stirs 6 hours under vacuum or inert gas shielding, is made into the solution that main electrolyte molality is 1.0M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, be to discharge and recharge under 15 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 5.
Embodiment 6:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than the mixture main solvent of EC, the EMC, 1.3-PS, the BS (butylene sulfite) four that mix, equal-volume than the admixture solvent additive of any three kinds in HMDS (HMDS), the TS (sulfuric acid propylene), the CDE (methane-disulfonic acid methylene ester) that mix, with mass ratio be that the prior vacuumize of solvent 3% is to the drier lithia (Li of constant weight
2o) mix, stir 8 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.35%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.85: 0.25: 0.04: 0.04 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.35%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3, and the mixture additive agent electrolyte of LiAc (lithium acetate) four, join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 6 hours, be made into the solution that main electrolyte molality is 1.1M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, be to discharge and recharge under 25 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 6.
Embodiment 7:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than the mixture main solvent of 1.3-PS, the ES/DTO (sulfurous acid glycol ester), DCC (dicyclohexyl carbon dimethylamine), the BS (butylene sulfite) four that mix, equal-volume than the admixture solvent additive of any three kinds in HMDS (HMDS), the TS (sulfuric acid propylene), the CDE (methane-disulfonic acid methylene ester) that mix, with mass ratio be that the prior vacuumize of solvent 2% is to the drier lithia (Li of constant weight
2o) mix, stir 6 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.4%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.9: 0.26: 0.04: 0.04 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.4%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3, and the mixture additive agent electrolyte of LiAc (lithium acetate) four, join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 6 hours, be made into the solution that main electrolyte molality is 1.25M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, be to discharge and recharge under 35 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 7.
Embodiment 8:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than all mixture main solvent of EC, DME, BS (butylene sulfite), VEC (vinylethylene carbonate) three mixing, equal-volume than the HMDS (HMDS), the DECP that mix (diethyl (cyano methyl) see acid esters), TS (sulfuric acid propylene) three's admixture solvent additive, be that the prior vacuumize of solvent 2% is to the drier lithia (Li of constant weight with mass ratio respectively
2o) mix, stir 4 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.4%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 0.95: 0.28: 0.046: 0.046 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.45%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3, and the mixture additive agent electrolyte of LiAc (lithium acetate) four, join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 4 hours, be made into the solution that main electrolyte molality is 1.3M.
Described a kind of nickel-base alkaline electrokinetic cell special electrolysis liquid is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, be to discharge and recharge under 45 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 8.
Embodiment 9:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; by equal-volume than the mixture main solvent of EC, the 1.3-PS, ES/DTO (sulfurous acid glycol ester), the DCC (dicyclohexyl carbon dimethylamine) four that mix, equal-volume than the HMDS (HMDS), the DECP that mix (diethyl (cyano methyl) see acid esters), CDE (methane-disulfonic acid methylene ester) three's admixture solvent additive, be that the prior vacuumize of solvent 1% is to the drier lithia (Li of constant weight with mass ratio respectively
2o) mix, stir 4 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.5%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 1: 0.3: 0.045: 0.045 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight, etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.45%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3, and the mixture additive agent electrolyte of LiAc (lithium acetate), join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 8 hours, be made into the solution that main electrolyte molality is 1.4M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, be to discharge and recharge under 55 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 9.
Embodiment 10:
A preparation method for lithium-ion battery electrolytes, the steps include:
The first step; under the condition of vacuum or inert gas shielding; than the admixture solvent additive of three kinds of HMDS (HMDS), TS (sulfuric acid propylene), the CDE (methane-disulfonic acid methylene ester) of the mixture main solvent of four kinds of 1.3-PS, the ES/DTO (sulfurous acid glycol ester), DCC (dicyclohexyl carbon dimethylamine), the BS (butylene sulfite) that mix, the mixing of equal-volume ratio, be that the prior vacuumize of solvent 1% is to the drier lithia (Li of constant weight with mass ratio by equal-volume respectively
2o) mix, stir 12 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm.
Second step, mixes than the main solvent mixing dried first step equal-volume with solvent additive dried, that account for main solvent volume ratio 0.5%, under the condition of vacuum or inert gas shielding, mix, and obtains electrolyte solvent.
The 3rd step, by under vacuum condition, be dried to constant weight, mol ratio is respectively 1: 0.3: 0.05: 0.05 LiPF
6, LiBF
4, Li
2siF
6and LiClO
4four mixing owner electrolyte, and be dried to constant weight etc. mole mixing, total mole number accounts for the LiPF of main electrolyte mixture total mole number 0.5%
3(C
2f
5)
3, LiCF
3sO
3, Li
2cO
3, and the mixture additive agent electrolyte of four kinds of LiAc (lithium acetate), join in the solvent that second step mixes, under vacuum or inert gas shielding, stir 8 hours, be made into the solution that main electrolyte molality is 1.5M.
Described a kind of lithium-ion battery electrolytes is exactly to be prepared from according to the method described above.
With a kind of lithium-ion battery electrolytes of preparation, 18650 type 2000mAh lithium ion batteries of assembling, be to discharge and recharge under 65 DEG C of condition 2C rate charge-discharge conditions in temperature, test charge-discharge performance, high temperature performance etc., and with contrast test battery the same terms under test, the results detailed in accompanying drawing 10.
Claims (1)
1. a lithium-ion battery electrolytes, is made up of main electrolyte, additive agent electrolyte, main solvent and solvent additive;
Described main electrolyte is the mixture of the mol ratio lithium hexafluoro phosphate, LiBF4, lithium fluorosilicate and the lithium perchlorate that are respectively 0.5～1:0.1～0.3:0.01～0.05:0.01～0.05;
Described additive agent electrolyte be mol ratio be in three perfluor ethyl three lithium fluophosphates, trifluoromethyl sulfonic acid lithium, lithium carbonate and the lithium acetate of main electrolyte molal quantity 0.1～0.5% three kinds or four kinds etc. the mixture that mixes of mass ratio;
Described main solvent is that equal-volume is than the ethylene carbonate, diethyl carbonate, dimethyl carbonate, glycol dimethyl ether, the methyl ethyl carbonate, 1 that mix, three kinds or the mixture of four kinds in 3-propane sultone, sulfurous acid glycol ester, dicyclohexyl carbon dimethylamine, butylene sulfite, vinylethylene carbonate;
Described solvent additive is that equal-volume is than the mixture of any three kinds in the HMDS mixing, account for main solvent volume ratio 0.1～0.5%, diethyl (cyano methyl) phosphonate ester, sulfuric acid propylene, methane-disulfonic acid methylene ester;
The main electrolyte concentration of above-mentioned electrolyte is 0.5～1.5M, and additive agent electrolyte concentration is not counted in;
The preparation method of described lithium-ion battery electrolytes, the steps include:
The first step, under the condition of vacuum 1～10kpa or inert gas shielding, the drier lithia that prior vacuum 1～10kpa of 1～5% of solvent and solvent quality is dried to constant weight mixes, stir 4～12 hours, remove by filter lithia and lithium hydroxide precipitation, ensure in solvent that water content is lower than 10ppm;
Described solvent represents main solvent or solvent additive;
Second step, mixes the main solvent dried first step with dried solvent additive, under the condition of vacuum 1～10kpa or inert gas shielding, mix, and obtains electrolyte solvent;
The 3rd step; to under vacuum 1～10kpa condition, be dried to the main electrolyte mixture of constant weight and be dried to the additive agent electrolyte of constant weight; join in the solvent that second step mixes; under vacuum or inert gas shielding, stir 4～8 hours, be made into the solution that main electrolyte molar concentration is 0.5～1.5M.
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| JP5655842B2 (en) * | 2012-10-30 | 2015-01-21 | トヨタ自動車株式会社 | Non-aqueous electrolyte secondary battery |
| CN103219508B (en) * | 2013-04-12 | 2014-12-24 | 北京理工大学 | Electrolyte modifying method for improving cycling stability and low temperature performance of 5V LiNi0.5Mn1.5O4 anode material |
| CN104112869A (en) * | 2013-04-19 | 2014-10-22 | 南通力合新能源有限公司 | Nonaqueous electrolyte additive capable of improving high-temperature impedance performance of manganese-contained lithium ion battery |
| JP6433486B2 (en) | 2014-03-27 | 2018-12-05 | ダイキン工業株式会社 | Electrolytic solution and electrochemical device |
| CN106848234A (en) * | 2017-02-20 | 2017-06-13 | 海宁聚兴新能源科技有限公司 | A kind of cell negative electrode material |
| CN108155415A (en) * | 2017-11-29 | 2018-06-12 | 清远佳致新材料研究院有限公司 | A kind of lithium-ion battery electrolytes and lithium ion battery |
| CN108306018A (en) * | 2017-12-28 | 2018-07-20 | 骆驼集团武汉光谷研发中心有限公司 | A kind of lithium iron phosphate dynamic battery improving low temperature charging performance |
| CN110994023B (en) * | 2019-11-29 | 2023-05-16 | 湖北宇电能源科技股份有限公司 | Lithium ion battery safety electrolyte, preparation method and application thereof, and lithium ion battery |
| CN111640986B (en) * | 2020-05-28 | 2021-05-25 | 珠海冠宇电池股份有限公司 | High-safety electrolyte suitable for high-energy-density lithium ion battery |
| CN112038696B (en) * | 2020-08-07 | 2022-07-05 | 合肥国轩高科动力能源有限公司 | High-voltage electrolyte and lithium ion battery comprising same |
| CN112133958A (en) * | 2020-09-25 | 2020-12-25 | 天科新能源有限责任公司 | Method for inhibiting moisture generation in lithium ion battery |
| JP2024540381A (en) * | 2022-03-16 | 2024-10-31 | エルジー エナジー ソリューション リミテッド | Lithium secondary battery |
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| CN101442144A (en) * | 2009-01-14 | 2009-05-27 | 北京化学试剂研究所 | Method for stabilizing color and luster, moisture and fluohydric acid content of non-aqueous electrolyte |
| CN101783422A (en) * | 2009-01-16 | 2010-07-21 | 比亚迪股份有限公司 | Additive and electrolyte containing the same and lithium-ion battery |
| CN102064344A (en) * | 2010-12-21 | 2011-05-18 | 东莞市杉杉电池材料有限公司 | Novel electrolyte for power battery |
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| CN101442144A (en) * | 2009-01-14 | 2009-05-27 | 北京化学试剂研究所 | Method for stabilizing color and luster, moisture and fluohydric acid content of non-aqueous electrolyte |
| CN101783422A (en) * | 2009-01-16 | 2010-07-21 | 比亚迪股份有限公司 | Additive and electrolyte containing the same and lithium-ion battery |
| CN102064344A (en) * | 2010-12-21 | 2011-05-18 | 东莞市杉杉电池材料有限公司 | Novel electrolyte for power battery |
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Address after: 510000 No. 38, Yunfeng Road, Xinhua Industrial Zone, Xinhua Town, Huadu District, Guangzhou, Guangdong Patentee after: Guangzhou Yuntong Lithium Battery Co.,Ltd. Address before: 510800, Yunfeng Road, Xinhua Industrial Zone, Huadu District, Guangdong, Guangzhou 38, China Patentee before: GUANGZHOU WINTONIC BATTERY & MAGNET Co.,Ltd. |