CN106684448A - Preparation method for high-temperature resistant lithium battery electrolyte - Google Patents
Preparation method for high-temperature resistant lithium battery electrolyte Download PDFInfo
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- 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
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Abstract
The invention relates to a preparation method for high-temperature resistant lithium battery electrolyte and belongs to the technical field of electrolyte preparation. According to the method, lithium hydroxide, boric acid and phosphorus pentoxide are uniformly mixed and are compressed into a sheet; oxalic acid is heated to sublimate; the sheet is fumigated by the sublimated oxalic acid; then the sheet is placed in a drying oven for reaction, thereby obtaining crude electrolyte; impurities are removed through anhydrous acetonitrile; refined electrolyte is obtained through concentration and drying; through utilization of nano titanium dioxide as catalyst, chlorine is catalyzed to react with partial ethylene carbonate and propylene carbonate under an UV-irradiation condition, thereby generating halides; and mixing is carried out to obtain the electrolyte. Through application of the high-temperature resistant lithium battery electrolyte prepared by the method, the service life of a lithium battery is prolonged; and 670-750 charge/discharge cycles can be achieved. When the lithium battery works in an environment with the temperature of 50-55 degrees centigrade, the electrode discharge capacity of the lithium battery reaches 220-240 mAh/g, and the lithium battery has relatively high thermal stability.
Description
Technical field
The present invention relates to a kind of preparation method of high-temperature-reslithium lithium battery electrolyte, belongs to electrolyte preparing technical field.
Background technology
Lithium ion battery is current specific energy highest rechargeable battery, and it instead of lithium metal and makees with the compound of embedding lithium
For anode, so as to overcome passivation and the Li dendrite problem of traditional lithium battery Anodic, and lithium ion battery has work electricity
The advantages of pressure is high, energy density is high, power density is big, has been widely used in the fields such as number, mobile communication, and progressively in state
Anti-, military aspect application, in recent years, with developing rapidly for electric bicycle and electric automobile, lithium ion battery is considered as
It is the Vehicular dynamic battery of current most potential development.Electrolyte is the important component part of lithium battery, and it is positive and negative in battery
Play the ion conductor of conduction between pole, the performance of itself and its state of interface that formed with both positive and negative polarity are largely
Affect the performance of battery.Excellent non-aqueous electrolyte for lithium cell should possess following some requirement：（1）Chemical stability is good, with electricity
Both positive and negative polarity active substance and collector in pond（Typically with aluminium foil and Copper Foil）There is no chemical reaction；（2）Electrochemical stability window
Mouth is wide；（3）Ionic conductivity is high, and electronic conductivity is low；（4）Temperature range is properly that boiling point is high, and fusing point is low；（5）Safety and low toxicity,
Non-environmental-pollution.
Traditional electrolyte that can obtain high circulation efficiency has LiAlCl4+SO2, the metal lithium electrode in this kind of electrolyte
Cycle efficieny close 100%, but due to the electrolytic corrosion it is strong, SO2Highly volatile, easily to environment, system
Standby technological requirement is high, therefore this electrolyte is not suitable for practical application；In addition LiAsF6/ DOL system electrolyte is close in small current
High circulation efficiency can also be obtained under degree, but the solute LiAsF in this electrolyte6It is poisonous, and system is unstable, to temperature
Sensitivity, is particularly in hot environment（55℃）, the stability of lithium battery electrolytes can drastically reduce, and there is greatly safety hidden
Suffer from.
The content of the invention
The technical problem to be solved is：It is quick to temperature in use for traditional lithium battery electrolytes
Sense, especially when ambient temperature is higher than more than 55 DEG C, electrolyte stability drastically declines, and there is a problem of larger potential safety hazard,
There is provided one kind to make borate by oneself as electrolyte, compound with chlorocarbonic acid vinyl acetate and Allyl carbonate, high temperature resistant lithium is obtained
The method of battery electrolyte.The present invention is uniform by Lithium hydrate, boric acid and phosphorus pentoxide ball milling mixing first, and is pressed into thin
Piece, subsequently by oxalic acid subliming by heating, using the stifling thin slice of the oxalic acid of distillation, then is placed in reaction in baking oven by thin slice, and crude product is obtained
Electrolyte, followed by anhydrous acetonitrile impurity is removed, and concentrated to be dried to obtain refined electrolyte, recycling nano titanium oxide is
Catalyst, chlorine is catalyzed under the conditions of ultraviolet light and is reacted with part ethylene carbonate and Allyl carbonate, generates halides,
Improve the electrochemical stability of solvent and the safety of battery, last blended prepared high-temperature-reslithium lithium battery electrolyte.The present invention
Homemade borate heat stability is high, and heat decomposition temperature can meet the height of electric automobile or hybrid electric vehicle up to more than 300 DEG C
Temperature needs, and improve lithium battery uses safety, efficiently solves the problems, such as that traditional lithium battery resistance to elevated temperatures is poor.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
（1）Count by weight, 25~35 parts of Lithium hydrates are taken successively, 60~70 parts of boric acid, 3~5 parts of phosphorus pentoxides are poured into
It is 10 by ball material mass ratio in ball grinder:1~15:1 adds zirconium oxide ball milling pearl, after 2~4h of ball-milling treatment, discharging, and by ball
Material is pressed into thickness as 0.6~0.8mm thin slices with 2~4MPa pressure in grinding jar；
（2）Above-mentioned gained thin slice is evenly laid out on wire gauze, and wire gauze is hung at 3~5cm of crucible top, subsequently
The oxalic acid of 6~8 times of above-mentioned Lithium hydrate quality, heating crucible is added to make crucible mesoxalic acid be warming up to 120~125 in crucible
DEG C, insulation distils completely up to oxalic acid, collects the thin slice on wire gauze, pours in crucible Jing after 5~10min of mortar grinder, and
Crucible is moved in baking oven, under the conditions of temperature is for 140~150 DEG C, 20~24h of insulation reaction, discharging, after naturally cool to room
Temperature, obtains crude product electrolyte；
（3）Above-mentioned gained crude product electrolyte is poured in beaker, the anhydrous acetonitrile of 4~6 times of crude product electrolyte quality is added, is used
After Glass rod stirring 20~30min of mixing, filter, collect filtrate, and gained filtrate is proceeded to into Rotary Evaporators, in temperature be 65
Under the conditions of~70 DEG C, the 1/10 of concentrated by rotary evaporation to original volume, concentrated solution is obtained, then gained concentrated solution is proceeded in baking oven, in temperature
To be dried under the conditions of 105~110 DEG C to constant weight, discharging, refined electrolyte is obtained, it is standby；
（4）600~800g ethylene carbonates are sequentially added in there-necked flask, 400~600g Allyl carbonaties, 30~50g receives
Rice titanium dioxide, then flask is placed in sonic oscillation instrument, it is 45~50 DEG C in temperature, frequency is under the conditions of 40~60KHz, to surpass
45~60min of sound oscillation, treats that ultrasound terminates, and there-necked flask is removed, with uviol lamp with 80~120W power prolonged exposure 3~
5h, in irradiation process, with 3~5mL/min speed chlorine is passed through in there-necked flask, and end to be illuminated, stopping is passed through chlorine,
And nitrogen is passed through in there-necked flask with 4~6mL/min speed, and until displacing all chlorine, filter, collect to obtain filtrate；
（5）Count by weight, 100~120 parts of above-mentioned gained filtrates, 20~30 parts of steps are sequentially added in batch mixer（3）
Standby refined electrolyte, in temperature be 55~60 DEG C, rotating speed be 600~800r/min under the conditions of, constant temperature stirring mixing 45~
60min, after naturally cool to room temperature, discharging, fill obtains final product high-temperature-reslithium lithium battery electrolyte.
The application process of the present invention：First in mass ratio 45:3:2:1, by LiFePO4, conductive agent Super P, poly- inclined two
After fluorothene and N-Methyl pyrrolidone mix homogeneously, it is placed in grinder and grinds, obtain A slurries, A slurries is evenly applied to
On aluminium foil, drying, to roller makes positive plate；Again in mass ratio 42:3:1, by Delanium, poly- inclined tetrafluoroethene, N- methyl
After ketopyrrolidine mix homogeneously, it is placed in grinder and grinds, obtain B slurries, B slurries is evenly applied on Copper Foil, drying,
To roller, negative plate is made, will be wound into shell after positive plate, barrier film, negative plate welding, resistance to height prepared by the present invention is injected in shell
Warm lithium battery electrolytes, the amount of injection preferably exceeds 7~8mm of pole plate, finally assembles, you can obtain lithium battery.After testing, using this
Lithium battery prepared by high-temperature-reslithium lithium battery electrolyte prepared by invention, can reach 670~750 charge and discharge cycles, in temperature
To work in 50~55 DEG C of environment, the discharge capacity of electrode reaches and do not found during 220~240mAh/g, and use drum
Phenomenon, thermal stability is superior.
Compared with additive method, Advantageous Effects are the present invention：
（1）The high-temperature-reslithium lithium battery electrolyte prepared using the present invention, extends the service life of lithium battery, can reach 670
~750 charge and discharge cycles；
（2）High-temperature-reslithium lithium battery electrolyte prepared by the present invention works in 50~55 DEG C of temperature environment so that lithium battery
The discharge capacity of electrode reaches 220~240mAh/g, improves its thermal stability.
Specific embodiment
Count by weight first, 25~35 parts of Lithium hydrates, 60~70 parts of boric acid, 3~5 part of five oxidation two are taken successively
Phosphorus, is 10 by ball material mass ratio in pouring ball grinder into:1~15:1 adds zirconium oxide ball milling pearl, after 2~4h of ball-milling treatment, goes out
Material, and material in ball grinder is pressed into into thickness as 0.6~0.8mm thin slices with 2~4MPa pressure；Above-mentioned gained thin slice is uniform
It is laid on wire gauze, and wire gauze is hung at 3~5cm of crucible top, then to adding above-mentioned Lithium hydrate in crucible
The oxalic acid that 6~8 times of quality, heating crucible makes crucible mesoxalic acid be warming up to 120~125 DEG C, and insulation distils completely up to oxalic acid,
The thin slice on wire gauze is collected, is poured into Jing after 5~10min of mortar grinder in crucible, and crucible is moved in baking oven, be in temperature
Under the conditions of 140~150 DEG C, 20~24h of insulation reaction, discharging, after naturally cool to room temperature, obtains crude product electrolyte；By above-mentioned institute
Obtain crude product electrolyte to pour in beaker, add the anhydrous acetonitrile of 4~6 times of crude product electrolyte quality, mixed with Glass rod stirring
After 20~30min, filter, collect filtrate, and gained filtrate is proceeded to into Rotary Evaporators, under the conditions of temperature is for 65~70 DEG C,
Concentrated by rotary evaporation obtains concentrated solution to the 1/10 of original volume, then gained concentrated solution is proceeded in baking oven, in temperature be 105~110 DEG C of bars
It is dried under part to constant weight, discharging, obtains refined electrolyte, it is standby；Sequentially add 600~800g ethylene carbonates in there-necked flask again
Ester, 400~600g Allyl carbonaties, 30~50g nano titanium oxides, then flask is placed in sonic oscillation instrument, it is in temperature
45~50 DEG C, frequency is that 45~60min of sonic oscillation treats that ultrasound terminates, and there-necked flask is removed under the conditions of 40~60KHz, is used
Uviol lamp in irradiation process, is led to 3~5mL/min speed with 80~120W power 3~5h of prolonged exposure in there-necked flask
Enter chlorine, end to be illuminated, stopping is passed through chlorine, and is passed through nitrogen in there-necked flask with 4~6mL/min speed, until putting
Swap out all chlorine, filters, and collects to obtain filtrate；Finally count by weight, sequentially add in batch mixer on 100~120 parts
State gained filtrate, 20~30 parts of standby refined electrolyte, in temperature be 55~60 DEG C, rotating speed be 600~800r/min under the conditions of,
Constant temperature stirring 45~60min of mixing, after naturally cool to room temperature, discharging, fill obtains final product high-temperature-reslithium lithium battery electrolyte.
Example 1
Count by weight first, take 35 parts of Lithium hydrates successively, 70 parts of boric acid, 5 parts of phosphorus pentoxides, in pouring ball grinder into,
It is 15 by ball material mass ratio:1 adds zirconium oxide ball milling pearl, after ball-milling treatment 4h, discharging, and by material in ball grinder with 4MPa pressures
Force and make thickness for 0.8mm thin slices；Above-mentioned gained thin slice is evenly laid out on wire gauze, and wire gauze is hung on into crucible
At the 5cm of top, then to the oxalic acid that 8 times of above-mentioned Lithium hydrate quality is added in crucible, heating crucible, crucible mesoxalic acid is set to heat up
To 125 DEG C, insulation distils completely up to oxalic acid, collects the thin slice on wire gauze, pours into Jing after mortar grinder 10min in crucible,
And crucible is moved in baking oven, under the conditions of temperature is for 150 DEG C, insulation reaction 24h, discharging, after naturally cool to room temperature, is obtained slightly
Product electrolyte；Above-mentioned gained crude product electrolyte is poured in beaker, the anhydrous acetonitrile of 6 times of crude product electrolyte quality is added, is used
After Glass rod stirring mixing 30min, filter, collect filtrate, and gained filtrate is proceeded to into Rotary Evaporators, in temperature be 70 DEG C of bars
Under part, the 1/10 of concentrated by rotary evaporation to original volume, obtain concentrated solution, then gained concentrated solution is proceeded in baking oven, in temperature be 110 DEG C of bars
It is dried under part to constant weight, discharging, obtains refined electrolyte, it is standby；Sequentially add 800g ethylene carbonates in there-necked flask again,
600g Allyl carbonaties, 50g nano titanium oxides, then flask is placed in sonic oscillation instrument, it is 50 DEG C in temperature, frequency is
Under the conditions of 40KHz, sonic oscillation 45min treats that ultrasound terminates, and there-necked flask is removed, with uviol lamp with 80W power prolonged exposures
3h, in irradiation process, with 3mL/min speed chlorine is passed through in there-necked flask, and end to be illuminated, stopping is passed through chlorine, and
Nitrogen is passed through in there-necked flask with 4mL/min speed, until displacing all chlorine, is filtered, collect to obtain filtrate；Finally by weight
Amount number meter, sequentially adds 100 parts of above-mentioned gained filtrates in batch mixer, 20 parts of standby refined electrolyte, in temperature be 55 DEG C,
Rotating speed is constant temperature stirring mixing 45min under the conditions of 600r/min, and after naturally cool to room temperature, discharging, fill obtains final product high temperature resistant
Lithium battery electrolytes.
First in mass ratio 45:3:2:1, by LiFePO4, conductive agent Super P, polyvinylidene fluoride and N- methylpyrroles
After alkanone mix homogeneously, it is placed in grinder and grinds, obtain A slurries, A slurries is evenly applied on aluminium foil, it is drying, right
Roller, makes positive plate；Again in mass ratio 42:3:1, by Delanium, poly- inclined tetrafluoroethene, N-Methyl pyrrolidone mix homogeneously
Afterwards, it is placed in grinder and grinds, obtain B slurries, B slurries are evenly applied on Copper Foil, drying, to roller makes negative plate,
To wind into shell after positive plate, barrier film, negative plate welding, high-temperature-reslithium lithium battery electrolyte prepared by the present invention injected in shell,
The amount of injection preferably exceeds pole plate 8mm, finally assembles, you can obtain lithium battery.After testing, the high temperature resistant lithium for being prepared using the present invention
Lithium battery prepared by battery electrolyte, can reach 750 charge and discharge cycles, work in the environment that temperature is 50 DEG C, electrode
Discharge capacity reach and do not found during 240mAh/g, and use drum phenomenon, thermal stability is superior.
Example 2
Count by weight first, take 35 parts of Lithium hydrates successively, 70 parts of boric acid, 5 parts of phosphorus pentoxides, in pouring ball grinder into,
It is 15 by ball material mass ratio:1 adds zirconium oxide ball milling pearl, after ball-milling treatment 4h, discharging, and by material in ball grinder with 4MPa pressures
Force and make thickness for 0.8mm thin slices；Above-mentioned gained thin slice is evenly laid out on wire gauze, and wire gauze is hung on into crucible
At the 5cm of top, then to the oxalic acid that 8 times of above-mentioned Lithium hydrate quality is added in crucible, heating crucible, crucible mesoxalic acid is set to heat up
To 125 DEG C, insulation distils completely up to oxalic acid, collects the thin slice on wire gauze, pours into Jing after mortar grinder 10min in crucible,
And crucible is moved in baking oven, under the conditions of temperature is for 150 DEG C, insulation reaction 24h, discharging, after naturally cool to room temperature, is obtained slightly
Product electrolyte；Above-mentioned gained crude product electrolyte is poured in beaker, the anhydrous acetonitrile of 6 times of crude product electrolyte quality is added, is used
After Glass rod stirring mixing 30min, filter, collect filtrate, and gained filtrate is proceeded to into Rotary Evaporators, in temperature be 70 DEG C of bars
Under part, the 1/10 of concentrated by rotary evaporation to original volume, obtain concentrated solution, then gained concentrated solution is proceeded in baking oven, in temperature be 110 DEG C of bars
It is dried under part to constant weight, discharging, obtains refined electrolyte, it is standby；Sequentially add 800g ethylene carbonates in there-necked flask again,
600g Allyl carbonaties, 50g nano titanium oxides, then flask is placed in sonic oscillation instrument, it is 50 DEG C in temperature, frequency is
Under the conditions of 60KHz, sonic oscillation 60min treats that ultrasound terminates, and there-necked flask is removed, with uviol lamp with 120W power persistently according to
5h is penetrated, in irradiation process, chlorine is passed through in there-necked flask with 5mL/min speed, end to be illuminated, stopping is passed through chlorine,
And nitrogen is passed through in there-necked flask with 6mL/min speed, and until displacing all chlorine, filter, collect to obtain filtrate；Finally press
Parts by weight meter, sequentially adds 120 parts of above-mentioned gained filtrates in batch mixer, 30 parts of standby refined electrolyte, in temperature be 60
DEG C, rotating speed is constant temperature stirring mixing 60min under the conditions of 800r/min, and after naturally cool to room temperature, discharging, fill obtains final product resistance to height
Warm lithium battery electrolytes.
First in mass ratio 45:3:2:1, by LiFePO4, conductive agent Super P, polyvinylidene fluoride and N- methylpyrroles
After alkanone mix homogeneously, it is placed in grinder and grinds, obtain A slurries, A slurries is evenly applied on aluminium foil, it is drying, right
Roller, makes positive plate；Again in mass ratio 42:3:1, by Delanium, poly- inclined tetrafluoroethene, N-Methyl pyrrolidone mix homogeneously
Afterwards, it is placed in grinder and grinds, obtain B slurries, B slurries are evenly applied on Copper Foil, drying, to roller makes negative plate,
To wind into shell after positive plate, barrier film, negative plate welding, high-temperature-reslithium lithium battery electrolyte prepared by the present invention injected in shell,
The amount of injection preferably exceeds pole plate 7mm, finally assembles, you can obtain lithium battery.After testing, the high temperature resistant lithium for being prepared using the present invention
Lithium battery prepared by battery electrolyte, can reach 670 charge and discharge cycles, work in the environment that temperature is 55 DEG C, electrode
Discharge capacity reach and do not found during 220mAh/g, and use drum phenomenon, thermal stability is superior.
Example 3
Count by weight first, take 30 parts of Lithium hydrates successively, 65 parts of boric acid, 4 parts of phosphorus pentoxides, in pouring ball grinder into,
It is 12 addition zirconium oxide ball milling pearls by ball material mass ratio, after ball-milling treatment 3h, discharging, and by material in ball grinder with 3MPa pressure
Thickness is pressed into for 0.7mm thin slices；Above-mentioned gained thin slice is evenly laid out on wire gauze, and wire gauze is hung on crucible
At square 4cm, then to the oxalic acid that 7 times of above-mentioned Lithium hydrate quality is added in crucible, heating crucible, it is warming up to crucible mesoxalic acid
122 DEG C, insulation distils completely up to oxalic acid, collects the thin slice on wire gauze, pours in crucible Jing after mortar grinder 7min, and will
Crucible is moved in baking oven, and under the conditions of temperature is for 145 DEG C, insulation reaction 22h, discharging, after naturally cool to room temperature, obtains crude product electricity
Xie Zhi；Above-mentioned gained crude product electrolyte is poured in beaker, the anhydrous acetonitrile of 5 times of crude product electrolyte quality is added, glass is used
After rod stirring mixing 25min, filter, collect filtrate, and gained filtrate is proceeded to into Rotary Evaporators, in temperature be 67 DEG C of conditions
Under, the 1/10 of concentrated by rotary evaporation to original volume, obtain concentrated solution, then gained concentrated solution is proceeded in baking oven, in temperature be 107 DEG C of conditions
Lower drying obtains refined electrolyte to constant weight, discharging, standby；Sequentially add 700g ethylene carbonates, 500g in there-necked flask again
Allyl carbonate, 40g nano titanium oxides, then flask is placed in sonic oscillation instrument, it is 47 DEG C in temperature, frequency is 50KHz
Under the conditions of, sonic oscillation 50min treats that ultrasound terminates, and there-necked flask is removed, with uviol lamp with 100W power prolonged exposure 4h,
In irradiation process, chlorine is passed through in there-necked flask with 4mL/min speed, end to be illuminated, stopping is passed through chlorine, and with
5mL/min speed is passed through nitrogen in there-necked flask, until displacing all chlorine, filters, and collects to obtain filtrate；By weight finally
Number meter, sequentially adds 110 parts of above-mentioned gained filtrates in batch mixer, and 25 parts of standby refined electrolyte are 57 DEG C in temperature, are turned
Speed is under the conditions of 700r/min, constant temperature stirring mixing 50min, after naturally cool to room temperature, discharges, and fill obtains final product high temperature resistant lithium
Battery electrolyte.
First in mass ratio 45:3:2:1, by LiFePO4, conductive agent Super P, polyvinylidene fluoride and N- methylpyrroles
After alkanone mix homogeneously, it is placed in grinder and grinds, obtain A slurries, A slurries is evenly applied on aluminium foil, it is drying, right
Roller, makes positive plate；Again in mass ratio 42:3:1, by Delanium, poly- inclined tetrafluoroethene, N-Methyl pyrrolidone mix homogeneously
Afterwards, it is placed in grinder and grinds, obtain B slurries, B slurries are evenly applied on Copper Foil, drying, to roller makes negative plate,
To wind into shell after positive plate, barrier film, negative plate welding, high-temperature-reslithium lithium battery electrolyte prepared by the present invention injected in shell,
The amount of injection preferably exceeds pole plate 7mm, finally assembles, you can obtain lithium battery.After testing, the high temperature resistant lithium for being prepared using the present invention
Lithium battery prepared by battery electrolyte, can reach 700 charge and discharge cycles, work in the environment that temperature is 52 DEG C, electrode
Discharge capacity reach and do not found during 230mAh/g, and use drum phenomenon, thermal stability is superior.
Claims (1)
1. a kind of preparation method of high-temperature-reslithium lithium battery electrolyte, it is characterised in that concrete preparation process is：
（1）Count by weight, 25~35 parts of Lithium hydrates are taken successively, 60~70 parts of boric acid, 3~5 parts of phosphorus pentoxides are poured into
It is 10 by ball material mass ratio in ball grinder:1~15:1 adds zirconium oxide ball milling pearl, after 2~4h of ball-milling treatment, discharging, and by ball
Material is pressed into thickness as 0.6~0.8mm thin slices with 2~4MPa pressure in grinding jar；
（2）Above-mentioned gained thin slice is evenly laid out on wire gauze, and wire gauze is hung at 3~5cm of crucible top, subsequently
The oxalic acid of 6~8 times of above-mentioned Lithium hydrate quality, heating crucible is added to make crucible mesoxalic acid be warming up to 120~125 in crucible
DEG C, insulation distils completely up to oxalic acid, collects the thin slice on wire gauze, pours in crucible Jing after 5~10min of mortar grinder, and
Crucible is moved in baking oven, under the conditions of temperature is for 140~150 DEG C, 20~24h of insulation reaction, discharging, after naturally cool to room
Temperature, obtains crude product electrolyte；
（3）Above-mentioned gained crude product electrolyte is poured in beaker, the anhydrous acetonitrile of 4~6 times of crude product electrolyte quality is added, is used
After Glass rod stirring 20~30min of mixing, filter, collect filtrate, and gained filtrate is proceeded to into Rotary Evaporators, in temperature be 65
Under the conditions of~70 DEG C, the 1/10 of concentrated by rotary evaporation to original volume, concentrated solution is obtained, then gained concentrated solution is proceeded in baking oven, in temperature
To be dried under the conditions of 105~110 DEG C to constant weight, discharging, refined electrolyte is obtained, it is standby；
（4）600~800g ethylene carbonates are sequentially added in there-necked flask, 400~600g Allyl carbonaties, 30~50g receives
Rice titanium dioxide, then flask is placed in sonic oscillation instrument, it is 45~50 DEG C in temperature, frequency is under the conditions of 40~60KHz, to surpass
45~60min of sound oscillation, treats that ultrasound terminates, and there-necked flask is removed, with uviol lamp with 80~120W power prolonged exposure 3~
5h, in irradiation process, with 3~5mL/min speed chlorine is passed through in there-necked flask, and end to be illuminated, stopping is passed through chlorine,
And nitrogen is passed through in there-necked flask with 4~6mL/min speed, and until displacing all chlorine, filter, collect to obtain filtrate；
（5）Count by weight, 100~120 parts of above-mentioned gained filtrates, 20~30 parts of steps are sequentially added in batch mixer（3）
Standby refined electrolyte, in temperature be 55~60 DEG C, rotating speed be 600~800r/min under the conditions of, constant temperature stirring mixing 45~
60min, after naturally cool to room temperature, discharging, fill obtains final product high-temperature-reslithium lithium battery electrolyte.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019000583A1 (en) * | 2017-06-29 | 2019-01-03 | 谭柳 | Lithium battery electrolyte |
| CN114160291A (en) * | 2021-11-15 | 2022-03-11 | 广东派勒智能纳米科技股份有限公司 | Preparation method of lithium battery conductive agent |
| CN114773371A (en) * | 2022-05-30 | 2022-07-22 | 无锡威孚环保催化剂有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN115477632A (en) * | 2022-08-30 | 2022-12-16 | 惠州市宙邦化工有限公司 | Method for purifying ethylene carbonate |
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| US7172834B1 (en) * | 2002-07-29 | 2007-02-06 | The United States Of America As Represented By The Secretary Of The Army | Additive for enhancing the performance of electrochemical cells |
| CN100426582C (en) * | 2004-03-30 | 2008-10-15 | 三星Sdi株式会社 | Electrolyte for lithium battery and lithium battery comprising the same |
| CN101789520A (en) * | 2009-01-23 | 2010-07-28 | 索尼公司 | Electrolyte and secondary cell |
| EP3041078A1 (en) * | 2013-08-30 | 2016-07-06 | UBE Industries, Ltd. | Nonaqueous electrolyte solution for electricity storage devices |
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| US7172834B1 (en) * | 2002-07-29 | 2007-02-06 | The United States Of America As Represented By The Secretary Of The Army | Additive for enhancing the performance of electrochemical cells |
| CN100426582C (en) * | 2004-03-30 | 2008-10-15 | 三星Sdi株式会社 | Electrolyte for lithium battery and lithium battery comprising the same |
| CN101789520A (en) * | 2009-01-23 | 2010-07-28 | 索尼公司 | Electrolyte and secondary cell |
| EP3041078A1 (en) * | 2013-08-30 | 2016-07-06 | UBE Industries, Ltd. | Nonaqueous electrolyte solution for electricity storage devices |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019000583A1 (en) * | 2017-06-29 | 2019-01-03 | 谭柳 | Lithium battery electrolyte |
| CN114160291A (en) * | 2021-11-15 | 2022-03-11 | 广东派勒智能纳米科技股份有限公司 | Preparation method of lithium battery conductive agent |
| CN114773371A (en) * | 2022-05-30 | 2022-07-22 | 无锡威孚环保催化剂有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN115477632A (en) * | 2022-08-30 | 2022-12-16 | 惠州市宙邦化工有限公司 | Method for purifying ethylene carbonate |
| CN115477632B (en) * | 2022-08-30 | 2023-11-03 | 惠州市宙邦化工有限公司 | Purification method of ethylene carbonate |
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