CN104201416B - A kind of high voltage lithium ion battery functional electrolyte and preparation method and application - Google Patents
A kind of high voltage lithium ion battery functional electrolyte and preparation method and application Download PDFInfo
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- CN104201416B CN104201416B CN201410419347.XA CN201410419347A CN104201416B CN 104201416 B CN104201416 B CN 104201416B CN 201410419347 A CN201410419347 A CN 201410419347A CN 104201416 B CN104201416 B CN 104201416B
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- H—ELECTRICITY
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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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- H—ELECTRICITY
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Abstract
The invention belongs to field of lithium ion battery, disclose a kind of high voltage lithium ion battery functional electrolyte and preparation method and application.Described high voltage lithium ion battery functional electrolyte adds functional additive glutaric anhydride in traditional lithium-ion battery electrolyte and obtains；Wherein general electrolytic liquid is made up of cyclic carbonate solvents, linear carbonates solvent and electric conducting lithium salt.The functional additive that the present invention uses is in the discharge and recharge system of 3～5.0V; one layer of more stable film with protective value the thinnest is formed at positive electrode surface; on the one hand the oxidation Decomposition of electrolyte under high voltage is inhibited; on the other hand protection positive electrode, thus improve cycle performance and the security performance of high-voltage lithium ion batteries.
Description
Technical field
The invention belongs to field of lithium ion battery, be specifically related to a kind of high voltage lithium ion battery functional electrolyte
And preparation method and application.
Background technology
The advantage that lithium ion battery has that energy density is big, running voltage is high and has extended cycle life etc..Currently
The positive electrode of business lithium ion battery has LiMn2O4, cobalt acid lithium, LiFePO4, ternary material, and these are several,
Charge cutoff voltage is typically no more than 4.2V, along with progress and the development in market of science and technology, promotes lithium
The energy density of battery seems important and urgent day by day.Except current material and battery production technology improvement it
Outward, high voltage (> 4.5V) positive electrode is one of popular research direction of comparison, mainly by just promoting
The depth of charge of pole active material realizes the high-energy-density of battery.
But, improving while positive electrode voltage, the performance such as the charge and discharge cycles of battery is but declining, and one
Aspect reason positive electrode is not sufficiently stable, and is on the other hand i.e. the matching problem of electrolyte, and general electrolytic liquid exists
High voltage (> 4.5V) under can be in positive electrode surface generation oxidation Decomposition, the oxidative decomposition of electrolyte is the most also
The destruction of positive electrode can be promoted.So, developing high voltage withstanding electrolyte has important actual application valency
Value.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the primary and foremost purpose of the present invention is to provide a kind of high voltage
Lithium ion battery function electrolyte；
Another object of the present invention is to provide the preparation side of above-mentioned high voltage lithium ion battery functional electrolyte
Method；
It is still another object of the present invention to provide the application of above-mentioned high voltage lithium ion battery functional electrolyte.
The purpose of the present invention is achieved through the following technical solutions:
A kind of high voltage lithium ion battery functional electrolyte, including traditional lithium-ion battery electrolyte, described often
Rule lithium-ion battery electrolytes is made up of cyclic carbonate solvents, linear carbonates solvent and electric conducting lithium salt；Also
Including functional additive, described functional additive is glutaric anhydride.
Described traditional lithium-ion battery electrolyte can be prepared according to the conventional constituents of state of the art and method
Obtain.
Preferably, the addition of described functional additive is equivalent to described traditional lithium-ion battery electrolyte quality
1%～5%；
Preferably, in described traditional lithium-ion battery electrolyte, cyclic carbonate solvents and linear carbonates are molten
The mass ratio of agent is (1:3)～(3:2)；Electric conducting lithium salt end in described traditional lithium-ion battery electrolyte
Concentration is 0.8～1.2mol/L；
Preferably, described cyclic carbonate solvents is ethylene carbonate (EC)；
Preferably, described linear carbonates solvent be dimethyl carbonate (DMC), Ethyl methyl carbonate (EMC),
At least one in diethyl carbonate (DEC) or methyl propyl carbonate (MPC)；
Preferably, described electric conducting lithium salt is LiPF6、LiBOB、LiSO3CF3、LiClO4、LiAsF6、
Li(CF3SO2)2N or LiC (CF3SO2)3In at least one.
The preparation method of above-mentioned high voltage lithium ion battery functional electrolyte, comprises the steps:
(1) cyclic carbonate solvents and linear carbonates solvent are mixed, clarification, except water, mixed
Bonding solvent；At ambient temperature, electric conducting lithium salt is added in described mixed solvent, stirs, often obtain
Rule lithium-ion battery electrolytes；
(2) in the traditional lithium-ion battery electrolyte that step (1) obtains, add functional additive, obtain
High voltage lithium ion battery functional electrolyte；Described functional additive is glutaric anhydride.
Preferably, the cyclic carbonate solvents described in step (1) and the matter of described linear carbonates solvent
Amount ratio is (1:3)～(3:2)；
Preferably, the cyclic carbonate solvents described in step (1) is ethylene carbonate (EC)；
Preferably, the linear carbonates solvent described in step (1) is dimethyl carbonate (DMC), carbonic acid
At least one in methyl ethyl ester (EMC), diethyl carbonate (DEC) or methyl propyl carbonate (MPC)；
Preferably, the final concentration in traditional lithium-ion battery electrolyte of the electric conducting lithium salt described in step (1)
It is 0.8～1.2mol/L；
Preferably, the electric conducting lithium salt described in step (1) is LiPF6、LiBOB、LiSO3CF3、LiClO4、
LiAsF6、Li(CF3SO2)2N or LiC (CF3SO2)3In at least one；
Preferably, the clarification described in step (1), except water by molecular sieve, activated carbon, calcium hydride,
Any one in lithium hydride, anhydrous calcium oxide, calcium chloride, phosphorus pentoxide, alkali metal or alkaline-earth metal
Plant or at least two processes；
Preferably, the molecular sieve described in step (1) usesOrType；
Preferably, room temperature described in step (1) is in the range of 25～40 DEG C；
Preferably, the addition of functional additive shown in step (2) is equivalent to traditional lithium-ion battery electrolysis
The 1%～5% of liquid quality.
Described high voltage lithium ion battery functional electrolyte is applied to manufacture lithium ion battery.The lithium of gained from
Sub-battery has good charge-discharge performance.
The present invention has such advantages as relative to prior art and effect:
The functional additive that the present invention uses is in the discharge and recharge system of 3～5.0V, and contrast conventional lithium ion is electric
Pond electrolyte, it is possible to form one layer of more stable film with protective value the thinnest at positive electrode surface, by this layer
Film, restrained effectively electrolyte solvent component oxidation Decomposition further under high voltage, and in certain journey
Decreasing the dissolution phenomenon of positive electrode on degree, to a certain degree Shangdi protects positive electrode, thus improves
The cycle performance of high-voltage lithium ion batteries and security performance.
Accompanying drawing explanation
Fig. 1 is the line of the V-type electrolysis bath of the electrolyte making that the embodiment of the present invention 1 is prepared with comparative example
Property scanning comparison diagram.
Fig. 2 is the lithium ion battery circulation of the electrolyte making that the embodiment of the present invention 1 is prepared with comparative example
The discharge and recharge comparison diagram of 300 circles.
Fig. 3 is the lithium ion battery circulation of the electrolyte making that the embodiment of the present invention 1 is prepared with comparative example
AC impedance comparison diagram after 200 circles.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention
It is not limited to this.
Embodiment 1
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent dimethyl carbonate
(DMC) mixing of EC:DMC=1:1 in mass ratio, and useMolecular sieve, calcium hydride, lithium hydride are pure
Eliminate miscellaneous, except water, obtain mixed solvent；Under the conditions of room temperature 25 DEG C, by electric conducting lithium salt LiPF6It is dissolved in institute
State in mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 1.0mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 2%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 2
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent dimethyl carbonate
(DMC) mix according to mass ratio EC:DMC=1:2, and useMolecular sieve, calcium hydride, lithium hydride
Clarification, except water, obtain mixed solvent；Under the conditions of room temperature 28 DEG C, by electric conducting lithium salt LiPF6It is dissolved in
In described mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 0.8mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 1%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 3
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent dimethyl carbonate
(DMC) mixing of EC:DMC=1:3 in mass ratio, and useMolecular sieve, calcium hydride, lithium hydride are pure
Eliminate miscellaneous, except water, obtain mixed solvent；Under the conditions of room temperature 28 DEG C, by electric conducting lithium salt LiPF6It is dissolved in institute
State in mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 1.0mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 1%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 4
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate
(EMC) mix according to mass ratio EC:EMC=1:2, and useMolecular sieve, calcium hydride, lithium hydride
Clarification, except water, obtain mixed solvent；Under the conditions of room temperature 30 DEG C, by electric conducting lithium salt LiPF6It is dissolved in
In described mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 1.0mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 1%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 5
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate
(EMC) mix according to mass ratio EC:EMC=1:1, and useMolecular sieve, calcium hydride, lithium hydride
Clarification, except water, obtain mixed solvent；Under the conditions of room temperature 25 DEG C, by electric conducting lithium salt LiPF6It is dissolved in
In described mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 0.8mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 2%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 6
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent dimethyl carbonate
(DMC) mix according to mass ratio EC:DMC=3:2, and useMolecular sieve, calcium hydride, lithium hydride
Clarification, except water, obtain mixed solvent；Under the conditions of room temperature 35 DEG C, by electric conducting lithium salt LiPF6It is dissolved in
In described mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 1.0mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 1%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 7
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent Ethyl methyl carbonate
(EMC) mix according to mass ratio EC:EMC=3:2, and useMolecular sieve, calcium hydride, lithium hydride
Clarification, except water, obtain mixed solvent；Under the conditions of room temperature 40 DEG C, by electric conducting lithium salt LiPF6It is dissolved in
In described mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 0.8mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 2%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Embodiment 8
A kind of high voltage lithium ion battery functional electrolyte, its preparation method is as follows:
(1) by cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent dimethyl carbonate
(DMC) mix according to mass ratio EC:DMC=1:2, and useMolecular sieve, calcium hydride, lithium hydride
Clarification, except water, obtain mixed solvent；Under the conditions of room temperature 25 DEG C, by electric conducting lithium salt LiPF6It is dissolved in
In described mixed solvent, stir, obtain traditional lithium-ion battery electrolyte；Wherein, electric conducting lithium salt LiPF6
Final concentration of 1.2mol/L in traditional lithium-ion battery electrolyte；
(2) in traditional lithium-ion battery electrolyte prepared by step (1), glutaric anhydride, glutaric anhydride are added
Consumption is traditional lithium-ion battery electrolyte quality 5%, obtain described high-voltage lithium ion batteries function electricity
Solve liquid.
Comparative example
A kind of lithium-ion battery electrolytes, its preparation method is as follows:
By cyclic carbonate solvents ethylene carbonate (EC) and linear carbonates solvent dimethyl carbonate (DMC)
EC:DMC=1:1 in mass ratio mixes, and usesMolecular sieve, calcium hydride, lithium hydride clarification,
Except water, obtain mixed solvent；Under the conditions of room temperature 25 DEG C, by electric conducting lithium salt LiPF6It is dissolved in described mixing molten
In agent, electric conducting lithium salt LiPF6Final concentration of 1.0mol/L, stir, obtain described lithium ion battery battery
Solve liquid.
Effectiveness comparison:
Lithium ion prepared by high voltage lithium ion battery functional electrolyte embodiment 1 prepared and comparative example
Battery electrolyte compares:
(1) the V-type electrolysis bath that Fig. 1 electrolyte that to be embodiment 1 prepare with comparative example makes is linear
Scanning comparison diagram.Method of testing is: work electrode with platinum disk electrode, and lithium sheet does electrode, adds embodiment
Lithium-ion battery electrolytes prepared by the high voltage lithium ion battery functional electrolyte of 1 preparation or comparative example is each
2ml, then carries out linear scanning electro-chemical test at Solartron-1470 (Britain) multi-channel analyzer.With
The scanning speed of 1mV/s sweeps to 6V from OCP.Fig. 1 shows high-voltage lithium ion electricity prepared by embodiment 1
Pond function electrolyte occurs in that oxidation current at about 4.1V, and the lithium-ion battery electrolytes of comparative example
The oxidation current of correspondence is not had at about 4.1V, and about after 4.8V, the height of embodiment 1 preparation
Voltage lithium ion battery function electrolyte oxidation current under high potential is significantly less than comparative example, illustrates penta
Dicarboxylic anhydride can preferentially aoxidize at positive electrode surface, forms layer protecting film, thus suppress carbonate solvent enter one
Step oxidation Decomposition.
(2) Fig. 2 is high voltage lithium ion battery functional electrolyte and the comparative example of the embodiment of the present invention 1
The discharge and recharge comparison diagram of lithium ion battery circulation 300 circle that the lithium-ion battery electrolytes of preparation makes respectively.Survey
Method for testing is: work electrode with nickel ion doped, and lithium sheet does electrode, adds the height that embodiment 1 prepares
The lithium-ion battery electrolytes each 30 that voltage lithium ion battery function electrolyte or comparative example prepare
μ L, carries out charge-discharge test blue electrical testing system (Chinese) after being then assembled into battery.Room temperature 25 DEG C
Under, between 3～5.0V scopes, after charge and discharge cycles 300 circle, measure charge and discharge electrical with the charge and discharge multiplying power of 0.5C
Energy.As shown in Figure 2, after circulation 300 circle, embodiment 1 compares comparative example has preferably circulation steady
Qualitative.
(3) Fig. 3 is high voltage lithium ion battery functional electrolyte and the comparative example of the embodiment of the present invention 1
AC impedance contrast after lithium ion battery circulation 300 circle that the lithium-ion battery electrolytes of preparation makes respectively
Figure.Method of testing is: work electrode with nickel ion doped, and lithium sheet does electrode, adds embodiment 1 and is prepared into
To high voltage lithium ion battery functional electrolyte or the lithium-ion battery electrolytes for preparing of comparative example
Each 30 μ L, carry out ac impedance measurement at Autolab (Dutch) electrochemical workstation after being then assembled into battery.
At room temperature 25 DEG C, after charge and discharge cycles 300 circle, survey between 3～5.0V scopes with the charge and discharge multiplying power of 0.5C
The change of fixed electrode surface impedance.From the figure 3, it may be seen that the high-voltage lithium ion batteries merit that embodiment 1 prepares
The lithium-ion battery electrolytes that the impedance ratio comparative example of the cathode film that energy electrolyte is formed obtains just is being formed
The impedance of pole film is little, further illustrates glutaric anhydride and can form densification, stable cathode film at positive electrode surface.
Through same comparison and detection, the performance of the high voltage lithium ion battery functional electrolyte of embodiment 2～8 gained
It is superior to the lithium-ion battery electrolytes of comparative example.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-mentioned enforcement
The restriction of example, the change made, modifies, replaces under other any spirit without departing from the present invention and principle
In generation, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (9)
1. a high voltage lithium ion battery functional electrolyte, including traditional lithium-ion battery electrolyte, institute
State traditional lithium-ion battery electrolyte to be made up of cyclic carbonate solvents, linear carbonates solvent and electric conducting lithium salt；
It is characterized in that: also include that functional additive, described functional additive are glutaric anhydride；Described function is added
The addition of agent is equivalent to described traditional lithium-ion battery electrolyte quality 1%～5%.
A kind of high voltage lithium ion battery functional electrolyte the most according to claim 1, its feature exists
In: in described traditional lithium-ion battery electrolyte, cyclic carbonate solvents and the quality of linear carbonates solvent
Than being (1:3)～(3:2)；Electric conducting lithium salt in described traditional lithium-ion battery electrolyte final concentration of 0.8～
1.2mol/L。
A kind of high voltage lithium ion battery functional electrolyte the most according to claim 1, it is characterised in that:
Described cyclic carbonate solvents is ethylene carbonate；Described linear carbonates solvent be dimethyl carbonate,
At least one in Ethyl methyl carbonate, diethyl carbonate or methyl propyl carbonate；Described electric conducting lithium salt is LiPF6、
LiBOB、LiSO3CF3、LiClO4、LiAsF6、Li(CF3SO2)2N or LiC (CF3SO2)3In
At least one.
4. according to the preparation side of the high voltage lithium ion battery functional electrolyte described in any one of claims 1 to 3
Method, it is characterised in that comprise the steps:
(1) cyclic carbonate solvents and linear carbonates solvent are mixed, clarification, except water, mixed
Bonding solvent；At ambient temperature, electric conducting lithium salt is added in described mixed solvent, stirs, often obtain
Rule lithium-ion battery electrolytes；
(2) in the traditional lithium-ion battery electrolyte that step (1) obtains, add functional additive, obtain
High voltage lithium ion battery functional electrolyte；Described functional additive is glutaric anhydride.
Preparation method the most according to claim 4, it is characterised in that: cyclic carbonate in step (1)
The mass ratio of ester solvent and linear carbonates solvent is (1:3)～(3:2)；Described electric conducting lithium salt described often
In rule lithium-ion battery electrolytes final concentration of 0.8～1.2mol/L.
6. according to the preparation method described in claim 4 or 5, it is characterised in that: described in step (1)
Cyclic carbonate solvents be ethylene carbonate；Linear carbonates solvent described in step (1) is carbonic acid two
At least one in methyl ester, Ethyl methyl carbonate, diethyl carbonate or methyl propyl carbonate；Described in step (1)
Electric conducting lithium salt be LiPF6、LiBOB、LiSO3CF3、LiClO4、LiAsF6、Li(CF3SO2)2N or
LiC(CF3SO2)3In at least one.
Preparation method the most according to claim 4, it is characterised in that: pure described in step (1)
Eliminate miscellaneous, except water by molecular sieve, activated carbon, calcium hydride, lithium hydride, anhydrous calcium oxide, calcium chloride,
Any one or at least two in phosphorus pentoxide, alkali metal or alkaline-earth metal process；Described
Molecular sieve useOrType；
Described in step (1), room temperature is in the range of 25～40 DEG C.
Preparation method the most according to claim 4, it is characterised in that: function described in step (2)
The addition of additive is equivalent to the 1%～5% of traditional lithium-ion battery electrolyte quality.
9. manufacturing lithium according to the high voltage lithium ion battery functional electrolyte described in any one of claims 1 to 3
Application in ion battery.
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| CN1595711A (en) * | 2003-09-09 | 2005-03-16 | 三洋电机株式会社 | Non-aqueous solvent secondary battery |
| CN101783526A (en) * | 2010-01-31 | 2010-07-21 | 黄宇嵩 | Electronic switching unit without energy consumption for standby power supply of model airplane receiver |
| CN103928707A (en) * | 2014-05-07 | 2014-07-16 | 华南师范大学 | High voltage lithium ion battery functional electrolyte and preparation method and application |
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| CN1595711A (en) * | 2003-09-09 | 2005-03-16 | 三洋电机株式会社 | Non-aqueous solvent secondary battery |
| CN101783526A (en) * | 2010-01-31 | 2010-07-21 | 黄宇嵩 | Electronic switching unit without energy consumption for standby power supply of model airplane receiver |
| CN103928707A (en) * | 2014-05-07 | 2014-07-16 | 华南师范大学 | High voltage lithium ion battery functional electrolyte and preparation method and application |
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Effective date of registration: 20191213 Address after: 400802 Yutianbao group, Pingshan Industrial Park, Wansheng Economic Development Zone, Chongqing Patentee after: Chongqing Guanyu Battery Co., Ltd Address before: 510006 , Guangzhou, Panyu District, Guangzhou University, 378 West Ring Road, South China Normal University Patentee before: South China Normal University |