CN106711503A - Single-ion gel polymer electrolyte and preparation method thereof - Google Patents
Single-ion gel polymer electrolyte and preparation method thereof Download PDFInfo
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- CN106711503A CN106711503A CN201611173765.0A CN201611173765A CN106711503A CN 106711503 A CN106711503 A CN 106711503A CN 201611173765 A CN201611173765 A CN 201611173765A CN 106711503 A CN106711503 A CN 106711503A
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- lithium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to single-ion gel polymer electrolyte and a preparation method thereof. The preparation method is characterized by comprising the following steps: firstly, selecting double-bond sulfonate and preparing double-bond lithium sulfonate by utilizing the characteristic that sodium sulfate is not dissolved into absolute ethyl alcohol; preparing the double-bond lithium sulfonate into a single-ion gel polymer base body, wherein the mol ratio of an added monomer to a carbon-carbon double bond in the lithium sulfonate ranges from (10 to 1) to (1 to 10), a catalyst is 2,2'-azobis(2-methylpropionitrile) with the concentration of 2wt%, and a solvent is toluene; reacting at 70 DEG C-80 DEG C for 7h-12h; and taking the prepared polymer as a base body and preparing the single-ion gel polymer electrolyte, wherein the adding amounts of the polymer and the organic solvent, and liquid electrolyte are 1g-3g and 20ml-50ml respectively. The single-ion gel polymer electrolyte has the beneficial effects that the transport number of lithium ions of the electrolyte is improved through introducing the lithium ions into the polymer in a chemical bond connecting manner, so that the possibility is provided for further improving the energy density of a lithium-ion battery, and a certain foundation is laid for application of the gel polymer electrolyte in actual production.
Description
Technical field
The present invention relates to single ion gel polymer electrolyte and preparation method thereof, belong to technical field of lithium ion.
Background technology
Currently, lithium ion battery has been achieved for tremendous development, in digital product, electric tool, the vehicles and illumination
It is widely applied Deng field.But, lithium ion battery still has the energy density endurance brought not high not strong
Weakness.Lithium ion battery the use of the lithium ion transference number of electrolyte is one of key factor for determining the energy content of battery.In order to carry
Lithium ion transference number in polyelectrolyte, most common method be increase electrolyte in add lithium salts anion volume,
Organic macroanion group lithium salts is such as introduced, this method achieves some effects to a certain extent really.However, these have
There is the lithium salts of big organic group but bring the not good problem of stable electrochemical property.In addition, gel polymer electrolyte
It is made up of polymeric matrix, plasticizer and the part of lithium salts three, is that a class has high ionic conductivity, high security and good electricity
The electrolyte of chemical property, is that lithium ion battery can obtain one of important support of great development.The present invention is poly- based on gel
The advantage of polymer electrolyte, while for this problem of raising electrolyte lithium-ion transport number, proposing in gel polymer electrolyte
Lithium ion is introduced with chemical bond form in polymeric matrix in matter, this method causes that polymeric matrix macromolecular chain becomes
Anionic group.The electrolyte diversion period of the day from 11 p.m. to 1 a.m, macromolecular chain anionic group obviously will not be migrated, therefore, lithium ion mobility
Number can access large increase.Correlative study is not appeared in also in report both at home and abroad.
The content of the invention
The technical problem to be solved
In order to improve the lithium ion transference number of gel polymer electrolyte, the present invention proposes single ion gelatin polymer electricity
Solution matter and preparation method thereof.
Technical scheme
Single ion gel polymer electrolyte and preparation method thereof, it is characterised in that：Comprise the following steps that：
(1) with the preparation of double bond sulfonic acid lithium salts：The water miscible sulfonate sodium with carbon-carbon double bond is weighed to pour into beaker, plus
Enter deionized water, be sufficiently stirred for, prepare sulfonate sodium saturated solution；Sulfuric acid solution of the configuration concentration in the range of 1-5mol/L；
Sulfuric acid solution is added in sulfonate sodium saturated solution, is stirred, it is ensured that the mol ratio of sodium ion and sulfate ion is 2
∶1；Then, the homogeneous solution that will be obtained is transferred in separatory funnel, from funnel square opening with glass bar drainage anhydrous ethanol solvent,
The characteristics of not dissolving in ethanol using sodium sulphate, sodium sulphate is precipitated out at water and ethanol intersection interface；By the water below funnel
Solution is released into beaker, then is transferred in separatory funnel, is precipitated with absolute ethyl alcohol.Operated more than repeating, sodium ion is gone completely
Remove, obtain the sulfonic acid aqueous solution；Anhydrous lithium hydroxide is added in the sulfonic acid aqueous solution, is stirred, until pH=7, rotary evaporation is gone out
Aqueous solvent, obtains band double bond Sulfonic Lithium salt powder.
(2) preparation of single-ion polymer matrix：By esters of acrylic acid, vinyl cyanide, vinylidene class, phosphonitrile class and vinegar
One or more mixing in vinyl acetate class monomer, are added to and dissolved in advance in the toluene solvant with double bond sulfonic acid lithium salts,
In addition monomer in carbon-carbon double bond and double bond sulfonic acid lithium salts carbon-carbon double bond mol ratio 10: within the scope of 1-1: 10, add anti-
Answer the catalyst azodiisobutyronitrile of thing gross mass 2wt.%, lead to nitrogen, at 70-80 DEG C in there-necked flask stirring reaction 7-
12h.The material that will be obtained is poured into the beaker equipped with deionized water, obtains light yellow latex shaped polymer precipitation.Again with toluene
Dissolving, deionized water are precipitated, and are repeated three times, obtain white latex shape solid.The solid crushed after being dried that will be obtained,
Deionized water is washed three times, is vacuum dried two days, obtains white powder.
(3) preparation of single ion gel polymer electrolyte：Prepared polymer is placed in weighing 1-3g above-mentioned steps (2)
In beaker, 20-50ml organic solvents are added, stirred to being completely dissolved, poured into Teflon dish, treat that organic solvent is complete
Transparent dura mater is obtained after volatilization, film is immersed in liquid electrolyte enough for a long time, obtain soft gel polymer dielectric
Film.
Described single ion gel polymer electrolyte and preparation method thereof, it is characterised in that：Described sulfonate sodium is
Sodium p styrene sulfonate, sodium vinyl sulfonate, sodium allylsulfonate, methylpropene sodium sulfonate, 2- acrylamido -2- methyl-prop sulphurs
The mixing of one or more of sour sodium.
Described single ion gel polymer electrolyte and preparation method thereof, it is characterised in that：Described organic solvent is
The mixing of one or more solution in acetone, tetrahydrofuran, DMF, dimethyl sulfoxide etc..
Described single ion gel polymer electrolyte and preparation method thereof, it is characterised in that：In the liquid electrolyte
Plasticizer be one kind in propene carbonate, ethylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate etc. or
Several mixing；Lithium salts in the liquid electrolyte is lithium perchlorate, lithium hexafluoro phosphate, LiBF4, trifluoromethyl sulphur
One or several mixing in sour lithium etc..
Beneficial effect
The beneficial effects of the invention are as follows introducing lithium ion on the polymeric matrix in gel polymer electrolyte and improve
The lithium ion transference number of electrolyte, this not only provides possibility, Er Qiewei further to improve the energy density of lithium ion battery
Certain basis is established in application of the gel polymer electrolyte in actual production.
Brief description of the drawings
Fig. 1 is P (MMA-SSS-Li) single ion gel polymer electrolyte film outside drawing.
Fig. 2 is P (MMA-SSS-Li) single ion gel polymer electrolyte films at 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C
With the AC impedance spectroscopy at a temperature of 50 DEG C.
Specific embodiment
The present invention is further illustrated with specific embodiment below in conjunction with the accompanying drawings：
Embodiment
(1) with the preparation of double bond sulfonic acid lithium salts：Water miscible sodium p styrene sulfonate (SSS) 0.05mol is weighed, burning is poured into
In cup, 40ml deionized waters are added, be sufficiently stirred for, prepare sulfonate sodium saturated solution；Sulphur in the range of configuration concentration 5mol/L
Acid solution 5ml；Sulfuric acid solution is added in sulfonate sodium saturated solution, is stirred, it is ensured that sodium ion and sulfate ion
Mol ratio be 2: 1；Then, the homogeneous solution that will be obtained is transferred in separatory funnel, from funnel square opening with glass bar drainage without
Alcoholic solvent, using sodium sulphate do not dissolve in ethanol the characteristics of, sodium sulphate is precipitated out at water and ethanol intersection interface；Will leakage
The aqueous solution below bucket is released into beaker, then is transferred in separatory funnel, is precipitated with absolute ethyl alcohol.Operated more than repeating, by sodium
Ion is removed completely, obtains the p styrene sulfonic acid aqueous solution；Anhydrous lithium hydroxide is added in the p styrene sulfonic acid aqueous solution, is stirred
Mix, until pH=7, rotary evaporation is gone out aqueous solvent, obtains p styrene sulfonic acid lithium (SSS-Li) powder.
(2) preparation of single-ion polymer matrix：Measure 6.7ml methyl methacrylates (MMA), weigh 4.13g to benzene
Vinyl sulfonic acid lithium (SSS-Li), azodiisobutyronitrile 0.01g, are placed in beaker, add 150ml toluene, stirring to fully it is molten
Solution is into clear solution；Solution is transferred in there-necked flask, 75 DEG C are heated to, is led to nitrogen, be stirred at reflux 8h；The material that will be obtained falls
Enter in the beaker equipped with deionized water, obtain light yellow latex shaped polymer precipitation.Again with toluene dissolving, deionized water are sunk
Form sediment, repeat three times, obtain white latex shape solid.The solid crushed after being dried that will be obtained, deionized water washing three times, very
Sky is dried two days, obtains poly- (methyl methacrylate-p styrene sulfonic acid lithium) (P (MMA-SSS-Li)) white powder.
(3) preparation of single ion gel polymer electrolyte：Weigh prepared polymer P (MMA- in 2g above-mentioned steps (2)
SSS-Li) it is placed in beaker, adds 40ml organic solvents, stir to being completely dissolved, pour into Teflon dish, treats organic
Solvent obtains transparent dura mater after volatilizing completely, film is immersed in liquid electrolyte enough for a long time, obtains soft gel polymerization
Thing electrolytic thin-membrane.
Test analysis are carried out to P (MMA-SSS-Li) single ion gel polymer electrolyte films prepared by embodiment, in
Carried out on the electrochemical workstation CHI-660D of Shanghai Chen Hua company of state.Ac impedance measurement condition is that the frequency range of scanning is
0.1Hz~100kHz, exchange signal amplitude is 10mV, and electrode is that two areas are 1cm2Stainless steel；Linear scan test-strips
Part is that the frequency range of scanning is 0.1Hz~100kHz, and the speed of scanning is 1mVs-1, negative pole is lithium piece, just extremely stainless
Steel；Lithium ion transference number test condition is AC impedance frequency separation 0.1Hz~100kHz, exchanges signal amplitude 10mV, direct current
The polarizing voltage for applying that polarizes is 10mV.The result of test is P (MMA-SSS-Li) single ion gel polymer electrolyte 25
DEG C, 30 DEG C, 35 DEG C, 40 DEG C, the ionic conductivity at a temperature of 45 DEG C and 50 DEG C be respectively 1.22 × 10-3S·cm-1、1.43×10-3S·cm-1、1.68×10-3S·cm-1、1.96×10-3S·cm-1、2.24×10-3S·cm-1With 2.69 × 10-3S·cm-1；
The electrochemical stability window of gel polymer electrolyte reaches 4.65V；Lithium ion transference number reaches 6.88.
Claims (4)
1. single ion gel polymer electrolyte and preparation method thereof, it is characterised in that：Comprise the following steps that：
(1) with the preparation of double bond sulfonic acid lithium salts：Weigh the water miscible sulfonate sodium with carbon-carbon double bond to pour into beaker, addition is gone
Ionized water, is sufficiently stirred for, and prepares sulfonate sodium saturated solution；Sulfuric acid solution of the configuration concentration in the range of 1-5mol/L；By sulphur
Acid solution is added in sulfonate sodium saturated solution, is stirred, it is ensured that the mol ratio of sodium ion and sulfate ion is 2: 1；
Then, the homogeneous solution that will be obtained is transferred in separatory funnel, and square opening is utilized with glass bar drainage anhydrous ethanol solvent from funnel
The characteristics of sodium sulphate does not dissolve in ethanol, sodium sulphate is precipitated out at water and ethanol intersection interface；By the aqueous solution below funnel
It is released into beaker, then is transferred in separatory funnel, is precipitated with absolute ethyl alcohol.Operated more than repeating, sodium ion is removed completely, obtained
To the sulfonic acid aqueous solution；Anhydrous lithium hydroxide is added in the sulfonic acid aqueous solution, is stirred, until pH=7, rotary evaporation is gone out water-soluble
Agent, obtains band double bond Sulfonic Lithium salt powder.
(2) preparation of single-ion polymer matrix：By esters of acrylic acid, vinyl cyanide, vinylidene class, phosphonitrile class and acetic acid second
One or more mixing in alkene esters monomer, are added to and dissolved in advance in the toluene solvant with double bond sulfonic acid lithium salts, addition
In monomer in carbon-carbon double bond and double bond sulfonic acid lithium salts carbon-carbon double bond mol ratio 10: within the scope of 1-1: 10, add reactant
The catalyst azodiisobutyronitrile of gross mass 2wt.%, lead to nitrogen, at 70-80 DEG C in there-necked flask stirring reaction 7-12h.Will
The material for obtaining is poured into the beaker equipped with deionized water, obtains light yellow latex shaped polymer precipitation.Again with toluene dissolves, goes
Ionized water is precipitated, and is repeated three times, obtains white latex shape solid.The solid crushed after being dried that will be obtained, deionization
Water washing three times, is vacuum dried two days, obtains white powder.
(3) preparation of single ion gel polymer electrolyte：Prepared polymer is placed in beaker in weighing 1-3g above-mentioned steps (2)
In, 20-50ml organic solvents are added, stir to being completely dissolved, pour into Teflon dish, treat that organic solvent volatilizees completely
Transparent dura mater is obtained afterwards, film is immersed in liquid electrolyte enough for a long time, obtain soft gel polymer electrolyte film.
2. single ion gel polymer electrolyte according to claim 1 and preparation method thereof, it is characterised in that：Described
Sulfonate sodium be sodium p styrene sulfonate, sodium vinyl sulfonate, sodium allylsulfonate, methylpropene sodium sulfonate, 2- acrylamidos-
The mixing of one or more of 2- methyl propane sulfonic acid sodium.
3. described single ion gel polymer electrolyte according to claim 1 and preparation method thereof, it is characterised in that：
Described organic solvent is one or more solution in acetone, tetrahydrofuran, DMF, dimethyl sulfoxide etc.
Mixing.
4. described single ion gel polymer electrolyte according to claim 1 and preparation method thereof, it is characterised in that：
Plasticizer in the liquid electrolyte is propene carbonate, ethylene carbonate, dimethyl carbonate, diethyl carbonate, carbonic acid first
The mixing of one or more in ethyl ester etc.；Lithium salts in the liquid electrolyte is lithium perchlorate, lithium hexafluoro phosphate, tetrafluoro boron
One or several mixing in sour lithium, trifluoromethyl sulfonic acid lithium etc..
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Cited By (3)
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| CN114335715A (en) * | 2021-12-31 | 2022-04-12 | 珠海冠宇电池股份有限公司 | Single lithium ion polymer electrolyte membrane and battery comprising same |
| CN114665149A (en) * | 2022-02-28 | 2022-06-24 | 合肥国轩高科动力能源有限公司 | Single-ion gel polymer electrolyte and application thereof |
| CN114976229A (en) * | 2022-05-25 | 2022-08-30 | 济南大学 | Method for preparing tetrafluoroethylene-based polymer electrolyte for lithium battery |
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| CN114335715A (en) * | 2021-12-31 | 2022-04-12 | 珠海冠宇电池股份有限公司 | Single lithium ion polymer electrolyte membrane and battery comprising same |
| WO2023125545A1 (en) * | 2021-12-31 | 2023-07-06 | 珠海冠宇电池股份有限公司 | Electrolyte membrane and preparation method therefor, and battery |
| CN114665149A (en) * | 2022-02-28 | 2022-06-24 | 合肥国轩高科动力能源有限公司 | Single-ion gel polymer electrolyte and application thereof |
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