CN109873196A - A kind of gel electrolyte and lithium-sulfur rechargeable battery - Google Patents
A kind of gel electrolyte and lithium-sulfur rechargeable battery Download PDFInfo
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- CN109873196A CN109873196A CN201711245539.3A CN201711245539A CN109873196A CN 109873196 A CN109873196 A CN 109873196A CN 201711245539 A CN201711245539 A CN 201711245539A CN 109873196 A CN109873196 A CN 109873196A
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Abstract
The present invention relates to a kind of gel electrolyte, including liquid electrolyte, polymerizable unimolecule organic matter and initiator, the polymerizable unimolecule organic matter includes one of substance shown in formula one or a variety of, formula one:Wherein, R1、R2、R3、R4Independently selected from alkyl, alkyl acrylic ester group, ether, halogenated alkyl, halogenated alkyl be acrylate-based or halogenated ether, and a, b, c, d are independently selected from the number between 0~5.Gel electrolyte of the invention can effectively increase the probability of monomolecular reaction when polymerization reaction occurs, improve the degree of polymerization of polymer, gel electrolyte of the invention has good chemical property and safety, thus the lithium-sulfur rechargeable battery of gel electrolyte preparation, it is able to ascend the efficiency for charge-discharge, capacity retention ratio and first all discharge capacities with higher of battery, and preparation process of the invention is simple, easily realizes and produces in enormous quantities.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of gel electrolyte and lithium-sulfur rechargeable battery.
Background technique
Operating voltage is high, energy density is big, memory-less effect, has extended cycle life and nothing because having for lithium ion secondary battery
The advantages that pollution.Since commercialization in 1991, lithium ion secondary battery has become the preferred power supply of each electronic product.But
As electric bicycle, electric car, large-scale energy-accumulating power station enter extensive development and application stage, to lithium ion secondary battery
Propose the requirement of more height ratio capacity.At this stage, low (the practical ratio of positive electrode of the capacity of lithium ion secondary battery positive and negative pole material
Capacity < 300mAh/g；Negative electrode material specific capacity < 400mAh/g) become the principal element for restricting its development.Lithium-sulfur rechargeable battery must
So become the first choice of battery of new generation.As positive electrode, the theoretical specific capacity of elemental sulfur reach 1675mAh/g and hypotoxicity,
The advantages that amount of storage is big, cheap.
At this stage, there are main problems first is that lithium polysulfide is dissolved in nonaqueous electrolytic solution for lithium-sulfur rechargeable battery.Lithium sulphur
The intermediate discharging product of secondary cell can be dissolved into organic electrolyte, increase the viscosity of electrolyte, reduce ionic conductivity.Sulphur
More sulphions that reduction reaction generates, which occur, for electrode to migrate between lithium battery positive and negative anodes, lead to the loss of active material；Together
When, the polysulfide of dissolution can be diffused into cathode across diaphragm, with negative reaction, destroy anolyte interfacial film.In addition,
Lithium-sulfur rechargeable battery uses lithium metal as cathode, and other than the high activity of lithium metal itself, lithium anode is in charge and discharge
Li dendrite is easily formed in journey.Therefore, main solution first is that start in terms of electrolyte, made in early days using ether compound
For the electrolyte solvent of lithium-sulfur cell, some additives are added in electrolyte, the problems of dissolution of lithium polysulfide can be alleviated.
Publication No. is that CN106532115A discloses a kind of gel electrolyte and lithium-sulfur rechargeable battery, embodiment 1 and 2 are adopted
Trimethylolpropane trimethacrylate is used to prepare lithium-sulfur rechargeable battery, the lithium of Examples 1 and 2 as polymerizable unimolecule organic matter
The battery capacity of sulfur rechargeable battery is 995~1002mAh, and 10 weeks capacity retention ratios 80~83%, 10 weeks efficiency for charge-discharges are 90
~93%；Embodiment 3 and 4 prepares the secondary electricity of lithium sulphur as polymerizable unimolecule organic matter using pentaerythritol tetraacrylate
Pond, the battery capacity of the lithium-sulfur rechargeable battery of embodiment 3 and 4 are 1010~1015mAh, 10 weeks capacity retention ratios 85~86%,
10 weeks efficiency for charge-discharges are 91~92%；Embodiment 5 and 6 is organic as polymerizable unimolecule using neopentylglycol diacrylate
Object prepares lithium-sulfur rechargeable battery, and the battery capacity of the lithium-sulfur rechargeable battery of embodiment 5 and 6 is 980~990mAh, and capacity is protected within 10 weeks
80~85%, 10 weeks efficiency for charge-discharges of holdup are 86~88%.The battery capacity of lithium-sulfur rechargeable battery in the patent, capacity are protected
The comprehensive performance of holdup and efficiency for charge-discharge is still to be improved.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of battery capacity, capacity retention ratio and efficiency for charge-discharges
The gel electrolyte of good combination property.
Another technical problem to be solved by this invention is to provide a kind of secondary electricity of lithium sulphur using above-mentioned gel electrolyte
Pond.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
It is an object of the present invention to provide a kind of gel electrolyte, including liquid electrolyte, polymerizable unimolecule are organic
Object and initiator, the polymerizable unimolecule organic matter includes one of substance shown in formula one or a variety of,
Formula one:Wherein,
R1、R2、R3、R4Independently selected from alkyl, alkyl acrylic ester group, ether, halogenated alkyl, halogenated alkyl acrylic acid
Ester group or halogenated ether, a, b, c, d are independently selected from the number between 0~5.
Acrylate-based functional group in polymerizable unimolecule organic matter of the invention primarily forms the net of gel electrolyte
Shape structure makes gel electrolyte have certain mechanical strength and hardness；Ether and alkyl in polymerizable unimolecule organic matter
Functional group primarily forms lithium ion mobility channel, move freely lithium ion can in gel electrolyte under electric field action.
Preferably, R1、R2、R3、R4Independently selected from carbon atom number be 1~5 alkyl, carbon atom number be 1~5 alkyl
Halogenated alkyl that ether that acrylate-based, carbon atom number is 1~5, carbon atom number are 1~5, carbon atom number be 1~5 it is halogenated
The halogenated ether that alkyl acrylic ester group or carbon atom number are 1~5, a, b, c, d are independently selected from the integer between 0~2.
Specifically, R1、R2、R3And R4Independently selected from CH3-、C2H5-、C3H7-、C4H9-、CH3CH2COOCH2-、
CH2CHCOOCH2-、CH3CH2COOCH2CH2-、CH2CHCOOCH2CH2-、CF3-、C2F5-、C3F7-、C4F9-、C2F5COOCH2-、
C2F3COOCH2-、C2F5COOCH2CH2-、C2F3COOCH2CH2Etc..
Preferably, it is total to account for the polymerizable unimolecule organic matter for the acrylate-based molecular weight in substance shown in formula one
The 20~90% of molecular weight, the molecular weight of alkyl account for the 10~80% of the polymerizable unimolecule organic matter total molecular weight.
It is further preferred that the acrylate-based molecular weight in substance shown in formula one, which accounts for the polymerizable unimolecule, to be had
The 50~70% of machine object total molecular weight, the molecular weight of alkyl account for the polymerizable unimolecule organic matter total molecular weight 30~
50%.
Most preferably, substance shown in formula one is 2- [[2,2- bis- [[(1- oxo -2- acrylic] methyl] butoxy] first
Base] -2- ethyl -1,3- propane diyl -2- acrylate.
Preferably, the polymerizable unimolecule organic matter further includes one of substance shown in formula two or a variety of,
Formula two:Wherein, R5、R6、R7Independently selected from alkyl or alkyl third
Olefin(e) acid ester group.
It is further preferred that R5、R6、R7Independently selected from carbon atom number be 1~5 alkyl or carbon atom number be 1~5
Alkyl acrylic ester group.
It is further preferred that the acrylate-based molecular weight in substance shown in formula two, which accounts for the polymerizable unimolecule, to be had
The 20~90% of machine object total molecular weight, the molecular weight of alkyl account for the polymerizable unimolecule organic matter total molecular weight 10~
80%.
It is further preferable that account for the polymerizable unimolecule organic for the acrylate-based molecular weight in substance shown in formula two
The 65~85% of object total molecular weight, the molecular weight of alkyl account for the polymerizable unimolecule organic matter total molecular weight 15~
35%.
Most preferably, substance shown in formula two be trimethylolpropane trimethacrylate, it is pentaerythritol tetraacrylate, new
The combination of one or more of Diacrylate.
According to a preferred embodiment, the polymerizable unimolecule organic matter includes the formula one that mass ratio is 1~2:1
Substance shown in shown substance and formula two.
Most preferably, the polymerizable unimolecule organic matter is 2- [[2,2- bis- [[(1- oxo -2- acrylic] first
Base] butoxy] methyl] and -2- ethyl -1,3- propane diyl -2- acrylate and neopentylglycol diacrylate mixture.
Preferably, the addition quality of the polymerizable unimolecule organic matter is the 1 of the gel electrolyte gross mass
~10%, further preferably 1~3%.
Specifically, the liquid electrolyte includes ether organic solvent and lithium salts.
More specifically, the ether organic solvent is selected from glycol dimethyl ether, 1,3- dioxolane, Isosorbide-5-Nitrae-dioxy
The combination of one or more of six rings, four (ethylene glycol) dimethyl ether, three (ethylene glycol) dimethyl ether.
Preferably, the ether organic solvent is the glycol dimethyl ether and 1 that volume ratio is 1:0.9~1.1,3- dioxy
The mixture at five rings.
More specifically, the lithium salts is in two (trimethyl fluoride sulfonyl) imine lithiums, double fluorine sulfimide lithiums
One or more of combinations.
Preferably, concentration of the lithium salts in the liquid electrolyte is 0.9~1.1mol/L.
Specifically, the initiator is selected from one of organic peroxide, inorganic peroxide, azo or several
The combination of kind.
Specifically, the addition quality of the initiator is the 0.001~3% of the gel electrolyte gross mass, it is excellent
It is selected as 0.005%~0.008%.
Preferably, the liquid electrolyte further includes additive, and the additive is selected from LiNO3、CrNO3、
RbNO3One or more of combination.
It is further preferred that the addition quality of the additive be the gel electrolyte gross mass 0.01%~
5%, more preferably 0.5%~2%.
It is a further object to provide a kind of lithium-sulfur rechargeable batteries, using the gel electrolyte.
Lithium-sulfur rechargeable battery in the present invention the preparation method comprises the following steps: anode, cathode, diaphragm and shell are assembled into battery core,
By in the described gel electrolyte injection battery core, sealing, then initiated polymerization, battery is successively melted into again,
Circulation deflates, seals the lithium-sulfur rechargeable battery described in obtaining.
Preferably, 20~100 DEG C at a temperature of cause the polymerization reaction or cause under the action of uv light
The polymerization reaction.
It is further preferred that 60~80 DEG C at a temperature of cause the polymerization reaction.
It is outer that lithium-sulfur rechargeable battery of the invention is not limited to monetary apparatus, cylindrical steel shell-type, rectangular aluminum shell type, Soft Roll polymer etc.
See feature.
Due to the above technical solutions, the present invention has the following advantages over the prior art:
Gel electrolyte of the invention can effectively increase the probability of monomolecular reaction when polymerization reaction occurs, and improve poly-
The degree of polymerization of object is closed, gel electrolyte of the invention has good chemical property and safety, thus gel electrolyte system
Standby lithium-sulfur rechargeable battery is able to ascend the efficiency for charge-discharge, capacity retention ratio and first all discharge capacities with higher of battery,
And preparation process of the invention is simple, easily realizes and produces in enormous quantities.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.If not special herein
Illustrate, " % " representation quality percentage.
Comparative example 1:
It prepares liquid electrolyte: weighing, mixed for use by following volume ratio relationship: glycol dimethyl ether (it writes a Chinese character in simplified form:
DME): it is 50:50 that 1,3- dioxolane, which (writes a Chinese character in simplified form: DOL) volume ratio, adds (the letter of two (trimethyl fluoride sulfonyl) imine lithiums later
Write: LiTFSI), obtain the liquid electrolyte E1 that LiTFSI concentration is 1mol/L.
Prepare battery core to be injected: by elemental sulfur, conductive agent and bonding agent, the works such as agitated, coating, cold pressing, slitting, welding
Sequence obtains positive plate；Sulphur positive plate, lithium cathode sheet and diaphragm prepare naked battery core together, the use of aluminum plastic film are that packaging bag is sealed
Dress, is toasted later.
Fluid injection and anode ring forming: it by the battery core after above-mentioned liquid electrolyte E1 injection baking, stands until electrolyte soaks
Moisten entire diaphragm, then be melted into, shaping, the processes such as degasification, finally obtains lithium-sulfur cell comparative example B1.
Comparative example 2:
After preparing by liquid electrolyte E1, add 1%LiNO3As additive, liquid electrolyte E2 is obtained；
Fluid injection and anode ring forming: by the battery core after above-mentioned liquid electrolyte E2 injection baking, (battery core prepares same comparative example
1) it in, stands until electrolyte infiltrates entire diaphragm, then is melted into, shaping, the processes such as degasification, finally obtain lithium-sulfur cell ratio
Compared with example B2.
Comparative example 3:
After preparing by liquid electrolyte E2,5% methyl methacrylate and 0.05% perbenzoic acid initiator are added,
Obtain gel electrolyte E3；
Fluid injection and anode ring forming: by the battery core after above-mentioned liquid electrolyte E3 injection baking, (battery core prepares same comparative example
1) it in, stands until electrolyte infiltrates entire diaphragm, after 80 DEG C of high temperature are shelved 6 hours, then is melted into, shaping, the works such as degasification
Sequence finally obtains lithium-sulfur cell comparative example B3.
Embodiment 1:
After preparing by liquid electrolyte E1,1% 2- [[2,2- bis- [[(1- oxo -2- acrylic] methyl] fourth oxygen is added
Base] methyl] -2- ethyl -1,3- propane diyl -2- acrylate (No. CAS: 94108-97-1) and 0.05% perbenzoic acid
Initiator obtains gel electrolyte ES1；
Fluid injection and anode ring forming: by the battery core after above-mentioned gel electrolyte ES1 injection baking, (battery core prepares same comparative example
1) it in, stands until electrolyte infiltrates entire diaphragm, after 80 DEG C of high temperature are shelved 4 hours, then is melted into, shaping, the works such as degasification
Sequence finally obtains lithium-sulfur cell embodiment BS1.
Embodiment 2:
After preparing by liquid electrolyte E2,1% 2- [[2,2- bis- [[(1- oxo -2- acrylic] methyl] fourth oxygen is added
Base] methyl] -2- ethyl -1,3- propane diyl -2- acrylate (No. CAS: 94108-97-1) and 0.05% perbenzoic acid
Initiator obtains gel electrolyte ES2；
Fluid injection and anode ring forming: by the battery core after above-mentioned electrolyte ES2 injection baking (preparation of battery core is with comparative example 1)
In, it stands until electrolyte infiltrates entire diaphragm, after 65 DEG C of high temperature are shelved 6 hours, then is melted into, shaping, the processes such as degasification,
Finally obtain lithium-sulfur cell embodiment BS2.
Embodiment 3:
After preparing by liquid electrolyte E1,2% 2- [[2,2- bis- [[(1- oxo -2- acrylic] methyl] fourth oxygen is added
Base] methyl] -2- ethyl -1,3- propane diyl -2- acrylate (No. CAS: 94108-97-1) and 0.08%AIBN, are coagulated
Glue electrolyte ES3；
Fluid injection and anode ring forming: by the battery core after above-mentioned electrolyte ES3 injection baking (preparation of battery core is with comparative example 1)
In, it stands until electrolyte infiltrates entire diaphragm, after 80 DEG C of high temperature are shelved 4 hours, then is melted into, shaping, the processes such as degasification,
Finally obtain lithium-sulfur cell embodiment BS3.
Embodiment 4: after preparing by liquid electrolyte E2,2% 2- [[2,2- bis- [[(1- oxo -2- acrylic] first is added
Base] butoxy] methyl] -2- ethyl -1,3- propane diyl -2- acrylate (No. CAS: 94108-97-1) and 0.08%AIBN,
Obtain gel electrolyte ES4；
Fluid injection and anode ring forming: by the battery core after above-mentioned electrolyte ES4 injection baking (preparation of battery core is with comparative example 1)
In, it stands until electrolyte infiltrates entire diaphragm, after 65 DEG C of high temperature are shelved 6 hours, then is melted into, shaping, the processes such as degasification,
Finally obtain lithium-sulfur cell embodiment BS4.
Embodiment 5: after preparing by liquid electrolyte E1,1% neopentylglycol diacrylate (No. CAS: 2223- is added
82-7), 1.5%2- [[bis- [[(1- oxo -2- acrylic] methyl of 2,2-] butoxy] methyl] -2- ethyl -1,3- propane two
Base -2- acrylate (No. CAS: 94108-97-1) and 0.08% perbenzoic acid initiator, obtain gel electrolyte ES5；
Fluid injection and anode ring forming: by the battery core after above-mentioned electrolyte ES5 injection baking (preparation of battery core is with comparative example 1)
In, it stands until electrolyte infiltrates entire diaphragm, after 80 DEG C of high temperature are shelved 4 hours, then is melted into, shaping, the processes such as degasification,
Finally obtain lithium-sulfur cell embodiment BS5.
Embodiment 6: after preparing by liquid electrolyte E2,1% neopentylglycol diacrylate (No. CAS: 2223- is added
82-7), 1.5%2- [[bis- [[(1- oxo -2- acrylic] methyl of 2,2-] butoxy] methyl] -2- ethyl -1,3- propane two
Base -2- acrylate (No. CAS: 94108-97-1) and 0.08% perbenzoic acid initiator, obtain gel electrolyte ES6；
Fluid injection and anode ring forming: by the battery core after above-mentioned electrolyte ES6 injection baking (preparation of battery core is with comparative example 1)
In, it stands until electrolyte infiltrates entire diaphragm, after 65 DEG C of high temperature are shelved 6 hours, then is melted into, shaping, the processes such as degasification,
Finally obtain lithium-sulfur cell embodiment BS6.
Table 1 is the battery performance comparison of comparative example and embodiment.
Table 1
By experimental result as it can be seen that capacity using gel state lithium-sulfur rechargeable battery of the invention, in cyclic process in 10 weeks
Conservation rate and efficiency for charge-discharge are above lithium-sulfur rechargeable battery using liquid electrolyte.Illustrate that the gel state lithium-sulfur rechargeable battery has
There is more preferably chemical property.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention, it is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (11)
1. a kind of gel electrolyte, including liquid electrolyte, polymerizable unimolecule organic matter and initiator, it is characterised in that: institute
The polymerizable unimolecule organic matter stated includes one of substance shown in formula one or a variety of,
Formula one:Wherein,
R1、R2、R3、R4Independently selected from alkyl, alkyl acrylic ester group, ether, halogenated alkyl, halogenated alkyl it is acrylate-based or
Halogenated ether, a, b, c, d are independently selected from the number between 0~5.
2. gel electrolyte according to claim 1, it is characterised in that: R1、R2、R3、R4It is 1 independently selected from carbon atom number
Ether that alkyl acrylic ester group that~5 alkyl, carbon atom number are 1~5, carbon atom number are 1~5, carbon atom number are 1~5
Halogenated alkyl, carbon atom number be 1~5 the halogenated ether that halogenated alkyl is acrylate-based or carbon atom number is 1~5, a, b,
C, d is independently selected from the integer between 0~2.
3. gel electrolyte according to claim 1, it is characterised in that: acrylate-based point in substance shown in formula one
Son amount accounts for the 20~90% of the polymerizable unimolecule organic matter total molecular weight, and the molecular weight of alkyl accounts for the polymerizable list
The 10~80% of molecular organic total molecular weight.
4. gel electrolyte according to claim 3, it is characterised in that: acrylate-based point in substance shown in formula one
Son amount accounts for the 50~70% of the polymerizable unimolecule organic matter total molecular weight, and the molecular weight of alkyl accounts for the polymerizable list
The 30~50% of molecular organic total molecular weight.
5. gel electrolyte according to claim 1, it is characterised in that: the polymerizable unimolecule organic matter further includes
One of substance shown in formula two is a variety of,
Formula two:Wherein, R5、R6、R7Independently selected from alkyl or alkyl acrylic
Ester group.
6. gel electrolyte according to claim 5, it is characterised in that: the polymerizable unimolecule organic matter includes matter
Amount is than being substance shown in substance shown in the formula one of 1~2:1 and formula two.
7. gel electrolyte according to claim 5, it is characterised in that: the polymerizable unimolecule organic matter is 2-
[[bis- [[(1- oxo -2- acrylic] methyl of 2,2-] butoxy] methyl] -2- ethyl -1,3- propane diyl -2- acrylate and
The mixture of neopentylglycol diacrylate.
8. gel electrolyte according to any one of claim 1 to 7, it is characterised in that: the polymerizable unimolecule
The addition quality of organic matter is the 1~10% of the gel electrolyte gross mass.
9. gel electrolyte according to any one of claim 1 to 7, it is characterised in that: the liquid electrolyte packet
Ether organic solvent and lithium salts are included,
The ether organic solvent is selected from glycol dimethyl ether, 1,3- dioxolane, Isosorbide-5-Nitrae-dioxane, four (ethylene glycol)
The combination of one or more of dimethyl ether, three (ethylene glycol) dimethyl ether；
The lithium salts is the group selected from one or more of two (trimethyl fluoride sulfonyl) imine lithiums, double fluorine sulfimide lithiums
It closes；
The initiator is the combination selected from one or more of organic peroxide, inorganic peroxide, azo；Institute
The addition quality for the initiator stated is the 0.001~3% of the gel electrolyte gross mass.
10. gel electrolyte according to claim 9, it is characterised in that: the liquid electrolyte further includes additive,
The additive is selected from LiNO3、CrNO3、RbNO3One or more of combination.
11. a kind of lithium-sulfur rechargeable battery, it is characterised in that: using gel electrolyte described in any one of claims 1 to 10.
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| CN201711245539.3A CN109873196B (en) | 2017-12-01 | 2017-12-01 | Gel electrolyte and lithium-sulfur secondary battery |
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| CN201711245539.3A CN109873196B (en) | 2017-12-01 | 2017-12-01 | Gel electrolyte and lithium-sulfur secondary battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113087856A (en) * | 2019-12-23 | 2021-07-09 | 通用汽车环球科技运作有限责任公司 | Gelling agents for forming gel electrolytes and methods relating thereto |
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|---|---|---|---|---|
| CN105428708A (en) * | 2006-12-21 | 2016-03-23 | 株式会社Lg化学 | Gel Polymer Electrolyte Composition, Gel Polymer Electrolyte And Electrochemical Device Comprising The Same |
| CN106532115A (en) * | 2016-11-25 | 2017-03-22 | 张家港市国泰华荣化工新材料有限公司 | Gel electrolyte and lithium-sulfur secondary battery |
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2017
- 2017-12-01 CN CN201711245539.3A patent/CN109873196B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105428708A (en) * | 2006-12-21 | 2016-03-23 | 株式会社Lg化学 | Gel Polymer Electrolyte Composition, Gel Polymer Electrolyte And Electrochemical Device Comprising The Same |
| CN106532115A (en) * | 2016-11-25 | 2017-03-22 | 张家港市国泰华荣化工新材料有限公司 | Gel electrolyte and lithium-sulfur secondary battery |
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| HYUN-SOO KIM ET AL: "Synthesis and electrochemical performances of di(trimethylolpropane)tetraacrylate-based gel polymer electrolyte", 《JOURNAL OF POWER SOURCES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113087856A (en) * | 2019-12-23 | 2021-07-09 | 通用汽车环球科技运作有限责任公司 | Gelling agents for forming gel electrolytes and methods relating thereto |
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