CN109546225A - A kind of preparation and application of the polymer dielectric improving lithium-sulfur cell self discharge - Google Patents
A kind of preparation and application of the polymer dielectric improving lithium-sulfur cell self discharge Download PDFInfo
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- CN109546225A CN109546225A CN201811243308.3A CN201811243308A CN109546225A CN 109546225 A CN109546225 A CN 109546225A CN 201811243308 A CN201811243308 A CN 201811243308A CN 109546225 A CN109546225 A CN 109546225A
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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
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- 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 discloses the preparations and application of a kind of polymer dielectric for improving lithium-sulfur cell self discharge, provide the preparation method of a kind of novel polymer electrolyte material and the material.This polymer dielectric includes sulfonic group lithium salts, high molecular polymer, lytic agent and plasticizer, can be realized efficient chemical property, avoids the dendrite problems and shuttle problem of existing battery.The single ion conductor method for preparing polymer electrolytes is simple and easy and environmental-friendly, and material can be made to generate good mechanical performance and heat resistance.Single ion conductor polymer dielectric of the invention is applied in the field of lithium-sulfur cell.
Description
Technical field
The invention belongs to the inside electrolyte field of lithium-sulfur cell, be related to electrolyte with and preparation method thereof,
The especially a kind of preparation and application of the single ion conductor polymer dielectric for improving lithium-sulfur cell self discharge.
Technical background
Lithium-sulfur cell is the novel battery that a kind of theoretical specific energy is much higher than conventional lithium ion battery.Sulphur is as active material
Lithium-sulfur cell theoretical specific capacity can achieve 1675 every gram of milliampere hour, energy density can achieve 2600 every kilogram of watt-hours, far
Higher than existing conventional lithium ion battery.At the same time, sulphur rich reserves in nature, environmental-friendly and cheap.
These advantages make lithium-sulfur cell show one's talent, and become the research hotspot of next-generation energy-density lithium ion battery.Existing lithium
Sulphur battery generallys use the structure of the ethers electrolyte combination polyolefin micropore barrier diaphragm of liquid.Core group as lithium-sulfur cell
At component, diaphragm material and electrolyte play a crucial role in the manufacture of battery.Diaphragm and electrolyte property it is excellent
The characteristics such as the bad energy density for directly affecting battery, cycle life and safety.
However, polyalkene diaphragm hole is larger and uneven, inside battery positive and negative anodes is easily caused to contact and microcell occurs
Short circuit；There are biggish mobility for liquid electrolyte, and ethers electrolyte has biggish dissolubility, therefore more sulphur to more sulphions
Ion is easily dissolved in the electrolytic solution and is migrated to negative side, influences the electrochemical stability of cathode of lithium stability and battery；Liquid
There are the security risks such as flammable, easy-to-leak liquid for state electrolyte.
Summary of the invention
The technical issues of in order to solve in the presence of the prior art, the present invention provides a kind of improvement lithium-sulfur cell self discharges
Polymer dielectric preparation and application.The preparation method and polymer electrolyte use in lithium-sulfur cell, relatively
The liquid electrolyte of the prior art adds the combination of diaphragm, has more excellent performance, and technical solution is as follows.
A kind of method for preparing polymer electrolytes improving lithium-sulfur cell self discharge, comprising the following steps:
S1, it is mixed to containing mineral solution of the addition containing lithium ion in sulfonic polymer, it is anti-to the two
After the completion of answering, the organic solution of the lithium salts containing sulfonic group is obtained；
S2, prepare lytic agent；
S3, the mixture that molar ratio is the sulfonic group lithium salts and high molecular polymer within the scope of 1:1-1:50 is weighed, then will
Lytic agent is added in the mixture, and dissolution then is sufficiently stirred in this three, obtains uniform clear solution；
S4, prepare smooth glass plate, on a glass by the coating of clear solution obtained in S3, stand dry in the air at room temperature
It is dry, then move under vacuum environment and be dried, film punching is obtained after dry；
S5, by film punching obtained in S4 remove vacuum environment, to the film punching be added molecular structure be chain or
The plasticizer of person's ring-type ethers finally obtains target product single ion conductor polymer dielectric.
Further, in step sl, the inorganic matter containing lithium ion includes lithium hydroxide, lithium carbonate, lithium chloride, nitric acid
One or more of lithium, lithium acetate, lithium phosphate lithium nitrite, lithium sulfate, lithium tetraborate and its hydrate；Step S1 preparation
Obtaining includes sulfonated polystyrene lithium, Pluronic F-127 base ethyl ester disulfonic acid lithium, polymethylacrylic acid containing sulfonic lithium salts
Alkyl ester sulfonate lithium contains the sulfonic polymer lithium salts such as sulfonic super branched polyurethane lithium；In step S3, high molecular polymerization
Object is Kynoar, Kynoar-hexafluoropropylene copolymer, polyethylene oxide, polymethyl methacrylate, polyacrylonitrile
One or more of.
Further, the lytic agent in step S2 further includes n,N-dimethylacetamide, N-Methyl pyrrolidone, dimethyl
One or more of sulfoxide.
Further, in step S3, the molar ratio of sulfonic group lithium salts and high molecular polymer is specially 1:10-1:50.
Further, in step S4, the drying temperature under vacuum environment is 70-120 degrees Celsius, drying time 12-48
Hour；Standing the time dried at room temperature is 12-48 hours.
Further, in step S5, plasticizer is 1,3-dioxolane/glycol dimethyl ether of volume ratio 1:1, volume ratio
Triglyme/1,3- dioxolanes, the volume ratio 1:1 of triglyme/glycol dimethyl ether of 1:1, volume ratio 1:2
One of triglyme/ionic liquid；The lithium salts that plasticizer also contains, lithium salts are trifluoromethanesulfonic acid lithium, difluoro first
One of base sulfimide lithium, lithium trifluoromethanesulp,onylimide, the content of lithium salts in plasticizers are 1 mole every liter；Plasticising
Agent also contains additive lithium nitrate, and the mass percent of lithium nitrate in plasticizers is 0.1-2wt%.
Further, the moulding process of single ion conductor polymer dielectric is using tipping, blade coating, dimple transfer
One or more of coating, print roll coating, extrusion coated coating process；The thickness model of single ion conductor polymer dielectric
Enclose is 50-200 microns.
This method for preparing polymer electrolytes, the beneficial effect is that:
This method is easily operated and low in cost, can either bench-scale testing can be mass produced again.In preparation process
Raw material, which is fully utilized, is converted into target product, has the characteristics that environmental-friendly.And in preparation process various raw materials chemical property
Stablize, reaction condition coincide, and is convenient for its preparation process of personnel's control.
A kind of polymer dielectric that the method for preparing polymer electrolytes improving lithium-sulfur cell self discharge is produced, packet
Lithium salts containing sulfonic group, high molecular polymer, lytic agent n,N-Dimethylformamide and plasticizer are included, polymer dielectric is aforementioned
The solid polymer that four kinds of components mix.
A kind of application of polymer dielectric, single ion conductor polymer dielectric are to apply improving lithium-sulfur cell electrification
Learn the aspect of performance.
Further, the single ion conductor polymer dielectric is the side applied improving lithium-sulfur cell security performance
Face.
Polymer dielectric of the invention and the application in lithium-sulfur cell, have the advantages that
1, single ion conductor polymer dielectric, instead of common porous polyolefin diaphragm and liquid ethers electrolyte,
It fundamentally avoids inside battery positive and negative anodes and self-discharge phenomenon caused by microcell short circuit occurs, greatly improve lithium-sulfur cell
Initial discharge specific capacity and capacity retention ratio；
2, single ion conductor polymer dielectric, instead of the biggish liquid ethers electrolyte of mobility, so as to avoid
Excessive lysis and migration of the polysulfide anion in liquid ethers electrolyte, slow down the shuttle phenomenon of more sulphions；
3, single ion conductor polymer dielectric is rich in polar functional group abundant, can further enhance to polysulfide yin
The electrostatic repulsion of ion, thus inhibit more sulphions to shuttle to negative side and side reaction occurs with cathode of lithium, it is final to improve
The chemical properties such as cyclical stability, the coulombic efficiency of battery.
4, single ion conductor polymer dielectric, while instead of flammable polyalkene diaphragm and inflammability liquid organic
The use for solving liquid, not only reduces the security risk of battery, also simplifies the composition of battery, reduce battery cost.
5, single ion conductor polymer dielectric, also with electrochemical stability is high, cost of material is low, reaction condition temperature
With with advantages of environment protection.
Detailed description of the invention
The content of Figure of description is described below.
Fig. 1 is the flow chart of single ion conductor polymer dielectric preparation method of the invention.
Fig. 2 is respectively single ion conductor polymer electrolyte battery of the invention, using traditional PP film adds ethers electrolyte
Battery, cycle efficieny comparison and coulombic efficiency comparison diagram when for identical conditions；
In Fig. 2: blue lines represent single ion conductor polymer electrolyte battery, and black lines represent tradition PP film and add ether
Class electrolytic cell；
Abscissa indicates the recurring number (unit: secondary) that two kinds of electrolyte use in lithium-sulfur cell, the left side section 0-1600
The ordinate of range indicates the specific capacity (unit: every gram of milliampere hour) of lithium-sulfur cell, the ordinate table of right side 0-110 interval range
Show the coulombic efficiency (percentage) of lithium-sulfur cell；
The curve of lower section two indicates the specific capacity of lithium-sulfur cell, and the curve of top two indicates the coulombic efficiency of lithium-sulfur cell.
Specific embodiment
It, below will be to the single ion of improvement lithium-sulfur cell self discharge of the invention according to Figure of description and Detailed description of the invention
The preparation and application of Conductive polymers electrolyte combine to form embodiment, further illustrate the principle of the present invention.
As shown in Figure 1, inorganic lithium salt solution is mixed with sulfonic polymeric object produces sulfonic group lithium salts as step 1；Prepare molten
Solution agent is step 2；Sulfonic group lithium salts, lytic agent, high molecular polymer are mixed, and generation residuite liquid is step 3；According to
It is secondary to take out film punching after glass surface coating, room temperature are dried, are dried in vacuo as step 4；It instills and increases in last film punching
Moulding agent and obtaining target product is step 5.
As shown in Fig. 2, the coulombic efficiency of this single-ion polymer electrolytic cell is higher than tradition PP film close to 100%
Add the 85% of ethers electrolytic cell.Under multiple circulation, the specific capacity of this single-ion polymer electrolytic cell is always significant
Add the electrolytelike battery of ether higher than traditional PP film.
The process of each embodiment combination Fig. 1 below is specifically illustrated the preparation of polymer dielectric and application.
It illustrates, following embodiment all has technical effect described in Fig. 2.
Embodiment 1
Sulfonated polystyrene lithium and Kynoar-hexafluoropropylene copolymer polymer electrolyte and preparation side
Method.The specific raw material and preparation process of the single ion conductor polymer dielectric are as follows:
(1) sulfonated polystyrene and lithium hydroxide solution are mixed, reaction waits until sulfonated polystyrene lithium；
(2) prepare a certain amount of n,N-Dimethylformamide；
(3) the sulfonated polystyrene lithium prepared is weighed according to molar ratio 1:10 and Kynoar-hexafluoropropene is total
Polymers；Then a certain amount of N, N- dimethyl methyl is added in sulfonated polystyrene lithium and Kynoar-hexafluoropropylene copolymer
In amide, stirring and dissolving obtains uniform clear solution；
(4) clear solution is poured into clean glass pane surface using scraper, successively carries out blade coating, is placed at room temperature for 12
Hour naturally volatilization dry, dry 12 hours processes under 70 degrees Celsius of vacuum, it is smooth and there is certain machinery to obtain surface
The transparent membrane of intensity, thickness are about 50 microns；
(5) obtained film is finally transferred to glove box, instills appropriate plasticizer 1,3-dioxolane/glycol dinitrate
Ether (volume ratio 1:1) obtains target single ion conductor polymer dielectric: Kynoar-hexafluoropropene and sulfonated polyphenyl second
The polymer of alkene lithium.
The polymer of the Kynoar-hexafluoropropene and sulfonated polystyrene lithium is put into lithium-sulfur cell, as electricity
The electrolyte of the Xie Zhilai substitution prior art adds diaphragm to combine.The electrolyte does not have inside battery positive and negative anodes microcell short circuit to make
At self-discharge phenomenon and shuttle effect, greatly improve the chemical property of lithium-sulfur cell.
Embodiment 2
The polymer electrolyte and preparation method of polyalkyl methacrylate Sulfonic Lithium and Kynoar.The list
The specific raw material and preparation process of ion conductor polymer dielectric are as follows:
(1) polyalkyl methacrylate sulfonic acid and lithium hydroxide solution are mixed, reaction obtains polymethylacrylic acid alkane
Base ester Sulfonic Lithium；
(2) prepare a certain amount of n,N-dimethylacetamide；
(3) the polyalkyl methacrylate Sulfonic Lithium and Kynoar prepared is weighed according to molar ratio 1:20；
Then polyalkyl methacrylate Sulfonic Lithium and Kynoar are added in a certain amount of n,N-dimethylacetamide, stirring
Dissolution obtains uniform clear solution；
(4) clear solution is passed through the method toppled over to be laid on smooth glass plate, successively carries out being placed at room temperature for 24 small
Shi Ziran volatilization dries, dry 24 hours processes under 90 degrees Celsius of vacuum, and it is smooth and have certain mechanical strength to obtain surface
Transparent membrane, thickness is about 100 microns；
(5) obtained film is transferred to glove box, instills appropriate plasticizer triglyme/glycol dimethyl ether
(volume ratio 1:1), additive lithium trifluoromethanesulp,onylimide (1mol/L) obtain target single ion conductor polymer dielectric:
The polymer of Kynoar and polyalkyl methacrylate Sulfonic Lithium.
The polymer of the Kynoar and polyalkyl methacrylate Sulfonic Lithium is put into lithium-sulfur cell, as electricity
The electrolyte of the Xie Zhilai substitution prior art adds diaphragm to combine.The electrolyte does not have inside battery positive and negative anodes microcell short circuit to make
At self-discharge phenomenon and shuttle effect, greatly improve the chemical property of lithium-sulfur cell.
Embodiment 3
Polymer electrolyte and preparation method containing sulfonic super branched polyurethane lithium and polyethylene oxide.The list
The specific raw material and preparation process of ion conductor polymer dielectric are as follows:
(1) sulfonic super branched polyurethane and lithium sulfate solution mixing will be contained, reaction is obtained containing sulfonic hyperbranched
Polyurethane lithium；
(2) prepare a certain amount of N-Methyl pyrrolidone amine；
(3) weighed according to molar ratio 1:30 prepared containing sulfonic super branched polyurethane lithium and polyethylene oxide；
Then it will contain sulfonic super branched polyurethane lithium and polyethylene oxide is added in a certain amount of N-Methyl pyrrolidone amine, stirring
Dissolution obtains uniform clear solution；
(4) it is successively coated using dimple transfer coating technology in smooth glass plate plate surface, to be placed at room temperature for 24 small
Shi Ziran volatilization dries, dry 36 hours processes under 100 degrees Celsius of vacuum, and it is smooth and have certain mechanical strength to obtain surface
Transparent membrane, thickness is about 150 microns；
(5) obtained film is transferred to glove box, instills appropriate plasticizer triglyme/1,3-dioxolane
(volume ratio 1:2), additive difluoromethyl sulfimide lithium (1mol/L) obtain target single ion conductor polymer dielectric:
Polyethylene oxide and polymer containing sulfonic super branched polyurethane lithium.
The polyethylene oxide and the polymer containing sulfonic super branched polyurethane lithium are put into lithium-sulfur cell, as electricity
The electrolyte of the Xie Zhilai substitution prior art adds diaphragm to combine.The electrolyte does not have inside battery positive and negative anodes microcell short circuit to make
At self-discharge phenomenon and shuttle effect, greatly improve the chemical property of lithium-sulfur cell.
Embodiment 4
Polymer electrolyte and its preparation of Pluronic F-127 base ethyl ester disulfonic acid lithium and polymethyl methacrylate
Method.The specific raw material and preparation process of the single ion conductor polymer dielectric are as follows:
(1) Pluronic F-127 base ethyl ester disulfonic acid and lithium hydroxide solution are mixed, reaction obtains Pluronic F-127 base second
Ester disulfonic acid lithium；
(2) prepare a certain amount of dimethyl sulfoxide；
(3) the Pluronic F-127 base ethyl ester disulfonic acid lithium and polymethylacrylic acid prepared is weighed according to molar ratio 1:50
Methyl esters；Then a certain amount of dimethyl sulfoxide is added in Pluronic F-127 base ethyl ester disulfonic acid lithium and polymethyl methacrylate
In, stirring and dissolving obtains uniform clear solution；
(4) be successively coated using extrusion coated technique in smooth glass pane surface, be placed at room temperature for 36 hours it is natural
Volatilization dries, dry 48 hours processes under 120 degrees Celsius of vacuum, and it is smooth and transparent with certain mechanical strength to obtain surface
Film, thickness are about 200 microns；
(5) obtained film is transferred to glove box, instills appropriate plasticizer triglyme/ionic liquid (volume
Than 1:1), additive lithium trifluoromethanesulp,onylimide (1mol/L) obtains target single ion conductor polymer dielectric: poly- methyl
The polymer of methyl acrylate and Pluronic F-127 base ethyl ester disulfonic acid lithium.
The polymer of the polymethyl methacrylate and Pluronic F-127 base ethyl ester disulfonic acid lithium is put into lithium-sulfur cell,
The electrolyte that the prior art is substituted as electrolyte adds diaphragm to combine.The electrolyte does not have inside battery positive and negative anodes microcell
Self-discharge phenomenon caused by short circuit and shuttle effect, greatly improve the chemical property of lithium-sulfur cell.
Above embodiments are present invention embodiment arranged side by side, to illustrate concrete principle of the invention.Art technology
Personnel are it will be appreciated that protection scope of the present invention content according to claims defines, any original according to the present invention
The improvement or equivalent replacement carried out is managed, in scope of protection of the claims.
Claims (10)
1. a kind of single ion conductor method for preparing polymer electrolytes for improving lithium-sulfur cell self discharge, which is characterized in that packet
Include following steps:
S1, it is mixed to containing mineral solution of the addition containing lithium ion in sulfonic polymer, has been reacted to the two
Cheng Hou obtains the organic solution of the lithium salts containing sulfonic group；
S2, prepare lytic agent；
S3, the mixture that molar ratio is the sulfonic group lithium salts and high molecular polymer within the scope of 1:1-1:50 is weighed, then will dissolution
Agent is added in the mixture, and dissolution then is sufficiently stirred in three, obtains uniform clear solution；
S4, prepare smooth glass plate, on a glass by the coating of clear solution obtained in S3, stand dry at room temperature, then
It moves under vacuum environment and is dried, obtain film punching after dry；
S5, film punching obtained in S4 is removed into vacuum environment, it is chain or ring that molecular structure, which is added, to the film punching
The plasticizer of shape ethers finally obtains target product containing sulfonic single ion conductor polymer dielectric.
2. improving the preparation side of the single ion conductor polymer dielectric of lithium-sulfur cell self discharge described according to claim 1
Method, it is characterised in that: in the preparation step S1 of single ion conductor polymer dielectric, inorganic matter of the step S1 containing lithium ion includes
Lithium hydroxide, lithium carbonate, lithium chloride, lithium nitrate, lithium acetate, lithium phosphate lithium nitrite, lithium sulfate, lithium tetraborate and its hydrate
One or more of；The sulfonic group lithium salts that step S1 is obtained includes sulfonated polystyrene lithium, Pluronic F-127 base ethyl ester pair
Sulfonic Lithium, polyalkyl methacrylate Sulfonic Lithium, one or more of containing sulfonic super branched polyurethane lithium；Step
In S3, high molecular polymer includes Kynoar, Kynoar-hexafluoropropylene copolymer, polyethylene oxide, poly- methyl-prop
One or more of e pioic acid methyl ester, polyacrylonitrile.
3. improving the preparation side of the single ion conductor polymer dielectric of lithium-sulfur cell self discharge described according to claim 1
Method, it is characterised in that: the lytic agent in the preparation step S2 of the single ion conductor polymer dielectric further includes N, N-
One or more of dimethyl acetamide, N-Methyl pyrrolidone, dimethyl sulfoxide.
4. improving the preparation side of the single ion conductor polymer dielectric of lithium-sulfur cell self discharge described according to claim 1
Method, it is characterised in that: in the preparation step S3 of the single ion conductor polymer dielectric, the sulfonic group lithium salts and the height
The molar ratio of Molecularly Imprinted Polymer is specially 1:10-1:50.
5. improving the preparation side of the single ion conductor polymer dielectric of lithium-sulfur cell self discharge described according to claim 1
Method, it is characterised in that: in the preparation step S4 of the single ion conductor polymer dielectric, the drying temperature under vacuum environment is
70-120 degrees Celsius, drying time is 12-48 hours；Standing the time dried at room temperature is 12-48 hours.
6. improving the preparation side of the single ion conductor polymer dielectric of lithium-sulfur cell self discharge described according to claim 1
Method, it is characterised in that: in the preparation step S5 of the single ion conductor polymer dielectric, the plasticizer is volume ratio 1:1
1,3- dioxolanes/glycol dimethyl ether, volume ratio 1:1 triglyme/glycol dinitrate ether mixture, volume ratio
Triglyme/ionic liquid mixture of the triglyme of 1:2/1,3- dioxolanes mixture, volume ratio 1:1
It is a kind of；The plasticizer also contains lithium salts, and the lithium salts is trifluoromethanesulfonic acid lithium, difluoromethyl sulfimide lithium, trifluoro
One of sulfonyloxy methyl imine lithium, content of the lithium salts in the plasticizer are 1 mole every liter；The plasticizer also contains
There is additive lithium nitrate, mass percent of the lithium nitrate in the plasticizer is 0.1-2wt%.
7. improve the single ion conductor method for preparing polymer electrolytes of lithium-sulfur cell self discharge according to claim 1,
It is characterized by: the moulding process of single ion conductor polymer dielectric described in step S4 is using tipping, blade coating, micro-
One or more of recessed transfer coated, print roll coating, extrusion coated coating process；Single ion conductor described in step S5 is poly-
The thickness range of polymer electrolyte is 50-200 microns.
8. a kind of single ion conductor polymer according to any one of claim 1 to 7 for improving lithium-sulfur cell self discharge
The made single ion conductor polymer dielectric obtained of electrolyte electrolyte preparation method, it is characterised in that: including described
Lithium salts containing sulfonic group, the high molecular polymer, the lytic agent N,N-dimethylformamide and the plasticizer；It is described isolated
Sub- Conductive polymers electrolyte electrolyte is the solid polymer that aforementioned four kinds of components mix.
9. the application of single ion conductor polymer dielectric described in a kind of claim 8, which is characterized in that the single ion is led
Body polymer dielectric electrolyte is applied in terms of improving lithium-sulfur cell chemical property.
10. the application of single ion conductor polymer dielectric according to claim 9, which is characterized in that the single ion is led
Body polymer dielectric electrolyte is applied in terms of improving lithium-sulfur cell security performance.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113299984A (en) * | 2021-04-29 | 2021-08-24 | 中国乐凯集团有限公司 | Single-ion conductor polymer solid electrolyte membrane and preparation method and application thereof |
| CN113363575A (en) * | 2021-06-28 | 2021-09-07 | 中国科学院青岛生物能源与过程研究所 | Sulfonic polymer eutectic solid electrolyte and preparation method thereof |
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