CN109980275A - A kind of wide warm solid polyelectrolyte and its preparation and the application in all solid state alkali metal/alkaline earth metal batteries - Google Patents
A kind of wide warm solid polyelectrolyte and its preparation and the application in all solid state alkali metal/alkaline earth metal batteries Download PDFInfo
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- CN109980275A CN109980275A CN201910215674.6A CN201910215674A CN109980275A CN 109980275 A CN109980275 A CN 109980275A CN 201910215674 A CN201910215674 A CN 201910215674A CN 109980275 A CN109980275 A CN 109980275A
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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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
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Abstract
The present invention discloses a kind of wide warm solid polyelectrolyte and its preparation and the application in all solid state alkali metal/alkaline earth metal batteries.Agar derivative and crosslinking agent are subjected to cross-linking reaction, obtain cross-linked matrix；Cross-linked matrix and alkali metal salt or alkali salt is compound to get having height to lead the warm solid polyelectrolyte of ionic width in -40 DEG C~120 DEG C temperature ranges；The preparation method is easy to operate, at low cost, and the warm solid polyelectrolyte of the width of preparation is suitable for alkali or alkaline earth metal battery, expands the Applicable temperature range of solid-state alkali metal or alkaline earth metal batteries.
Description
Technical field
The present invention relates to a kind of solid polyelectrolytes and its preparation method and application, in particular to one kind can be -40
DEG C~120 DEG C of wide temperature ranges in the all-solid-state battery electrolyte that works normally and its as all solid state alkali or alkaline earth metal
The application of cell electrolyte belongs to all-solid-state battery field of material technology.
Background technique
The development of energy storage device is maked rapid progress, and application field constantly expands, and application requirement is also continuously improved, and is obtained at present wide
The liquid lithium ionic cell of general application is as the essential device of portable device, for being applied to the power such as new-energy automobile
Field of batteries is placed high hopes, however the security risk of liquid lithium ionic cell is especially prominent, and further application is limited.
The appearance of solid electrolyte provides a breach, solid state battery with application to improve the safety of lithium ion battery
Cathode alkali metal can be used directly more can further be promoted the energy density of battery, however it is inorganic with high ionic conductivity
Solid electrolyte bad mechanical property, interface impedance are big；Lower with organic solid-state electrolyte ion conductivity flexible, low temperature makes
It is small with potentiality, and stability is poor at high temperature.
Summary of the invention
The problems such as poor for conductivity low and high temperature stability under solid polyelectrolyte low temperature in the prior art, this hair
First bright purpose is to be to provide a kind of polymer solid electricity in wide temperature range with good chemical property
Xie Zhi.
Second object of the present invention is to be that providing the wide warm polymer for preparing that a kind of step is simple, at low cost consolidates
The method of state electrolyte.
Third object of the present invention is to provide a kind of application method of wide warm polymer dielectric, as electrolysis
Matter be applied to all solid state alkali or alkaline earth metal battery, it is available can be worked normally in wide temperature range it is all solid state
Alkali or alkaline earth metal battery.
In order to achieve the above technical purposes, the present invention provides a kind of preparation method of wide warm solid polyelectrolyte,
This method is that agar derivative and crosslinking agent are carried out cross-linking reaction, obtains cross-linked matrix；By cross-linked matrix and alkali metal salt or
Alkali salt it is compound to get.
The present invention, which is crosslinked by using agar derivative with crosslinking agent, to react, and forms network cross-linked macromolecular, then will
After crosslinked is mixed with alkali metal salt or alkali salt, solvent flashing obtains all solid state electrolyte, alkali metal salt or alkaline earth gold
Belong to salt and is crosslinked macromolecular dissolution comprising wherein, all-solid-state battery being assembled into using all solid state electrolyte, in wide temperature model
Conduction of the metal ion inside electrolyte can be carried out in enclosing, and complete circulating battery.General agar derivative itself is a kind of
Linear polymer, mainly assembles to form three-dimensional net structure with double helix, can also although it can form gel at normal temperature
With film, but its temperature range adapted to is limited, the higher or lower stability and mechanical property that can all destroy gel of temperature.
Key of the invention be to carry out it by using crosslinking agent as basis material using agar derivative it is cross-linking modified, it is logical
After crossing crosslinking, the height temperature stability of its three-dimensional net structure is further enhanced by chemical bond, while being crosslinked the big of generation
The ether-oxygen bond of amount increases the low temperature flexibility of crosslinked, solves the problems, such as that its low temperature properties is crisp, while being introduced greatly by being crosslinked
Oxygen, the hetero atoms such as nitrogen are measured, with diversion subchannel is formed inside three-dimensional net structure agar derivative, to ensure that agar
Have under the stability of derivative high/low temperature and its high/low temperature and preferably leads ionic nature.
Preferred scheme, the agar derivative include at least one of agarose, agar pectin and agarose derivative.
Agarose derivative such as Ago-Gel.
Preferred scheme, the crosslinking agent, which is selected from, contains titanyl, borine radical, siloxy, carboxyl, amino, epoxy group, acyl
At least one of chlorine, acid anhydrides, hydroxyl and carbon-carbon double bond or three keys can with hydroxyl occur condensation (as dehydration, dealcoholysis), addition or
The compound of the functional group of reaction is replaced, to remove the main chain of the hydrogen-oxygen key and growth polymers matrix in agar derivative.
It is common such as 3- (the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, borine-tetrahydrofuran, isopropyl titanate, poly- methyl hydrogen
Siloxanes, aniline, epoxy resin and polyacrylic acid etc..
Preferred scheme, the ratio between agar derivative and crosslinking agent mole are 10:1~1:5, agar derivative and crosslinking agent
Mole with it includes active function groups metering.Crosslinker ratio is excessively high, then is difficult to be formed under high/low temperature condition and stablizes
Solid film, be likely to be at liquid, if very few, crosslinking degree is reduced, and hydrogen-oxygen key is more in agar, and battery is difficult to stablize, and
The solubility of lithium salts is reduced, ionic conductivity reduces.More preferably ratio is hydrogen-oxygen key functional group in agar sugar unit
Amount is 0.5~1.5:1, most preferably 1:1 with the amount for the functional group that can be reacted with hydroxyl in crosslinking agent.
Preferred scheme, the temperature of the cross-linking reaction are 25 DEG C~120 DEG C, and the reaction time is 2h~for 24 hours.Temperature is excessively high
Can make agar gelatinization denaturation, if temperature is too low, cross-linking reaction is incomplete, preferably at 80 DEG C~100 DEG C, the reaction time be 6h~
12h。
Preferred scheme, the solvent that the cross-linking reaction uses in the process is the polar solvent of not hydroxyl, such as N- methyl
Pyrrolidones, dimethyl sulfoxide, formamide etc..
The mass ratio of preferred scheme, cross-linked matrix and alkali metal salt is 1:5~10:1.Alkali metal salt content excessively can not
The film with mechanical stability is formed, the content of alkali metal salt is too low, then the lithium ion content in electrolyte reduces, ionic conductance
Rate can decline.The preferred mass ratio of cross-linked matrix and alkali metal salt or alkali salt is 1:1~5:1.Alkali metal salt or alkaline earth
It using alkali metal or alkaline-earth metal as the organic or inorganic salt of cation composition includes M (ClO that metal salt, which is conventional,4)x、M
(NO3)x、M3Nx、M(BF4)x、M(BF3Cl)x、M(PF6)x、M(X)x, boryl class alkali or alkaline earth metal salt, sulfonate alkali metal or
Alkali salt, alkali alkyl or alkali salt, imines alkali or alkaline earth metal salt, phosphorous organic alkali metal or alkaline earth
(alkali metal such as M Li, Na, K, corresponding x are the alkaline-earth metal such as 1 either Mg, Zn at least one of metal salt, 2) corresponding x is.
Preferred scheme, cross-linked matrix are compound by liquid phase method with alkali metal salt or alkali salt.It specially will crosslinking
After matrix is mixed with alkali metal salt or alkaline-earth metal salt solution, 25~120 DEG C of 2~48h of drying and volatilizing solvent are compound to get arriving
Body.
The present invention provides a kind of wide warm solid polyelectrolytes, are prepared by the above method.
Preferred scheme, it is ionic that there is the wide temperature solid electrolyte height to lead in -40 DEG C~120 DEG C temperature ranges,
So-called height lead it is ionic, for being relatively common solid electrolyte, common solid electrolyte just have at high temperature compared with
High ionic conductivity, and the warm solid polyelectrolyte of width of the invention not only has at room temperature and preferably leads ionic, such as exists
Its ionic conductivity is up to 10 at room temperature-4~10-3S cm-1, 2~4 orders of magnitude are improved compared to common PE O base electrolyte, are leaned on
Closely -40 DEG C still all have and preferably lead ionic, and conductivity at high temperature is also above general electrolyte.
The present invention also provides a kind of applications of wide warm solid polyelectrolyte, are applied to all solid state alkali metal battery
Or all solid state alkaline earth metal batteries.
In preferred scheme, the anode of all-solid-state battery can be lithium ion anode, sodium ion anode, sulphur anode, magnesium from
Sub- anode etc., cathode can be the various cathode such as cathode of lithium, sodium cathode, silicium cathode, tin cathode etc. to match with anode, assembling
At all-solid-state battery within the scope of -40~120 DEG C can normal circulation all-solid-state battery.
Compared with the existing technology, it is the advantages of technical solution of the present invention:
The warm solid polyelectrolyte of width of the invention still maintains preferable flexible and higher in wide temperature range
Ionic conductivity, and preparation process is easy to operate, at low cost, easily controllable；It is electrolysed using the warm polymer solid of width of the invention
The all-solid-state battery of matter assembling is suitable for the long-term stable operation in wide temperature range.
The raw material of the warm solid polyelectrolyte of width of the invention is easy to get, and preparation method is simple, is conducive to industrialized production.
Detailed description of the invention
Fig. 1 is electrolytic conductivity curve made from present example 1.
Fig. 2 is electrolyte electrochemical window made from present example 1.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the claims in the present invention protection scope.
Embodiment 1
0.5g agarose is taken, 12g N-Methyl pyrrolidone controls 90 DEG C of stirrings under protection of argon gas, until agarose is complete
Then fully dissolved is added 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane of 0.58384g, reacts 12 hours at 90 DEG C,
It obtains cross-linked matrix, is added and product is transferred to glove box is added after 1.08384g LiTFSI stirring and dissolving that obtain electrolyte molten
Liquid.By electrolyte solution at 60 DEG C after dry solidification 12h gained dielectric film, dress up steel-steel button cell, -20 DEG C~
100 DEG C of measurement ionic conductivities are as shown in Figure 1；Lithium is assembled into -20 DEG C of steel battery testing of electrochemistry using dielectric film
Window, as shown in Figure 2.
Embodiment 2
Using different agarose derivatives, 1g agar pectin is taken to be placed in three-necked flask, stirred for 60 DEG C under protection of argon gas
30min, stirring rate 500r/min are mixed, 1.16768g 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane is then added
It is reacted 10 hours at 25 DEG C, obtains cross-linked matrix, solution is transferred in glove box, 1.66768g KPF is added6It stirs molten
Electrolyte solution is obtained after solution.By electrolyte solution at 100 DEG C electricity of the gained dielectric film at 120 DEG C after dry solidification 8h
Conductance is 9.34 × 10-4S/cm。
Embodiment 3
Using different crosslinking agents, 0.5g agarose is taken, 12g N-Methyl pyrrolidone stirs for 90 DEG C under protection of argon gas,
Until agarose is completely dissolved, then the isopropyl titanate of addition 0.2262g, reacts 12 hours at 90 DEG C, obtains crosslinking group
Body is added after product is transferred to glove box addition 0.7262g LiTFSI stirring and dissolving and obtains electrolyte solution.By electrolyte
Solution at 70 DEG C after dry solidification 10h gained dielectric film, be assembled into lithium-steel battery, the electrochemical window at 120 DEG C
For 4.3V.
Embodiment 4
Using the different degrees of cross linking, 0.5g agarose is taken, 12g N-Methyl pyrrolidone controls 90 DEG C under protection of argon gas and stirs
It mixes, until agarose is completely dissolved, then addition 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, reacts 12 at 90 DEG C
Hour, cross-linked matrix is obtained, is added after product is transferred to glove box addition LiTFSI stirring and dissolving and obtains electrolyte solution, it will
Dielectric film obtained by electrolyte solution dry solidification at 60 DEG C is rear for 24 hours.When the molar ratio of crosslinking agent and agarose is 3:4 (fine jade
When the amount of hydrogen-oxygen key functional group and the amount for the functional group that can be reacted with hydroxyl in crosslinking agent are 1:1 in lipolysaccharide unit), in room temperature
Under conductivity reach 3.42 × 10-3S/cm, when the molar ratio of crosslinking agent and agarose is 10:1, conductivity at room temperature is only
It is 5.13 × 10-7S/cm, when crosslinking agent is 1:5 with agar sugar unit molar ratio, it is difficult to drying film forming.
Embodiment 5
Take 0.5g agarose, the 90 DEG C of stirrings under protection of argon gas of 12g dimethyl sulfoxide, until agarose is completely dissolved, so
3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane of 0.58384g is added afterwards, reacts 12 hours, is crosslinked at 90 DEG C
Matrix is added product being transferred to glove box addition 1.08384g NaCF3SO3Electrolyte solution is obtained after stirring and dissolving.It will be electric
Electrolyte solution gained dielectric film after 80 DEG C of dry solidification 12h on hot plate, is anode with sulphur, Na is cathode, is assembled into knob
Battery is detained, the first circle specific discharge capacity at 60 DEG C is 1135mAh/g, and first circle charge specific capacity is 786mAh/g.
Claims (10)
1. a kind of preparation method of wide warm solid polyelectrolyte, it is characterised in that: agar derivative is handed over crosslinking agent
Connection reaction, obtains cross-linked matrix；By cross-linked matrix and alkali metal salt or alkali salt it is compound to get.
2. a kind of preparation method of wide warm solid polyelectrolyte according to claim 1, it is characterised in that: the fine jade
Rouge derivative includes at least one of agarose, agar pectin and agarose derivative.
3. a kind of preparation method of wide warm solid polyelectrolyte according to claim 1, it is characterised in that: the friendship
Connection agent, which is selected from, contains titanyl, borine radical, siloxy, carboxyl, amino, epoxy group, acyl chlorides, acid anhydrides and carbon-carbon double bond or three keys
At least one of the active function groups that condensation, addition or displacement be reacted can occur with hydroxyl have a compound.
4. a kind of preparation method of described in any item wide warm solid polyelectrolytes, feature exist according to claim 1~3
In: the ratio between agar derivative and crosslinking agent mole are 10:1~1:5, and the mole of agar derivative and crosslinking agent is with its packet
The active function groups metering contained.
5. a kind of preparation method of described in any item wide warm solid polyelectrolytes, feature exist according to claim 1~3
It is 25 DEG C~120 DEG C in: the temperature of the cross-linking reaction, the reaction time is 2h~for 24 hours.
6. a kind of preparation method of described in any item wide warm solid polyelectrolytes, feature exist according to claim 1~3
In: the mass ratio of cross-linked matrix and alkali metal salt or alkali salt is 1:5~10:1.
7. a kind of preparation method of described in any item wide warm solid polyelectrolytes, feature exist according to claim 1~3
In: cross-linked matrix is compound by liquid phase method with alkali metal salt or alkali salt.
8. a kind of wide warm solid polyelectrolyte, it is characterised in that: be prepared by any one of claim 1~7 method.
9. a kind of wide warm solid polyelectrolyte according to claim 8, it is characterised in that: the wide warm solid state electrolysis
It is ionic that there is matter height to lead in -40 DEG C~120 DEG C temperature ranges.
10. a kind of application of wide warm solid polyelectrolyte according to claim 8 or claim 9, it is characterised in that: be applied to
All solid state alkali metal battery or all solid state alkaline earth metal batteries.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113140787A (en) * | 2021-03-23 | 2021-07-20 | 上海电气集团股份有限公司 | Solid electrolyte with wide temperature range and application thereof |
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Application publication date: 20190705 |