CN110265714A - A kind of Ionomer electrolyte and its preparation method and application - Google Patents
A kind of Ionomer electrolyte and its preparation method and application Download PDFInfo
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- CN110265714A CN110265714A CN201910497191.XA CN201910497191A CN110265714A CN 110265714 A CN110265714 A CN 110265714A CN 201910497191 A CN201910497191 A CN 201910497191A CN 110265714 A CN110265714 A CN 110265714A
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- preparation
- ether
- ketone
- electrolyte
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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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
-
- 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 discloses a kind of Ionomer electrolytes and its preparation method and application.Preparation method of the invention includes the following steps: that polyether-ether-ketone sulfonation 1) is obtained sulfonated polyether-ether-ketone；2) ionization step 1) obtained sulfonated polyether-ether-ketone.A kind of Ionomer electrolyte is prepared by above-mentioned preparation method.A kind of battery diaphragm, the Ionomer electrolyte preparation of preparation method preparation from the above mentioned.The battery diaphragm of diaphragm material preparation of the invention has higher thermal dimensional stability；The diaphragm material has various polarity group, so that its better compatibility with polar liquid electrolyte；In addition, such material itself has ionic conduction characteristic, ionic conductivity can be effectively improved；And since sulfonate radical anion is suspended on polymer backbone, such polymer electrolyte diaphragm material shows single-ion conductor characteristic, the transference number of ions of polymer dielectric can be made to be highly improved as battery diaphragm.
Description
Technical field
The present invention relates to energy storage device technical field more particularly to a kind of Ionomer electrolyte and its preparations
Methods and applications.
Background technique
Although the research and development of advanced energy storage device are the research emphasis of the important research personnel of global materials science field.It is modern
Electrochemistry is over the last couple of decades.Lithium ion battery provides power for most portable devices, and overcomes and permitted
Difficulty of more high-energy density equipment in large-scale use.
With diaphragm, the development of electrode fabrication, the shape of lithium ion battery can thin down (most thin can be with
Accomplish 0.5mm), this battery for also making it possible to prepare various shapes, size, capacity.At the same time, polymer Li-ion
The energy of battery is also far more than common lithium ion battery, compared to conventional lithium ion battery, capacity, charge-discharge characteristic, peace
There has also been be greatly improved for the performances such as Quan Xing, cycle life.Widely used diaphragm is mainly based upon poly- second currently on the market
The polyolefin-based separator of alkene (PE) and polypropylene (PP).This kind of diaphragm is cheap, preparation process is simple and fast, be used as battery every
Good cycle, specific capacity are high when film.But there is also some problems simultaneously, such as: high temperature resistance is bad, thermal contraction is big and electricity
Wellability difference and the conductivity for solving matter are low etc..Therefore, it is particularly significant to battery performance is promoted to develop new diaphragm system.
Summary of the invention
It is an object of the present invention to be directed to the above-mentioned deficiency of the prior art, a kind of Ionomer electrolysis material is proposed
Material and its preparation method and application.
1) a kind of preparation method of Ionomer electrolyte of the invention, includes the following steps: polyethers ether
Ketone sulfonation obtains sulfonated polyether-ether-ketone；2) ionization step 1) obtained sulfonated polyether-ether-ketone.
Preferably, the sulfonation degree for the sulfonated polyether-ether-ketone that step 1) obtains is 40%-95.0%.
Preferably, step 1) uses concentrated acid sulfonation polyether-ether-ketone.
Preferably, using the concrete operations of concentrated acid sulfonation polyether-ether-ketone: dense sulphur will be added in dried polyether-ether-ketone
In acid, it is stirred to react a period of time at a certain temperature, reaction solution is slowly poured into ice water, stirring is predominate on one side
Enter, until white stringy solids all separate out；Filtrate is removed in filtering, retains filter cake；In being with UP water washing to cleaning solution
Property, re-dry filter cake.
Preferably, sulfonated polyether-ether-ketone is ionized using the aqueous slkali that metal cation and hydroxyl are formed in step 2).
Preferably, step 2) comprises the concrete steps that for sulfonated polyether-ether-ketone to be added in certain density aqueous slkali and stirs one
Guarantee solution alkaline after the section time and alkalinity does not change for a long time；Filtering solution, by the solid being obtained by filtration wash to
It is dry after neutrality.
Preferably, the metal cation be lithium ion, potassium ion, sodium ion, magnesium ion, aluminium ion, zinc ion, manganese from
One of son, mercury ion, cadmium ion and nickel ion.
A kind of Ionomer electrolyte is prepared by above-mentioned preparation method.
A kind of battery diaphragm, the Ionomer electrolyte preparation of preparation method preparation from the above mentioned.
The preparation method of above-mentioned a kind of battery diaphragm, using solution casting method, method of electrostatic spinning, phase transfer method or template
Method preparation.
Polyether-ether-ketone is prepared a kind of heavy-duty battery polymerization by two steps of simple sulfonation and ionization by the present invention
Object electrolyte, the temperature and time by controlling sulfonation obtains different sulfonation degrees, by the exchange of different metal ions,
Obtain can be applied to the polymer dielectric of different batteries, including lithium ion battery, sodium-ion battery, kalium ion battery, zinc from
Sub- battery, Magnesium ion battery etc..It is prepared due to polyether-ether-ketone fusing point with higher, such polymer electrolyte diaphragm material
Battery diaphragm has higher thermal dimensional stability.Such polymer electrolyte diaphragm material has various polarity group, such as C=
O, O and SO3- etc., so that such material has the preferably compatibility with polar liquid electrolyte.In addition, such material itself
With ionic conduction characteristic, ionic conductivity can be effectively improved.Finally, due to which sulfonate radical anion is suspended in polymer backbone
On, such polymer electrolyte diaphragm material shows single-ion conductor characteristic, there is very high metal ion transport number, as
Battery diaphragm can make the transference number of ions of polymer dielectric be highly improved.
Detailed description of the invention
Fig. 1 is the hot weight curve of electrolyte membrance prepared by the embodiment of the present invention 1；
Fig. 2 is the hot dimensionally stable test chart of electrolyte membrance prepared by the embodiment of the present invention 1；
Fig. 3 is the contact angle test figure of electrolyte membrance prepared by the embodiment of the present invention 1；
Fig. 4 is the electrochemical window figure of electrolyte membrance prepared by the embodiment of the present invention 1；
Fig. 5 is the diaphragm and Li-SPEEK of electrolyte membrance prepared by the embodiment of the present invention 1 and commercialization electrolyte preparation
Spinning film adds the comparison diagram of the conductivity after business electrolyte；
Fig. 6 is the lithium ion transference number figure of electrolyte membrance prepared by the embodiment of the present invention 1；
Fig. 7 is the lithium ion transference number figure of PP/ commercialization electrolyte membrance；
Fig. 8 is the lithium ion transference number figure after Li-SPEEK spinning film addition commercialization electrolyte.
Specific embodiment
Following is a specific embodiment of the present invention in conjunction with the accompanying drawings, technical scheme of the present invention will be further described,
However, the present invention is not limited to these examples.
Embodiment 1
Prepare sulfonated polyether-ether-ketone: by 10g through dense sulphur 100mL is added in 60 DEG C of dried polyether-ether-ketones of vacuum drying oven,
The heating stirring 5h at 38 DEG C, heating stirring 3h at 50 DEG C, heating stirring 2h at 55 DEG C, to after the reaction was completed, be cooled to room temperature,
Above-mentioned reaction solution is slowly poured into mixture of ice and water, is poured into while stirring, until white stringy solids are all analysed
Out；Filtrate is removed in filtering, retains filter cake.With UP water washing to neutrality, at 60 DEG C of convection oven after dry 48h and 80
It is dried in vacuo at DEG C spare for 24 hours.
Ionization sulfonated polyether-ether-ketone: being added 20mL1mol/L lithium hydroxide solution and stir 2h, if solution detects after 2h
For acidity, then plus lithium hydroxide solution in right amount, until solution is that alkalinity does not change after alkalinity and stirring enough time.And it will
Solid is washed to neutrality, is dried in vacuo at 60 DEG C of convection oven after dry 48h and at 80 DEG C and is obtained Ionomer electricity for 24 hours
It is spare to solve material.
It prepares diaphragm: the Ionomer electrolyte of above-mentioned preparation being dissolved in N,N-dimethylformamide and forms concentration point
The uniform viscous fluid that number is 29%, then formed a film by electrostatic spinning.
Performance evaluation:
1. thermogravimetric analysis: using intelligent thermogravimetric analyzer (STA409PC, Germany NETZSCH) to polymer thermostable
It is analyzed.In N2Under atmosphere protection, from room temperature to 800 DEG C, heating rate is 10 DEG C of min-1.Measure sample quality and temperature
Spend change curve.
As shown in Figure 1, the thermal decomposition temperature of diaphragm manufactured in the present embodiment is at 450 DEG C or more as seen from Figure 1, completely
Meet requirement of the battery to temperature.
2. thermal dimensional stability is analyzed: diaphragm being put on a glass, is heated using heating plate, records diaphragm respectively
Half an hour is placed at room temperature, 50 DEG C, 100 DEG C, 150 DEG C and 200 DEG C, sees that the diameter of film shrinks the form of situation diaphragm.
As shown in Fig. 2, as can be seen from the figure diaphragm manufactured in the present embodiment has preferable thermal dimensional stability energy,
Phenomenon is heat-shrinked without apparent at 200 DEG C.
3. contact angle test: using the contact angle measurement of model JC2000D, drawing electrolyte with micro syringe
EC/DMC 1 drips the contact angle that PP film and Li-SPEEK film are taken pictures and measured respectively on diaphragm, after 3s.
As shown in figure 3, it can be seen from the figure that completing electrolysis in 3s by the diaphragm of the invention that method of electrostatic spinning obtains
The complete wetting of liquid, good wellability derive from the polar group of such material, have good with polarity liquid electrolyte
Compatibility.
4. electrochemical window: the electrolyte membrance that diameter is 19mm being placed on EC/DMC (v:v=1:1) mixed solvent and is impregnated
3 days, then for stainless steel substrates as working electrode, lithium piece was reference electrode, according to the device knot of " lithium piece | diaphragm | stainless steel substrates "
Structure assembled battery.Test scope is that -0.5V arrives 5V, and sweeping speed is 1mV s-1。
As shown in figure 4, saying it can be seen from the figure that oxidation peak does not occur in diaphragm manufactured in the present embodiment within 5V
Bright diaphragm manufactured in the present embodiment has very high electrochemical stability, can be applied in multiple battery, such as LiFePO4, cobalt
Sour lithium, LiMn2O4 even need in high-tension battery.
5. ionic conductivity: use electrochemical alternate impedance spectrum, scan frequency be 1MHz to 1Hz, oscillating voltage 10mV,
Measure required impedance value.Test temperature is 25 DEG C (room temperature) to 80 DEG C.The electrolyte membrance that diameter is 16mm is immersed in EC/
The in the mixed solvent of DMC (v:v=1:1) is taken out after 3 days and is clipped in the survey for being assembled into sandwich structure among two stainless steel wafers
Trial assembly is set, i.e., " stainless steel substrates | diaphragm | stainless steel substrates ".Conductivity is calculated using following equation:
L is the thickness (cm) of diaphragm, and R is the impedance (Ω) that EIS measures diaphragm, and A is effective contact area of diaphragm
(cm2)。
From fig. 5, it can be seen that Li-SPEEK diaphragm prepared by the present embodiment 1 itself shows higher ionic conductivity,
After adding business electrolyte, ionic conductivity more higher than conventional polyolefins diaphragm is shown.
6. lithium ion transference number: measuring lithium ion transference number using steady-state current method, give a very small polarization electricity
Pressure, and the impedance of rear (i.e. before and after lithium electrode passivation layer formation) difference test device before testing, frequency is 1MHz to 100Hz.
The electrolyte membrance that diameter is 19mm is placed on EC/DMC (v:v=1:1) mixed solvent to impregnate 3 days, is then assembled into " lithium piece
| diaphragm | lithium piece " battery structure.Transference number of ions t+ is calculated by following equation:
Δ V is the polarizing voltage of setting, I0And ISRespectively indicate initial current and steady-state current, R0And RSIndicate lithium electrode
Resistance when passivation layer initial resistance and stable state.
From fig. 6, it can be seen that the lithium ion transference number of Li-SPEEK spinning film prepared by the present embodiment 1 is 0.89, performance
Single-ion conductor characteristic out.Fig. 7 is that PP/ is commercialized electrolyte membrance, and the lithium ion transference number of the electrolyte system is only 0.28,
Show bi-ion conductor characteristic.Fig. 8 is the lithium ion transference number after Li-SPEEK spinning film addition commercialization electrolyte, from figure
In it is found that the lithium ion transference number of the system is 0.52, almost PP/ is commercialized twice of electrolyte membrance, illustrates single ion
The Li-SPEEK diaphragm of conduction helps to improve the lithium ion transference number of electrolyte.
In conclusion case study on implementation 1 of the invention provides a kind of Ionomer electrolysis that can be used for battery diaphragm
Matter, the film build method of the electrolyte membrance are method of electrostatic spinning, the polymer dielectric filmogen sulfonated polyether-ether-ketone
With high thermal decomposition temperature and high thermal dimensional stability, the excellent thermal stability of obtained polymer dielectric can guarantee.
It is same in the fiber filaments after the film forming raw material is ionized meanwhile under conditions of guarantee diaphragm excellent thermal stability
Containing lithium ion, lithium ion transference number to improve lithium ionic mobility and conductivity and is then increased with this.
It is not directed to place above, is suitable for the prior art.
Although some specific embodiments of the invention are described in detail by example, the skill of this field
Art personnel it should be understood that above example merely to be illustrated, the range being not intended to be limiting of the invention, belonging to the present invention
Those skilled in the art can make various modifications or additions to described specific embodiment or using class
As mode substitute, but without departing from direction of the invention or beyond the scope of the appended claims.Ability
Domain it is to be understood by the skilled artisans that according to the technical essence of the invention to made by embodiment of above it is any modification, etc.
With replacement, improvement etc., protection scope of the present invention should be included in.
Claims (10)
1. a kind of preparation method of Ionomer electrolyte, characterized by the following steps: 1) by polyethers ether
Ketone sulfonation obtains sulfonated polyether-ether-ketone；2) ionization step 1) obtained sulfonated polyether-ether-ketone.
2. a kind of preparation method of Ionomer electrolyte as described in claim 1, it is characterised in that: step 1)
The sulfonation degree of obtained sulfonated polyether-ether-ketone is 40%-95.0%.
3. a kind of preparation method of Ionomer electrolyte as described in claim 1, it is characterised in that: step 1)
Using concentrated acid sulfonation polyether-ether-ketone.
4. a kind of preparation method of Ionomer electrolyte as claimed in claim 3, it is characterised in that: using dense
The concrete operations of sulfuric acid sulfonation polyether-ether-ketone: it will be added in the concentrated sulfuric acid in dried polyether-ether-ketone, stir at a certain temperature
Reaction a period of time, reaction solution is slowly poured into ice water, is poured into while stirring, until white stringy solids are whole
It separates out；Filtrate is removed in filtering, retains filter cake；It is neutral, re-dry filter cake with UP water washing to cleaning solution.
5. a kind of preparation method of Ionomer electrolyte as described in claim 1, it is characterised in that: step 2)
The middle aqueous slkali formed using metal cation and hydroxyl ionizes sulfonated polyether-ether-ketone.
6. a kind of preparation method of Ionomer electrolyte as claimed in claim 5, it is characterised in that: step 2)
Comprise the concrete steps that sulfonated polyether-ether-ketone is added in certain density aqueous slkali stir a period of time after guarantee solution in alkali
Property and for a long time alkalinity do not change；Filtering solution is dried after washing the solid being obtained by filtration to neutrality.
7. a kind of preparation method of Ionomer electrolyte as claimed in claim 5, it is characterised in that: the gold
Belonging to cation is lithium ion, potassium ion, sodium ion, magnesium ion, aluminium ion, zinc ion, manganese ion, mercury ion, cadmium ion and nickel
One of ion.
8. a kind of Ionomer electrolyte, it is characterised in that: by the described in any item preparation methods of claim 1-7
Preparation.
9. a kind of battery diaphragm, it is characterised in that: gathered by the ionic of the described in any item preparation method preparations of claim 1-7
The preparation of polymer electrolyte material.
10. a kind of preparation method of battery diaphragm as claimed in claim 9, it is characterised in that: use solution casting method, electrostatic
Spin processes, phase transfer method or template preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694581A (en) * | 2020-12-25 | 2021-04-23 | 苏州大学附属第一医院 | Lithium-loaded three-dimensional microporous sulfonated polyether ether ketone, preparation method and application thereof |
| 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 |
| CN113299986A (en) * | 2021-05-24 | 2021-08-24 | 东莞新能安科技有限公司 | Electrolyte membrane, and electrochemical device and electronic device comprising same |
| 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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| CN108565384A (en) * | 2018-05-28 | 2018-09-21 | 中国地质大学（武汉） | A kind of preparation method and application of sulfonated polyether-ether-ketone lighium polymer electrolyte membrance |
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| CN112694581A (en) * | 2020-12-25 | 2021-04-23 | 苏州大学附属第一医院 | Lithium-loaded three-dimensional microporous sulfonated polyether ether ketone, preparation method and application thereof |
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| CN113299986A (en) * | 2021-05-24 | 2021-08-24 | 东莞新能安科技有限公司 | Electrolyte membrane, and electrochemical device and electronic device comprising same |
| 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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