CN106129468A - A kind of preparation method of single-ion polymer gel electrolyte materials - Google Patents
A kind of preparation method of single-ion polymer gel electrolyte materials Download PDFInfo
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- CN106129468A CN106129468A CN201610555927.0A CN201610555927A CN106129468A CN 106129468 A CN106129468 A CN 106129468A CN 201610555927 A CN201610555927 A CN 201610555927A CN 106129468 A CN106129468 A CN 106129468A
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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 present invention relates to the preparation method of a kind of single-ion polymer gel electrolyte materials, boric acid and Lithium hydrate are dissolved in deionized water, oil bath pan heats；Being added by dipropylene glycol aqueous solution in solution, heat up, stirring carries out polyreaction；Adding hexamethylene in polymerization system, utilize the water being azeotroped off in system, the white precipitate obtained is polymerizate；Polymerizate is collected by filtration, in vacuum drying, obtains white powder, be single-ion polymer electrolyte；By polymer electrolyte and Kynoar hexafluoropropene) copolymer is dissolved in dimethylformamide, and reheat and make solvent volatilization obtain dielectric film；Dielectric film is soaked in electrolyte Allyl carbonate, obtains single-ion polymer gel electrolyte membrane.Preparation method of the present invention is simple, and ionic conductivity has brought up to 1.2～2.0S cm‑1, lithium ion transference number has brought up to 0.85～0.91.
Description
Technical field
The present invention relates to the preparation method of a kind of single-ion polymer gel electrolyte materials, specifically by a contracting two
Propylene glycol, boric acid and Lithium hydrate are polymerized in aqueous, then by film forming and the preparation method of gelation process.
Technical background
Compared with traditional secondary cell (Ni-MH battery, nickel-cadmium cell etc.), lithium rechargeable battery have specific energy high,
Have extended cycle life, advantages of environment protection, therefore become a kind of important electrochmical power source.But, traditional lithium ion battery makes
Be volatile organic electrolyte, such as dimethyl carbonate (DMC), diethyl carbonate (DEC), vinyl carbonate (EC)
Deng, although there is the highest ionic conductivity, but inflammable volatile due to it, the user at lithium ion battery exists many
Potential safety hazard (as burnt, exploding, leakage etc.).In order to overcome this defect, there has been proposed and substitute with polymer dielectric
Electrolyte (Wu Yuping, Dai Xiaobing, horse army flag, the pre-river of journey " lithium ion battery applications with put into practice ". Beijing chemical industry is published
Society, 2004, pp.301).
But there are two problems in simple polymer dielectric: one be the lithium ion transference number of polymer dielectric very
Low, charge and discharge process easily produces concentration difference, forms Li dendrite, cause the short circuit of battery；Two is polymer dielectric ion
Conductivity is the lowest, and the ionic conductivity of the most simple polymer dielectric is not met by the actual application of lithium battery.In order to
Solve the low problem of lithium ion transference number, it is proposed that the concept of single-ion polymer electrolyte, refer to be fixed on anion poly-
On compound main chain, only cation migrates.This single ion conductor anion is fixed on main polymer chain, in charge and discharge
Electric process will not produce concentration polarization because zwitterion migration velocity is different, therefore there is the highest lithium ion mobility
Number, it is possible to effectively avoid the formation of Li dendrite, improves the performance of lithium ion battery.In order to solve low the asking of ionic conductivity
Topic, it is proposed that the concept of gel polymer electrolyte, it is simply that add minimal amount of organic electrolyte in polymeric system, thus
Improve its ionic conductivity.Therefore, the appearance of single-ion polymer gel electrolyte materials, it is possible to from lithium ion transference number and from
Two aspects of electronic conduction rate improve the performance of lithium battery.
At present, the most many researcheres have done many research work in terms of single-ion polymer gel electrolyte.Zhu
Deng with PVA and boric acid, oxalic acid carry out complexation polyreaction obtain single-ion polymer (Zhu Y S, Wang X J, Hou Y Y,
et al.A new single-ion polymer electrolyte based on polyvinyl alcohol for
Lithium ion batteries [J] .Electrochimica Acta, 2013,87 (1): 113-118.) but, due to PVA
Being semicrystalline structure, under room temperature, the transport number of lithium ion is close to 1, and ionic conductivity is only capable of reaching 6.11 × 10-6s cm-1。Wang
Single-ion polymer (Wang X, Liu Z, Kong Q, et al.A has been obtained Deng with tartaric acid and boric acid complex reaction
single-ion gel polymer electrolyte based on polymeric lithium tartaric acid
borate and its superior battery performance[J].Solid State Ionics,2014,262
(9):747-753.).Owing to the ether-oxygen bond on polymer is present on ring, motor capacity is poor, is unfavorable for the migration of lithium ion,
Room temperature ionic conductivity can reach 1.4 × 10-4s cm-1, lithium ion transference number is close to 1, but high rate performance is poor.In order to
Making polymerization process easy, electrolyte excellent performance, the present invention synthesizes on a kind of main chain the most in aqueous with ether-oxygen bond
Single-ion polymer structure, the motor capacity of ether-oxygen bond is strong, can prepare single-ion polymer gel electrolyte of good performance
Plasma membrane.
Summary of the invention
In order to solve problem of the prior art, the present invention is to use dipropylene glycol, boric acid and Lithium hydrate at aqueous solution
Middle complexation is polymerized, then prepares a kind of single-ion polymer gel electrolyte by film forming and gelation process.
The concrete technical scheme of the present invention is as follows:
The preparation method of a kind of single-ion polymer gel electrolyte materials: comprise the steps:
(1) boric acid and Lithium hydrate are dissolved in deionized water, the amount of the material of boric acid and two kinds of materials of Lithium hydrate it
Ratio is 1:1, heats in oil bath pan；
(2) adding in step (1) gained solution by dipropylene glycol aqueous solution, heat up, stirring carries out polyreaction；
(3) adding hexamethylene in polymerization system, utilize the water being azeotroped off in system, the white precipitate obtained produces for polymerization
Thing；
(4) polymerizate is collected by filtration, in vacuum drying, obtains white powder, be single-ion polymer electrolyte
Material；
(5) by polymer electrolyte and Kynoar-hexafluoropropene) copolymer is dissolved in two by the mol ratio of 1:2
In methylformamide, reheat and make solvent volatilization obtain dielectric film；Dielectric film is soaked in electrolyte Allyl carbonate,
Obtain single-ion polymer gel electrolyte membrane.
The concentration of described step (1) mesoboric acid and lithium hydroxide aqueous solution is 0.1～2mol/L, and heating-up temperature is 40～60
℃。
In described step (2), the concentration of dipropylene glycol aqueous solution is 0.2～4mol/L, dipropylene glycol molal quantity
Twice equal to boric acid molal quantity.
In described step (2), polymerization reaction time is 16～24h, and reaction temperature is 80 DEG C～100 DEG C.
Described step (3) adds hexamethylene in the ratio adding 60～80mL hexamethylene in every 100mL water.
Described step (4) vacuum drying temperature is 50～60 DEG C, vacuum for-0.1～-0.08MPa, the time be 12～
24h。
Single-ion polymer gel electrolyte membrane is carried out electric performance test, ionic conductivity brought up to 1.2～
2.0S·cm-1, lithium ion transference number has brought up to 0.85～0.91.
Beneficial effects of the present invention: (monomer molar ratio is the present invention with boric acid and diglycol aqueous solution first
1:2, solution concentration is 0.5～1mol/L) at a temperature of 80-100 DEG C, synthesize the isolated son with ether-oxygen bond on a kind of main chain
Polymer architecture, as shown in accompanying drawing 1, accompanying drawing 2.Experiment select Kynoar-hexafluoropropylene copolymer do film former, carbonic acid
Propylene makees plasticizer, and preparation method is simple, simple to operate, obtains pure by the concentration and reaction temperature adjusting reactant
Clean single-ion polymer, is obtaining single-ion polymer gel electrolyte of good performance by film forming and gelation process.
Accompanying drawing explanation
Fig. 1 concentration is the boric acid of 0.5mol/L and diglycol is polymerized under the conditions of 80 DEG C and obtains single-ion polymer
Infrared Characterization figure；
Fig. 2 concentration is the boric acid of 0.5mol/L and diglycol is polymerized under the conditions of 80 DEG C and obtains single-ion polymer
Nuclear-magnetism phenogram；
Fig. 3 concentration is the boric acid of 0.5mol/L and diglycol is polymerized under the conditions of 80 DEG C and obtains single-ion polymer
Gel electrolyte membrane ionic conductivity phenogram.
Detailed description of the invention
In order to make advantages of the present invention, technical scheme and purpose will be apparent from, below in conjunction with example, the present invention is entered
The explanation of one step.Embodiments of the invention are given below, are the model that the present invention further illustrates rather than limits the present invention
Enclose.
Embodiment 1
(1) 0.01mol boric acid and Lithium hydrate are dissolved in the deionized water of 100ml (concentration is 0.1mol/L), 60 DEG C
Stirring is to being completely dissolved；
(2) the dipropylene glycol aqueous solution that 100ml concentration is 0.2mol/L is added dropwise over step (1) gained solution
In, it being warming up to 80 DEG C, stirring carries out polyreaction, reacts 16 hours；
(3) in polymerization system, add hexamethylene in the ratio adding 60mL hexamethylene in every 100mL water, utilize azeotropic former
Water in reason removing system, the white precipitate obtained is polymerizate；
(4) polymerizate is collected by filtration, 50 DEG C, vacuum be-0.08MPa under conditions of be vacuum dried 24 hours,
Obtaining white powder, be single-ion polymer electrolyte, result characterizes as shown in Figure 1, 2.
(5) polymer electrolyte and Kynoar-hexafluoropropylene copolymer are dissolved in diformazan by the mol ratio of 1:2
In base Methanamide, make solvent volatilization obtain dielectric film, dielectric film is soaked in electrolyte Allyl carbonate, obtains isolated
Sub-gel-form solid polymer electrolyte.
Single-ion polymer gel electrolyte carries out electric performance test, and wherein ionic conductivity characterizes as it is shown on figure 3, count
Calculating room temperature ionic conductivity is 2.0 × 10-4S·cm-1, lithium ion transference number is 0.91.
Embodiment 2
(1) 0.03mol boric acid and Lithium hydrate are dissolved in the deionized water of 60ml (concentration is 0.5mol/L), and 40 DEG C are stirred
Mix to being completely dissolved；
(2) the dipropylene glycol aqueous solution that 60ml concentration is 1mol/L is added dropwise in step (1) gained solution, heats up
To 100 DEG C, stirring carries out polyreaction, reacts 24 hours；
(3) in polymerization system, add hexamethylene in the ratio adding 80mL hexamethylene in every 100mL water, utilize azeotropic former
Water in reason removing system, the white precipitate obtained is polymerizate；
(4) polymeric reaction product is collected by filtration, 60 DEG C, vacuum be-0.01MPa under conditions of be vacuum dried 12 little
Time, obtain white powder, be single-ion polymer electrolyte.
(5) polymer electrolyte and Kynoar-hexafluoropropylene copolymer are dissolved in diformazan by the mol ratio of 1:2
In base Methanamide, make solvent volatilization obtain dielectric film, dielectric film is soaked in electrolyte Allyl carbonate, obtains isolated
Sub-gel-form solid polymer electrolyte.
Single-ion polymer gel electrolyte is carried out electric performance test, and calculating the ionic conductivity under room temperature is 1.8
×10-4S·cm-1, lithium ion transference number is 0.88.
Embodiment 3
(1) 0.1mol boric acid and Lithium hydrate are dissolved in the deionized water of 100ml (concentration is 1mol/L), 60 DEG C of stirrings
To being completely dissolved；
(2) the dipropylene glycol aqueous solution that 100ml concentration is 2mol/L is added dropwise in step (1) gained solution, rises
Temperature is to 80 DEG C, and stirring carries out polyreaction, reacts 21 hours；
(3) in polymerization system, add hexamethylene in the ratio adding 60mL hexamethylene in every 100mL water, utilize azeotropic former
Water in reason removing system, the white precipitate obtained is polymerizate；
(4) polymerizate is collected by filtration, 60 DEG C, vacuum be-0.04MPa under conditions of be vacuum dried 20 hours,
Obtain white powder, be single-ion polymer electrolyte.
(5) polymer electrolyte and Kynoar-hexafluoropropylene copolymer are dissolved in diformazan by the mol ratio of 1:2
In base Methanamide, make solvent volatilization obtain dielectric film, dielectric film is soaked in electrolyte Allyl carbonate, obtains isolated
Sub-gel-form solid polymer electrolyte.
Single-ion polymer gel electrolyte is carried out electric performance test, and calculating the ionic conductivity under room temperature is 1.5
×10-4S·cm-1, lithium ion transference number is 0.89.
Embodiment 4
(1) 0.15mol boric acid and Lithium hydrate are dissolved in the deionized water of 100ml (concentration is 1.5mol/L), 50 DEG C
Stirring is to being completely dissolved；
(2) the dipropylene glycol aqueous solution that 100ml concentration is 3mol/L is added dropwise in step (1) gained solution, rises
Temperature is to 90 DEG C, and stirring carries out polyreaction, reacts 24 hours；
(3) in polymerization system, add hexamethylene in the ratio adding 70mL hexamethylene in every 100mL water, utilize azeotropic former
Water in reason removing system, the white precipitate obtained is polymerizate；
(4) polymerizate is collected by filtration, 50 DEG C, vacuum be-0.08MPa under conditions of be vacuum dried 20 hours,
Obtain white powder, be single-ion polymer electrolyte.
(5) polymer electrolyte and Kynoar-hexafluoropropylene copolymer are dissolved in diformazan by the mol ratio of 1:2
In base Methanamide, make solvent volatilization obtain dielectric film, dielectric film is soaked in electrolyte Allyl carbonate, obtains isolated
Sub-gel-form solid polymer electrolyte.
Single-ion polymer gel electrolyte is carried out electric performance test, and calculating the ionic conductivity under room temperature is 1.8
×10-4S·cm-1, lithium ion transference number is 0.85.
Embodiment 5
(1) 0.2mol boric acid and Lithium hydrate are dissolved in the deionized water of 100ml (concentration is 2mol/L), 50 DEG C of stirrings
To being completely dissolved；
(2) the dipropylene glycol aqueous solution that 100ml concentration is 4mol/L is added dropwise in step (1) gained solution, rises
Temperature is to 80 DEG C, and stirring carries out polyreaction, reacts 22 hours；
(3) in polymerization system, add hexamethylene in the ratio adding 60mL hexamethylene in every 100mL water, utilize azeotropic former
Water in reason removing system, the white precipitate obtained is polymerizate；
(4) polymerizate is collected by filtration, 55 DEG C, vacuum be-0.08MPa under conditions of be vacuum dried 23 hours,
Obtain white powder, be single-ion polymer electrolyte.
(5) polymer electrolyte and Kynoar-hexafluoropropylene copolymer are dissolved in diformazan by the mol ratio of 1:2
In base Methanamide, make solvent volatilization obtain dielectric film, dielectric film is soaked in electrolyte Allyl carbonate, obtains isolated
Sub-gel-form solid polymer electrolyte.
Single-ion polymer gel electrolyte is carried out electric performance test, and calculating the ionic conductivity under room temperature is 1.2
×10-4S·cm-1, lithium ion transference number is 0.88.
The present invention is open and proposes to be polymerized with dipropylene glycol, boric acid and Lithium hydrate complexation in aqueous, then leads to
Crossing a kind of method preparing single-ion polymer gel electrolyte of film forming and gelation process, those skilled in the art can be led to
Crossing reference present disclosure, the link such as suitable feed change and process route realizes, although the method for the present invention and technology of preparing are
Being described by preferred embodiment, person skilled substantially can be without departing from present invention, spirit and scope
Methods and techniques described herein route is modified or reconfigures, realizes final technology of preparing.Need especially to refer to
Going out, all similar replacements and change apparent to those skilled in the art, they are considered as bag
Include in present invention spirit, scope and content.
Claims (7)
1. a preparation method for single-ion polymer gel electrolyte materials, is characterized in that specifically comprising the following steps that
(1) boric acid and Lithium hydrate being dissolved in deionized water, the ratio of the amount of the material of boric acid and two kinds of materials of Lithium hydrate is
1:1, heats in oil bath pan；
(2) being added dropwise over by dipropylene glycol aqueous solution in step (1) gained solution, heat up, stirring carries out polyreaction；
(3) adding hexamethylene in polymerization system, utilize the water being azeotroped off in system, the white precipitate obtained is polymerizate；
(4) polymerizate is collected by filtration, in vacuum drying, obtains white powder, be single-ion polymer electrolyte；
(5) polymer electrolyte and Kynoar-hexafluoropropylene copolymer are dissolved in dimethyl methyl by the mol ratio of 1:2
In amide, reheat and make solvent volatilization obtain dielectric film；Dielectric film is soaked in electrolyte Allyl carbonate, obtains list
Ionic polymer gel dielectric film.
2. method as claimed in claim 2, is characterized in that the concentration of described step (1) mesoboric acid and lithium hydroxide aqueous solution is
0.1～2mol/L, heating-up temperature is 40～60 DEG C.
3. method as claimed in claim 2, is characterized in that in described step (2), the concentration of dipropylene glycol aqueous solution is
0.2～4mol/L.
4. method as claimed in claim 2, is characterized in that the dipropylene glycol molal quantity twice equal to boric acid molal quantity.
5. method as claimed in claim 2, is characterized in that in described step (2), polymerization reaction time is 16～24h, reaction temperature
Degree is 80 DEG C～100 DEG C.
6. method as claimed in claim 2, is characterized in that in described step (3) by adding 60～80mL rings in every 100mL water
The ratio of hexane adds hexamethylene.
7. method as claimed in claim 2, is characterized in that described step (4) vacuum drying temperature is 50～60 DEG C, vacuum
Degree is-0.1～-0.08MPa, the time is 12～24h.
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| CN110310842A (en) * | 2018-03-20 | 2019-10-08 | 中天储能科技有限公司 | Electrolyte of high voltage capacitor and preparation method thereof and capacitor element |
| CN111934006A (en) * | 2020-07-23 | 2020-11-13 | 深圳技术大学 | Intrinsically microporous polyaluminum/borate solid electrolytes and batteries |
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| CN110310842A (en) * | 2018-03-20 | 2019-10-08 | 中天储能科技有限公司 | Electrolyte of high voltage capacitor and preparation method thereof and capacitor element |
| CN111934006A (en) * | 2020-07-23 | 2020-11-13 | 深圳技术大学 | Intrinsically microporous polyaluminum/borate solid electrolytes and batteries |
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