CN105304939A - Composite kaolin modified WPU (Waterborne Poly Urethane) solid electrolyte - Google Patents
Composite kaolin modified WPU (Waterborne Poly Urethane) solid electrolyte Download PDFInfo
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- CN105304939A CN105304939A CN201510606971.5A CN201510606971A CN105304939A CN 105304939 A CN105304939 A CN 105304939A CN 201510606971 A CN201510606971 A CN 201510606971A CN 105304939 A CN105304939 A CN 105304939A
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- kaolin
- solid electrolyte
- composite modified
- emulsion
- aqueous polyurethane
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
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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
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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- 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
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- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a composite kaolin modified WPU (Waterborne Poly Urethane) solid electrolyte. The composite kaolin modified WPU solid electrolyte is prepared from nonionic WPU emulsion, hydrophilic modified kaolin and lithium salt. According to the composite kaolin modified WPU solid electrolyte disclosed by the invention, nonionic WPU is adopted as a macromolecule matrix, an operation process is carried out in a water system, a toxic solvent is not used, and the problems of safety and environmental protection during a preparing process and the stability of inorganic ionic salt in the emulsion are solved; hydrophilic modification is carried out on kaolin, the modified kaolin is then coupled to a nonionic WPU structure in a blending way, and the stability problem of inorganic kaolin in the nonionic WPU is solved; the mechanical performance and the ionic conductivity of the nonionic WPU are increased by adding of the kaolin, a problem that the conductivity of traditional PU (Poly Urethane) is low is solved, and the ionic conductivity under the condition of 90 DEG C can be up to 2.61*10<-3> S/cm.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to a kind of solid electrolyte.
Background technology
Lithium ion battery has been widely used in the stored energy etc. in commercialization electronic product, automotive powerplant and power station.The parts forming the key of lithium ion battery comprise positive pole, negative pole, barrier film and electrolyte.Electrolyte is one of key factor affecting integral battery door security and stability.At present, the perishable electrode slice of liquid electrolyte of extensive use thus cause battery capacity irreversible loss, liquid electrolyte easily decomposes generation fuel gas simultaneously, thus causes the severe safety such as fire and blast problem.Adopt solid electrolyte can avoid these drawbacks of liquid electrolyte, and its shape can be cut out arbitrarily and change, and makes the lighter and handier fashion of battery design.
A kind of solid state composite electrolyte and preparation method thereof, preparation process wants high temperature sintering, and energy consumption is comparatively large, and described electrolyte is gel composite electrolyte, needs adion liquid to form gel state.A kind of all solid state composite electrolyte membrane, be raw material with polyethylene glycol oxide, inorganic filler and lithium salts, prepare with solution blended process, poly(ethylene oxide) is the most applicable matrix preparing all solid state electrolyte of generally acknowledging at present, but polyethylene glycol oxide bad mechanical strength, and easily crystallization, cause later stage conductivity less.Full solid state polymer electrolyte membrane preparation method and a prepared dielectric film, use poly(ethylene oxide), liquid crystal polymer etc. containing sulfonate ion, preparation process will use the toxic solvents such as acetonitrile in a large number, not environmentally.A kind of polymer electrolyte, by blending method, polysiloxanes is dispersed in aqueous polyurethane dispersing liquid, and conducting salt is directly dissolved in mixed solution prepares aqueous polyurethane polysiloxanes solid electrolyte, this legal system needs to absorb 5-260% electrolyte for electrolyte and forms gel electrolyte, still can there is the problem that liquid is separated out in gel electrolyte Long-Time Service, and all solid state electrolyte of really.Due to the feature of polymer self, current polymer all solid state electrolyte substantially all will work more than 80 DEG C could show good conductivity, carry out commercial applications, such as France's all-solid lithium-ion battery that business-like pure electric taxi has adopted needs to carry out work at the temperature of 80 DEG C.
Summary of the invention
For the deficiency of the prior art existence that background technology describes, the invention provides a kind of lithium ion battery all solid state electrolyte.
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 80 ~ 97g
Hydrophilic modifying kaolin 2 ~ 10g
Lithium salts 1 ~ 10g;
Described non-ionic water polyurethane emulsion is scattered in water is obtained with reacting ethylenediamine by IPDI, polyoxyethylene glycol, trimethylolpropane-polyethylene glycol monoether, BDO polymerization reaction afterproduct;
Described hydrophilic modifying kaolin is scattered in without the kaolin calcined, titanate coupling agent in absolute ethyl alcohol, then obtain through grinding, oven dry; Described lithium salts is lithium perchlorate.
Described non-ionic water polyurethane emulsion to be scattered in after 6 hours in 200g water 70 DEG C of polymerization reactions by 30.1 IPDIs, 40.3g polyoxyethylene glycol, 15.7g trimethylolpropane-polyethylene glycol monoether, 6.1g1,4-butanediol and within 1 hour, to obtain with 2.0g reacting ethylenediamine; Described non-ionic water polyurethane emulsion is translucent emulsion, pH=7; The basic structure of the non-ionic water polyurethane obtained is:
R in formula
1for IPDI; Structure is:
R in formula
2for trimethylolpropane-polyethylene glycol monoether, mean molecule quantity 1000; Structure is:
R in formula
3for BDO; Structure is :-CH
2cH
2cH
2cH
2-;
R in formula
4for Polyoxypropylene diol, mean molecule quantity 2000; Structure is:
r in formula
5for trimethylolpropane, structure is:
Described titanate coupling agent is Di(dioctylpyrophosphato) ethylene titanate (C
26h
54o
16p
4ti).
Described kaolin composite modified water polyurethane emulsion mixes obtained by 2 ~ 10g hydrophilic modifying kaolin and 80 ~ 97g non-ionic water polyurethane.
Described hydrophilic modifying kaolinic preparation manipulation step is as follows:
(1) 10g is scattered in 30g absolute ethyl alcohol without the kaolin calcined, 0.3g titanate coupling agent,
(2) again through ball mill grinding 1h, rotating speed 1400r/min,
(3) grinding product is in 50 DEG C of baking ovens, dry 24h, obtained hydrophilic modifying kaolin.
The suspensibility of the hydrophilic modifying kaolin obtained by above-mentioned steps in water is 92%.
The concrete operation step preparing a kind of kaolin composite modified aqueous polyurethane solid electrolyte is as follows:
(1) by 2 ~ 10g hydrophilic modifying kaolin and the mixing of 80 ~ 97g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 82 ~ 99g kaolin composite modified water polyurethane emulsion, 1 ~ 10g lithium perchlorate is added, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtained kaolin composite modified aqueous polyurethane solid electrolyte film;
Described kaolin composite modified aqueous polyurethane solid electrolyte film appearance is from transparent to whiting, and hot strength is 8.7 ~ 17.3MPa.
The present invention adopt safety and environmental protection and the aqueous polyurethane of mechanical performance excellence as polymer backbone, and with the composite modified polyurethane of the kaolin with layer structure, provide more ion channel, and then improve the ionic conductivity of aqueous polyurethane.For improving the stability of kaolin in water-based system, the present invention carries out hydrophilic modifying to kaolin, adding in aqueous polyurethane emulsion, non-ionic water polyurethane is prepared by adopting isocyanates, polyethers etc., use the kaolin compound of hydrophilic modifying further, adulterate with lithium perchlorate again, the obtained composite modified aqueous polyurethane solid electrolyte of kaolin; Solid electrolyte of the present invention has the advantages such as good mechanical property, ionic conductivity are high, safety and environmental protection, may be used for the preparation of all-solid lithium-ion battery.
Advantageous Effects of the present invention embodies in the following areas:
1. because the present invention adopts aqueous polyurethane as macromolecule matrix, operating process is carried out in aqueous systems, does not use toxic solvent, solves the problem of safe preparation process environmental protection.
2., because inorganic salts can cause conventional anion aqueous polyurethane and cation aqueous polyurethane emulsion breakdown of emulsion, the present invention adopts non-ionic water polyurethane, solves the problem of inorganic ion salt stability in emulsion.
3. kaolin is carried out hydrophilic modifying by the present invention, is more blendedly coupled in aqueous polyurethane structure, solves the stability problem of inorganic kaolin in aqueous polyurethane.Kaolinicly add the mechanical property and ionic conductivity that improve polyurethane, solve the problem that conventional urethane conductivity is low, under 90 DEG C of conditions, ionic conductivity reaches 2.61 × 10
-3s/cm.
4. the kaolin starting material that the present invention uses is easy to get, and low price, has good using value.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1:
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 90g
Hydrophilic modifying kaolin 2g
Lithium perchlorate 8g
Concrete preparation manipulation step is as follows:
(1) by 2g hydrophilic modifying kaolin and the mixing of 90g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 92g kaolin composite modified water polyurethane emulsion, add 8g lithium perchlorate, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtain kaolin composite modified aqueous polyurethane solid electrolyte film; The kaolin composite modified aqueous polyurethane solid electrolyte film stretching intensity obtained is 8.7MPa, ion-electron conductance is respectively 4.03E-09 20 ~ 90 DEG C (temperature interval is 10 DEG C), 1.91E-08,6.64E-08,2.24E-07,6.33E-07,1.23E-06,2.61E-05,2.61E-03S/cm.
Embodiment 2:
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 86g
Hydrophilic modifying kaolin 4g
Lithium perchlorate 10g
Concrete preparation manipulation step is as follows:
(1) by 4g hydrophilic modifying kaolin and the mixing of 86g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 90g kaolin composite modified water polyurethane emulsion, 10g lithium perchlorate is added, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtained kaolin composite modified aqueous polyurethane solid electrolyte film; The kaolin composite modified aqueous polyurethane solid electrolyte film stretching intensity obtained is 10.2MPa, ion-electron conductance is respectively 1.13E-08 20 ~ 90 DEG C (temperature interval is 10 DEG C), 3.20E-08,1.00E-07,2.59E-07,6.32E-07,1.43E-06,2.89E-05,2.89E-03S/cm.
Embodiment 3:
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 97g
Hydrophilic modifying kaolin 2g
Lithium perchlorate 1g
Concrete preparation manipulation step is as follows:
(1) by 2g hydrophilic modifying kaolin and the mixing of 97g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 99g kaolin composite modified water polyurethane emulsion, add 1g lithium perchlorate, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtain kaolin composite modified aqueous polyurethane solid electrolyte film; The kaolin composite modified aqueous polyurethane solid electrolyte film stretching intensity obtained is 15.6MPa, ion-electron conductance is respectively 1.03E-08 20 ~ 90 DEG C (temperature interval is 10 DEG C), 3.69E-08,1.35E-07,3.74E-07,1.00E-06,2.15E-06,5.82E-05,5.82E-03S/cm.
Embodiment 4:
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 82g
Hydrophilic modifying kaolin 8g
Lithium perchlorate 10g
Concrete preparation manipulation step is as follows:
(1) by 8g hydrophilic modifying kaolin and the mixing of 82g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 90g kaolin composite modified water polyurethane emulsion, 10g lithium perchlorate is added, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtained kaolin composite modified aqueous polyurethane solid electrolyte film; The kaolin composite modified aqueous polyurethane solid electrolyte film stretching intensity obtained is 17.3MPa, ion-electron conductance is respectively 5.77E-09 20 ~ 90 DEG C (temperature interval is 10 DEG C), 1.96E-08,8.06E-08,2.61E-07,8.77E-07,2.10E-06,5.70E-05,5.70E-03S/cm.
Embodiment 5:
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 80g
Hydrophilic modifying kaolin 10g
Lithium perchlorate 10g
Concrete preparation manipulation step is as follows:
(1) by 4g hydrophilic modifying kaolin and the mixing of 86g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 90g kaolin composite modified water polyurethane emulsion, 10g lithium perchlorate is added, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtained kaolin composite modified aqueous polyurethane solid electrolyte film; The kaolin composite modified aqueous polyurethane solid electrolyte film stretching intensity obtained is 16.1MPa, ion-electron conductance is respectively 4.67E-09 20 ~ 90 DEG C (temperature interval is 10 DEG C), 1.73E-08,7.23E-08,1.63E-07,5.25E-07,1.10E-06,2.87E-05,2.87E-03S/cm.
Embodiment 6 (comparative example):
A kind of kaolin composite modified aqueous polyurethane solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 90g
Lithium perchlorate 10g
Concrete preparation manipulation step is as follows:
(1) in 90g kaolin composite modified water polyurethane emulsion, 10g lithium perchlorate is added, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtained kaolin composite modified aqueous polyurethane solid electrolyte film; The kaolin composite modified aqueous polyurethane solid electrolyte film stretching intensity obtained is 7.4MPa, ion-electron conductance is respectively 5.73E-09 20 ~ 90 DEG C (temperature interval is 10 DEG C), 1.63E-08,5.75E-08,1.27E-07,4.02E-07,7.36E-07,1.42E-06,1.42E-05S/cm.
As shown in the table to above-described embodiment solid-state conductivity data at different temperatures:
By such scheme, can obtain preparing the composite modified aqueous polyurethane solid electrolyte membrane of kaolin, film thickness is between 0.2mm-0.5mm, controlled under the conductivity at room temperature different temperatures of film, excellent in mechanical performance, cheap kaolin adds can significantly improve electrolytical conductivity, and this dielectric film can be applicable in lithium ion battery.
Claims (6)
1. the composite modified aqueous polyurethane solid electrolyte of kaolin, is characterized in that described solid electrolyte is made up of following material:
Non-ionic water polyurethane emulsion 80 ~ 97g
Hydrophilic modifying kaolin 2 ~ 10g
Lithium salts 1 ~ 10g;
Described non-ionic water polyurethane emulsion is scattered in water is obtained with reacting ethylenediamine by IPDI, polyoxyethylene glycol, trimethylolpropane-polyethylene glycol monoether, BDO polymerization reaction afterproduct;
Described hydrophilic modifying kaolin is scattered in without the kaolin calcined, titanate coupling agent in absolute ethyl alcohol, then obtain through grinding, oven dry;
Described lithium salts is lithium perchlorate.
2. the composite modified aqueous polyurethane solid electrolyte of a kind of kaolin according to claim 1, is characterized in that:
Described non-ionic water polyurethane emulsion to be scattered in after 6 hours in 200g water 70 DEG C of polymerization reactions by 30.1 IPDIs, 40.3g polyoxyethylene glycol, 15.7g trimethylolpropane-polyethylene glycol monoether, 6.1g1,4-butanediol and within 1 hour, to obtain with 2.0g reacting ethylenediamine; Described non-ionic water polyurethane emulsion is translucent emulsion, pH=7; The basic structure of the non-ionic water polyurethane obtained is:
R in formula
1for IPDI; Structure is:
R in formula
2for trimethylolpropane-polyethylene glycol monoether, mean molecule quantity 1000; Structure is:
R in formula
3for BDO; Structure is :-CH
2cH
2cH
2cH
2-;
R in formula
4for Polyoxypropylene diol, mean molecule quantity 2000; Structure is:
R in formula
5for trimethylolpropane, structure is:
3. the composite modified aqueous polyurethane solid electrolyte of a kind of kaolin according to claim 1, is characterized in that: described titanate coupling agent is Di(dioctylpyrophosphato) ethylene titanate (C
26h
54o
16p
4ti).
4. the composite modified aqueous polyurethane solid electrolyte of a kind of kaolin according to claim 1, is characterized in that: described kaolin composite modified water polyurethane emulsion mixes obtained by 2 ~ 10g hydrophilic modifying kaolin and 80 ~ 97g non-ionic water polyurethane.
5. the composite modified aqueous polyurethane solid electrolyte of a kind of kaolin according to claim 1, is characterized in that: described hydrophilic modifying kaolinic preparation manipulation step is as follows:
(1) 10g is scattered in 30g absolute ethyl alcohol without the kaolin calcined, 0.3g titanate coupling agent,
(2) again through ball mill grinding 1h, rotating speed 1400r/min,
(3) grinding product is in 50 DEG C of baking ovens, dry 24h, obtained hydrophilic modifying kaolin.
The suspensibility of the hydrophilic modifying kaolin obtained by above-mentioned steps in water is 92%.
6. the preparation method of the composite modified aqueous polyurethane solid electrolyte of a kind of kaolin according to claim 1, is characterized in that concrete operation step is as follows:
(1) by 2 ~ 10g hydrophilic modifying kaolin and the mixing of 80 ~ 97g non-ionic water polyurethane, obtained kaolin composite modified water polyurethane emulsion;
(2) in 82 ~ 99g kaolin composite modified water polyurethane emulsion, 1 ~ 10g lithium perchlorate is added, obtain the kaolin composite modified water polyurethane emulsion of lithium doping, emulsion film forming is dried, both obtained kaolin composite modified aqueous polyurethane solid electrolyte film;
Described kaolin composite modified aqueous polyurethane solid electrolyte film appearance is from transparent to whiting, and hot strength is 8.7 ~ 17.3MPa.
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| CN201510606971.5A CN105304939B (en) | 2015-09-22 | 2015-09-22 | A kind of composite modified aqueous polyurethane solid electrolyte of kaolin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102016005326A1 (en) | 2016-04-23 | 2016-09-29 | Daimler Ag | Solid electrolyte and process for producing a solid electrolyte |
| CN109585916A (en) * | 2018-11-13 | 2019-04-05 | 吉林师范大学 | A kind of flame-retardant polymer solid electrolyte material and its dielectric film and application |
| CN110112458A (en) * | 2019-05-16 | 2019-08-09 | 广东工业大学 | A kind of halloysite nanotubes modified polyurethane solid electrolyte, preparation method and its battery |
| CN112117488A (en) * | 2020-07-31 | 2020-12-22 | 华中科技大学 | Solid electrolyte, lithium metal negative electrode and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280104A (en) * | 2008-05-07 | 2008-10-08 | 北京理工大学 | Polymer electrolyte |
| WO2015081486A1 (en) * | 2013-12-03 | 2015-06-11 | Rohm And Haas Company | Aqueous polyurethane dispersion |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280104A (en) * | 2008-05-07 | 2008-10-08 | 北京理工大学 | Polymer electrolyte |
| WO2015081486A1 (en) * | 2013-12-03 | 2015-06-11 | Rohm And Haas Company | Aqueous polyurethane dispersion |
Non-Patent Citations (2)
| Title |
|---|
| CHUNLIU ZHU等: "Waterborne Polyurethane Used as Binders for Lithium-Ion Battery with Improved Electrochemical Properties", 《ADVANCED MATERIALS RESEARCH》 * |
| 石阳阳等: "改性高岭土/水性聚氨酯复合材料的制备与表征", 《化学推进剂与高分子材料》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102016005326A1 (en) | 2016-04-23 | 2016-09-29 | Daimler Ag | Solid electrolyte and process for producing a solid electrolyte |
| CN109585916A (en) * | 2018-11-13 | 2019-04-05 | 吉林师范大学 | A kind of flame-retardant polymer solid electrolyte material and its dielectric film and application |
| CN110112458A (en) * | 2019-05-16 | 2019-08-09 | 广东工业大学 | A kind of halloysite nanotubes modified polyurethane solid electrolyte, preparation method and its battery |
| CN112117488A (en) * | 2020-07-31 | 2020-12-22 | 华中科技大学 | Solid electrolyte, lithium metal negative electrode and preparation method thereof |
| CN112117488B (en) * | 2020-07-31 | 2021-11-02 | 华中科技大学 | Solid electrolyte, lithium metal negative electrode and preparation method thereof |
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| CN105304939B (en) | 2017-06-06 |
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