CN101075674A - Method for producing PEO/lithum salt/montmorillonite composite electrolyte with water as dispersant - Google Patents
Method for producing PEO/lithum salt/montmorillonite composite electrolyte with water as dispersant Download PDFInfo
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- CN101075674A CN101075674A CNA2007100722690A CN200710072269A CN101075674A CN 101075674 A CN101075674 A CN 101075674A CN A2007100722690 A CNA2007100722690 A CN A2007100722690A CN 200710072269 A CN200710072269 A CN 200710072269A CN 101075674 A CN101075674 A CN 101075674A
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- Prior art keywords
- lithium salts
- peo
- water
- imvite
- montmorillonite composite
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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
Abstract
The process method for a combined electrolyte of PEO/lithium salt/monthmorillonite with water as dispersant is as: solving lithium salt in ultrapure water and mixing in evenly with poly(ethylene oxide); evenly mixing in treated monthmorillonite into ultrapure water; mixing the first and the second solution evenly under airproof condition and instillation till water content reduced to 1/3 - 1/2; then molding, dry, mold remove.
Description
Background technology
The present invention relates to a kind of electrolyte preparation method; Being specifically related to a kind of water is the method that dispersant prepares composite electrolyte.
Technical field
PEO/ lithium salts/nano material (nanometer Al of present broad research
2O
3, nano-TiO
2, nanometer ZrO
2, nanometer SiO
2Deng) there is following shortcoming in composite electrolyte:
1. conductivity low (20 ℃, 5 * 10
-5Scm
-1Below) can not satisfy the preparation battery requirement (20 ℃, 1 * 10
-4Scm
-1).
2. organic solvent (acetonitrile, acetone etc.) is done dispersant, its cost height, and gas volatile, that produce produces environment and pollutes, human body is produced endanger.
Summary of the invention
The objective of the invention is to have in order to solve present PEO/ lithium salts/nano material composite electrolyte that conductivity is low can not to satisfy the requirement of preparation battery and the cost height that organic solvent is done dispersant, gas volatile, that produce produce the shortcoming of polluting and human body being produced harm to environment; And a kind of water is provided is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite.Water of the present invention is cooked dispersant, does additive with the layer structure imvite that intercalation processing is crossed, preparation PEO/ lithium salts/montmorillonite Composite electrolyte.Method step of the present invention is as follows: one, lithium salts is dissolved in the ultra-pure water (redistilled water), wherein the mass ratio of lithium salts and ultra-pure water is 1: 500～1000, then at 50～60 ℃, under the speed stirring condition with 60～600r/min, in aforesaid liquid, add poly-oxireme (being called for short PEO), heating 0.8～1.2h, the mol ratio of the EO base of lithium salts and poly-oxireme (finger ring oxidative ethane) is 1: 5～10, continues to stir 5～8h again; Two, the imvite that intercalation processing is crossed mixes with ultra-pure water, and ultrasonic oscillation or mechanical agitation are to even, and wherein the mass ratio of imvite and water is 1: 100～400, and the mass ratio of the lithium salts in imvite and the step 1 is 1: 5～10; Three, under the condition of sealing, the mixed liquor of step 1 and step 2 is stirred 0.5～3 day to even, under 45～65 ℃ of conditions, evaporate then, volume to ultra-pure water reduces 1/3～1/2, is poured in the mould dry 0.5～3 day aftershaping under 70～120 ℃ of conditions, the demoulding gets product.
Intercalation processing of the present invention is that water soaks, stirs imvite, and it is wetting that water is carried out the interlayer structure of imvite, enlarges its interlamellar spacing.The PEO strand inserts the interlayer structure through the intercalation processing imvite, and edge (stretching, extension is bordering on linear) the PEO strand that is beneficial to lithium ion is wriggled and moved, and increases its conductivity.]
Use water as dispersant, the chemical property that additive has improved PEO based polyalcohol composite electrolyte is significantly done in the imvite that the adding intercalation processing is crossed.
PEO/ lithium salts/montmorillonite Composite the electrolyte of the present invention's preparation can reach 1 * 10 20 ℃ of following conductivity
-4Scm
-1Use ultra-pure water to make dispersant, avoid foreign ion and imvite interlayer ion in the water to exchange.Compare with organic solvent, cost also has bigger reduction.
Method of the present invention is simple, cost is low, the harm that the volatilization of having avoided organic solvent in the preparation process simultaneously produces the operator and to the pollution of environment.
Embodiment
Embodiment one: the method step of preparation composite electrolyte is as follows in the present embodiment: one, lithium salts is dissolved in the ultra-pure water (being redistilled water), wherein the mass ratio of lithium salts and ultra-pure water is 1: 500～1000, then at 50～60 ℃, under the speed stirring condition with 60～600r/min, in aforesaid liquid, add poly-oxireme (being called for short PEO), heating 0.8～1.2h, the mol ratio of the EO base of lithium salts and poly-oxireme (finger ring oxidative ethane) is 1: 5～10, continues to stir 5～8h again; Two, the imvite that intercalation processing is crossed mixes with ultra-pure water, and ultrasonic oscillation or mechanical agitation are to even, and wherein the mass ratio of imvite and water is 1: 100～400, and the mass ratio of the lithium salts in imvite and the step 1 is 1: 5～10; Three, under the condition of sealing, the mixed liquor of step 1 and step 2 is stirred 0.5～3 day to even, under 45～65 ℃ of conditions, evaporate then, volume to ultra-pure water reduces 1/3～1/2, is poured in the mould dry 0.5～3 day aftershaping under 70～120 ℃ of conditions, the demoulding gets product.
PEO/ lithium salts/montmorillonite Composite the electrolyte of present embodiment preparation can reach 1 * 10 20 ℃ of following conductivity
-4Scm
-1
Embodiment two: present embodiment lithium salts in step 1 is LiClO
4, LiTFSI, LiCF
3SO
3In one or more mixing.Other step is identical with embodiment one.
When lithium salts is mixture in the present embodiment, press arbitrarily than mixing.
Embodiment three: present embodiment lithium salts in step 1 is LiClO
4, LiTFSI or LiCF
3SO
3Other step is identical with embodiment one.
Embodiment four: the lithium salts of present embodiment in step 1 is LiClO
4And LiTFSI.Other step is identical with embodiment one.
Lithium salts LiClO in the present embodiment
4Press arbitrarily than mixing with LiTFSI.
Embodiment five: present embodiment lithium salts in step 1 is LiCF
3SO
3Other step is identical with embodiment one.
Concrete true mode six: present embodiment mass ratio of lithium salts and ultra-pure water in step 1 is 1: 700～800.Other step is identical with embodiment one.
Embodiment seven: present embodiment mass ratio of lithium salts and ultra-pure water in step 1 is 1: 750.Other step is identical with embodiment one.
Embodiment eight: the mol ratio of present embodiment EO base (finger ring oxidative ethane) of lithium salts and poly-oxireme in step 1 is 1: 7～8.Other step is identical with embodiment one.
Embodiment nine: present embodiment mol ratio of lithium salts and the EO base (finger ring oxidative ethane) of poly-oxireme in step 1 is that 1: 7.5 other step is identical with embodiment one.
Embodiment ten: present embodiment mass ratio of imvite and water in step 2 is 1: 150～300.Other step is identical with embodiment one.
Embodiment 11: present embodiment mass ratio of imvite and water in step 2 is 1: 200.Other step is identical with embodiment one.
Embodiment 12: the mass ratio of present embodiment lithium salts in imvite and the step 1 in step 2 is 1: 6～9.Other step is identical with embodiment one.
Embodiment 13: the mass ratio of present embodiment lithium salts in imvite and the step 1 in step 2 is 1: 7.Other step is identical with embodiment one.
Embodiment 14: present embodiment adopts supersonic oscillations with diffusing imvite of oversubscription and ultra-pure water mixing in step 2, and the reaction time is 10～20min.Other step is identical with embodiment one.
Embodiment 15: present embodiment adopts mechanical agitation with diffusing imvite of oversubscription and ultra-pure water mixing in step 2, and the reaction time is 6～9h.Other step is identical with embodiment one.
Embodiment 16: the material of mould is a polytetrafluoroethylene in the present embodiment.Other step is identical with embodiment one.
Embodiment 17: the method step of preparation composite electrolyte is as follows in the present embodiment: one, weighing 0.56g three water lithium perchlorates, be dissolved in the 40ml ultra-pure water (being redistilled water), under 50～60 temperature, speed stirring condition with 60～600r/min, add the poly-oxireme of 1.23g, heating 1h continues to stir 5～8h then; Two, the imvite of crossing of weighing 0.080g intercalation processing mixes ultrasonic oscillation 10～20min with the 20ml ultra-pure water; Three, 0.5～3d is stirred in the mixed liquor sealing of step 1 and step 2, under 45～65 ℃ of conditions, evaporate then, to the volume minimizing 1/3～1/2 of ultra-pure water, be poured in the polytetrafluoroethylene mould, dry 0.5～3d under 70～120 ℃ of conditions then, the demoulding, product.
Claims (10)
1, a kind of water is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, the step that it is characterized in that this method is as follows: one, lithium salts is dissolved in the ultra-pure water, wherein the mass ratio of lithium salts and ultra-pure water is 1: 200～1000, then at 50～60 ℃, under the speed stirring condition with 60～600r/min, in aforesaid liquid, add poly-oxireme (being called for short PEO), heating 0.8～1.2h, the mol ratio of the EO base of lithium salts and poly-oxireme is 1: 5～10, continues to stir 5～8h again; Two, the imvite that intercalation processing is crossed mixes with ultra-pure water, and ultrasonic oscillation or mechanical agitation are to even, and wherein the mass ratio of imvite and water is 1: 100～400, and the mass ratio of the lithium salts in imvite and the step 1 is 1: 2～10; Three, under the condition of sealing, the mixed liquor of step 1 and step 2 is stirred 0.5～3 day to even, under 45～65 ℃ of conditions, evaporate then, volume to ultra-pure water reduces 1/3～1/2, is poured in the mould dry 0.5～3 day aftershaping under 70～120 ℃ of conditions, the demoulding gets product.
2, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that lithium salts is LiClO in step 1
4, LiTFSI, LiCF
3SO
3In one or more mixing.
3, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that lithium salts is LiCF in step 1
3SO
3
4, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that the mass ratio of lithium salts and ultra-pure water is 1: 700～800 in step 1.
5, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that the mol ratio of the EO base of lithium salts and poly-oxireme in step 1 is 1: 7～8.
6, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that the mass ratio of imvite and water is 1: 150～300 in step 2.
7, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that the mass ratio of the lithium salts in the imvite and step 1 in step 2 is 1: 6～9.
8, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that adopting in step 2 supersonic oscillations with diffusing imvite of oversubscription and ultra-pure water mixing, and the reaction time is 10～20min.
9, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, it is characterized in that adopting in step 2 mechanical agitation with diffusing imvite of oversubscription and ultra-pure water mixing, and the reaction time is 6～9h.
10, water according to claim 1 is that dispersant prepares the electrolytical method of PEO/ lithium salts/montmorillonite Composite, and the material that it is characterized in that mould is a polytetrafluoroethylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710072269A CN101075674B (en) | 2007-05-28 | 2007-05-28 | Method for producing PEO/lithum salt/montmorillonite composite electrolyte with water as dispersant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710072269A CN101075674B (en) | 2007-05-28 | 2007-05-28 | Method for producing PEO/lithum salt/montmorillonite composite electrolyte with water as dispersant |
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|---|---|
| CN101075674A true CN101075674A (en) | 2007-11-21 |
| CN101075674B CN101075674B (en) | 2010-05-26 |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101924246A (en) * | 2010-09-07 | 2010-12-22 | 上海交通大学 | Preparation method of composite solid electrolyte based on polyphosphazene carbide micro-nanometer material |
| CN109054092A (en) * | 2018-06-20 | 2018-12-21 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of the enhancing by polymer modified organic montmorillonite of graphene |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1452794A (en) * | 2000-05-24 | 2003-10-29 | 株式会社华仁电池 | Microporous solid electrolytes and methods for preparing them |
-
2007
- 2007-05-28 CN CN200710072269A patent/CN101075674B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101924246A (en) * | 2010-09-07 | 2010-12-22 | 上海交通大学 | Preparation method of composite solid electrolyte based on polyphosphazene carbide micro-nanometer material |
| CN109054092A (en) * | 2018-06-20 | 2018-12-21 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of the enhancing by polymer modified organic montmorillonite of graphene |
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| Publication number | Publication date |
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| CN101075674B (en) | 2010-05-26 |
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Granted publication date: 20100526 Termination date: 20110528 |