CN105355973A - Preparation method of gel electrolyte solution for sodium ion battery - Google Patents
Preparation method of gel electrolyte solution for sodium ion battery Download PDFInfo
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- CN105355973A CN105355973A CN201510658758.9A CN201510658758A CN105355973A CN 105355973 A CN105355973 A CN 105355973A CN 201510658758 A CN201510658758 A CN 201510658758A CN 105355973 A CN105355973 A CN 105355973A
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- preparation
- sodium
- electrolyte
- ion battery
- electrolyte solution
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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
- H01M10/058—Construction or manufacture
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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
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a preparation method of a gel electrolyte solution for sodium ion batteries. , and belongs to the technical field of lithium ion batteries. The preparation method of the gel electrolyte solution for the sodium ion batteries comprises the following steps: (1) preparation of a basic electrolyte solution: using an electrolyte lithium salt and a compound organic solvent to prepare the electrolyte solution for 1-20 h at the temperature of 0-90 DEG C; (2) cross-linking polymerization: preparing a mixed liquor of a polymeric monomer, a cross-linking agent and a solvent, and adding the mixed liquor to the electrolyte solution, wherein the polymeric monomer is methyl methacrylate, acrylonitrile, ethylene oxide or tetrafluoroethylene, and the cross-linking agent is hexyl acrylate; and (3) initiation before using: preparing an initiator solution and mixing uniformly before battery loading, then carrying out initiated polymerization at the temperature of 15-65 DEG C for 2-6 h to obtain the gel electrolyte solution for the polymeric sodium ion batteries. The preparation method has the advantages that the preparation method is simple in technology, convenient in operation, economical and practical, the performance of the batteries prepared by using the electrolyte solution is improved while the preparation cost is reduced, and the like.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of preparation method of sodium-ion battery gel electrolyte.
Background technology
At present, along with the development of accumulation power supply and electric vehicle power sources, sodium-ion battery, because of features such as its raw material rich reserves, low price, environmental friendliness, is considered to the ideal chose of energy storage of future generation and electrokinetic cell.
What sodium-ion battery major part adopted is liquid electrolyte, and Liquid Sodium ion battery has some shortcomings part:
(1) the liquid state organic electrolyte matter used in Liquid Sodium ion battery easily decomposes generation gas in discharge process, forms excessive vapour pressure, and there is the possibility of leakage.
(2) because the internal hematocrit of Liquid Sodium ion battery tires out insensitive, very easily to burn under abuse conditions, the danger such as blast.
Therefore on the basis of Liquid Sodium ion battery, develop sodium-ion battery of new generation: polymer sodium-ion battery, because it adopts structure of whole solid state, overcome the problems such as the insecurity that leakage that Liquid Sodium ion battery may occur causes.In addition, because battery adopts flexible material to encapsulate, allow bending, folding, configuration design can more flexibly, conveniently.
Summary of the invention
The present invention provides a kind of preparation method of sodium-ion battery gel electrolyte for solving in known technology the technical problem that exists.
The object of this invention is to provide one, to have technique simple, easy to operate, economical and practical, while the preparation cost reducing electrolyte and this electrolyte battery, improve the preparation method of the sodium-ion battery gel electrolyte of the features such as the battery performance using this electrolyte to prepare.
Preparation method of electrolyte involved in the present invention comprises basic electrolyte preparation, the three large steps such as electrolyte cross-linked polymeric and the front initiation of use:
1. basic electrolyte preparation
By electrolyte lithium salt, compounded organic solvent joins in reactor, and control temperature is at 0-90 DEG C, and be preferably 45 DEG C, the time is 1-20 hour, is preferably 10 hours,
Described electrolyte lithium salt is one or both combinations of sodium hexafluoro phosphate, sodium perchlorate, preferably sodium hexafluoro phosphate and sodium perchlorate press 20-32:1 (mol ratio) mixing, electrolyte total concentration is 1.15-1.2mol/L (in sodium), and preferred concentration is 1.17mol/L;
Described organic solvent system is carbonate based organic solvent, these carbonic esters comprise ethylene carbonate (EC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), organic solvent ratio is EC:DEC:EMC=1-9:1-10:2-20 (volume ratio), is preferably 5:5:16
2. cross-linked polymeric
After treating to dissolve completely, preparation polymerization single polymerization monomer, crosslinking agent and solvent liquid, join in electrolyte;
Described polymerization single polymerization monomer, for methyl methacrylate (MMA), one among acrylonitrile (AN), oxirane (EO), four kinds, tetrafluoroethene (VDF), be preferably VDF, addition, between 10-20% (weight ratio), is preferably 15%; Selected crosslinking agent be n-hexyl acrylate addition between 22-34% (weight ratio), be preferably 27%;
3. cause before using
Preparation initiator solution is even at packed battery forward slip value, and then initiated polymerization at 15-45 DEG C, polymerization time is 2-6 hour, obtains final polymer sodium-ion battery gel electrolyte.
Selected initator is one or more in azodiisobutyronitrile, dibenzoyl peroxide, peroxy dicarbonate isopropyl ester, be preferably dibenzoyl peroxide, addition is the 1.2%-2.2% of polymerization single polymerization monomer and crosslinking agent gross mass, is preferably 1.5%.
The technical scheme that the preparation method of sodium-ion battery gel electrolyte of the present invention takes is:
A preparation method for sodium-ion battery gel electrolyte, is characterized in: the preparation process of sodium-ion battery gel electrolyte comprises the following steps:
(1) basic electrolyte preparation
By electrolyte lithium salt, compounded organic solvent, at temperature 0-90 DEG C, under time 1-20 hour condition, prepare electrolyte; Electrolyte lithium salt is one or both combinations of sodium hexafluoro phosphate, sodium perchlorate, and electrolyte total concentration counts 1.15-1.2mol/L with sodium; Compounded organic solvent is carbonate based organic solvent, comprises ethylene carbonate, diethyl carbonate, methyl ethyl carbonate, and volume ratio is ethylene carbonate, diethyl carbonate, methyl ethyl carbonate=1-9:1-10:2-20;
(2) cross-linked polymeric
Preparation polymerization single polymerization monomer, crosslinking agent and solvent liquid, join in electrolyte;
Polymerization single polymerization monomer is methyl methacrylate, acrylonitrile, oxirane or tetrafluoroethene, and the weight ratio of addition is 10-20%; Crosslinking agent is n-hexyl acrylate, and the weight ratio of addition is 22-34%; Solvent is diethyl carbonate;
(3) cause before using
Preparation initiator solution is even at packed battery forward slip value, then initiated polymerization at 15-65 DEG C, and polymerization time is 2-6 hour, obtains polymer sodium-ion battery gel electrolyte;
Initator is one or more in azodiisobutyronitrile, dibenzoyl peroxide, peroxy dicarbonate isopropyl ester, and addition is the 1.2%-2.2% of polymerization single polymerization monomer and crosslinking agent gross mass.
The preparation method of sodium-ion battery gel electrolyte of the present invention can also adopt following technical scheme:
The preparation method of described sodium-ion battery gel electrolyte, is characterized in: electrolyte lithium salt is sodium hexafluoro phosphate by 20-32:1 mixed in molar ratio and sodium perchlorate.
The preparation method of described sodium-ion battery gel electrolyte, is characterized in: the solvent of initiator solution is diethyl carbonate, and solution quality percent concentration is 30-35%.
The advantage that the present invention has and good effect are:
The preparation method of sodium-ion battery gel electrolyte is owing to have employed the brand-new technical scheme of the present invention, compared with prior art, it is simple that the present invention has technique, easy to operate, economical and practical, while the preparation cost reducing electrolyte and this electrolyte battery, improve the advantages such as the battery performance using this electrolyte to prepare.
Accompanying drawing explanation
Fig. 1 is the cycle performance curve that various electrolyte circulates at normal temperatures.
Embodiment
For summary of the invention of the present invention, Characteristic can be understood further, hereby exemplify following examples, and coordinate accompanying drawing to be described in detail as follows:
Accompanying drawings 1.
Embodiment 1
A preparation method for sodium-ion battery gel electrolyte, comprises basic electrolyte preparation, the three large steps such as electrolyte cross-linked polymeric and the front initiation of use:
By electrolyte sodium salt (the 20:1 mixing in molar ratio of sodium hexafluoro phosphate and sodium perchlorate), compounded organic solvent EC:DEC:EMC=1:1:2 (volume ratio), join in reactor, control temperature is at 25 DEG C, time is 5 hours, after treating to dissolve completely, preparation polymerization single polymerization monomer (MMA, 15%), crosslinking agent (n-hexyl acrylate, 27%) and solvent liquid, join in electrolyte, preparation initator (azodiisobutyronitrile, addition is 1.5% of polymerization single polymerization monomer and crosslinking agent gross mass, solution is even at packed battery forward slip value, then initiated polymerization at 45-65 DEG C, obtain final polymer sodium-ion battery gel electrolyte.
Embodiment 2
A preparation method for sodium-ion battery gel electrolyte, comprises basic electrolyte preparation, the three large steps such as electrolyte cross-linked polymeric and the front initiation of use:
By electrolyte sodium salt (the 32:1 mixing in molar ratio of sodium hexafluoro phosphate and sodium perchlorate), compounded organic solvent EC:DEC:EMC=9:10:20 (volume ratio), join in reactor, control temperature is at 55 DEG C, time is 4 hours, after treating to dissolve completely, preparation polymerization single polymerization monomer (VDF, 20%), crosslinking agent (n-hexyl acrylate, 34%) and solvent liquid, join in electrolyte, preparation initator (dibenzoyl peroxide, addition is 2% of polymerization single polymerization monomer and crosslinking agent gross mass, solution is even at packed battery forward slip value, then initiated polymerization at 45-65 DEG C, obtain final polymer sodium-ion battery gel electrolyte.
Embodiment 3
A preparation method for sodium-ion battery gel electrolyte, comprises basic electrolyte preparation, the three large steps such as electrolyte cross-linked polymeric and the front initiation of use:
By electrolyte sodium salt (the 28:1 mixing in molar ratio of sodium hexafluoro phosphate and sodium perchlorate), compounded organic solvent EC:DEC:EMC=2:2:19 (volume ratio), join in reactor, control temperature is at 65 DEG C, time is 3 hours, after treating to dissolve completely, preparation polymerization single polymerization monomer (EO, 15%), crosslinking agent (n-hexyl acrylate, 29%) and solvent liquid, join in electrolyte, preparation initator (dibenzoyl peroxide, addition is 1.8% of polymerization single polymerization monomer and crosslinking agent gross mass, solution is even at packed battery forward slip value, then initiated polymerization at 45-65 DEG C, obtain final polymer sodium-ion battery gel electrolyte.
Comparative example 1
Electrolyte sodium salt is sodium hexafluoro phosphate, concentration is 1.1mol/L, organic solvent compound proportion is EC:DEC:EMC=3:6:1 (weight ratio), and additive is VC and PS addition is 1% and 2% (weight ratio), is mixed with liquid electrolyte.
Comparative example 2
Electrolyte sodium salt is sodium hexafluoro phosphate, and concentration is 1.1mol/L, and organic solvent compound proportion is EC:FEC:EMC=25:10:65 (W), and additive is PS and VEC, and addition is 2% and 1% (weight ratio).
The preparation method of the present embodiment sodium-ion battery gel electrolyte has technique simply, easy to operate, economical and practical, while the preparation cost reducing electrolyte and this electrolyte battery, improves the good effects such as the battery performance using this electrolyte to prepare.
Claims (3)
1. a preparation method for sodium-ion battery gel electrolyte, is characterized in that: the preparation process of sodium-ion battery gel electrolyte comprises the following steps:
(1) basic electrolyte preparation
By electrolyte lithium salt, compounded organic solvent, at temperature 0-90 DEG C, under time 1-20 hour condition, prepare electrolyte; Electrolyte lithium salt is one or both combinations of sodium hexafluoro phosphate, sodium perchlorate, and electrolyte total concentration counts 1.15-1.2mol/L with sodium; Compounded organic solvent is carbonate based organic solvent, comprises ethylene carbonate, diethyl carbonate, methyl ethyl carbonate, and volume ratio is ethylene carbonate, diethyl carbonate, methyl ethyl carbonate=1-9:1-10:2-20;
(2) cross-linked polymeric
Preparation polymerization single polymerization monomer, crosslinking agent and solvent liquid, join in electrolyte;
Polymerization single polymerization monomer is methyl methacrylate, acrylonitrile, oxirane or tetrafluoroethene, and the weight ratio of addition is 10-20%; Crosslinking agent is n-hexyl acrylate, and the weight ratio of addition is 22-34%; Solvent is diethyl carbonate;
(3) cause before using
Preparation initiator solution is even at packed battery forward slip value, then initiated polymerization at 15-65 DEG C, and polymerization time is 2-6 hour, obtains polymer sodium-ion battery gel electrolyte;
Initator is one or more in azodiisobutyronitrile, dibenzoyl peroxide, peroxy dicarbonate isopropyl ester, and addition is the 1.2%-2.2% of polymerization single polymerization monomer and crosslinking agent gross mass.
2. the preparation method of sodium-ion battery gel electrolyte according to claim 1, is characterized in that: electrolyte lithium salt is sodium hexafluoro phosphate by 20-32:1 mixed in molar ratio and sodium perchlorate.
3. the preparation method of sodium-ion battery gel electrolyte according to claim 1, is characterized in that: the solvent of initiator solution is diethyl carbonate, and solution quality percent concentration is 30-35%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510658758.9A CN105355973A (en) | 2015-10-13 | 2015-10-13 | Preparation method of gel electrolyte solution for sodium ion battery |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510658758.9A CN105355973A (en) | 2015-10-13 | 2015-10-13 | Preparation method of gel electrolyte solution for sodium ion battery |
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| CN105355973A true CN105355973A (en) | 2016-02-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116826162A (en) * | 2023-08-28 | 2023-09-29 | 河南新太行电源股份有限公司 | Solid sodium ion battery and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5603982A (en) * | 1995-09-19 | 1997-02-18 | Battery Engineering, Inc. | Thin film solid electrolyte production method |
| CN1317512A (en) * | 2001-05-25 | 2001-10-17 | 复旦大学 | Process for preparing gel-state lithium ion polymer as electrolyte and bettery |
| CN1554698A (en) * | 2003-12-24 | 2004-12-15 | 中国科学院广州化学研究所 | Colloidal polymer electrolyte for lithium ion cell and its preparing method |
| CN102522589A (en) * | 2011-12-16 | 2012-06-27 | 浙江大东南集团有限公司 | Novel gel polymer electrolyte with interpenetrating network structure and preparation method and application thereof |
| CN103772607A (en) * | 2014-01-26 | 2014-05-07 | 郑州大学 | Phosphorus-containing crosslinked gel polymer electrolyte and on-site thermal-polymerization preparation method and application thereof |
-
2015
- 2015-10-13 CN CN201510658758.9A patent/CN105355973A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5603982A (en) * | 1995-09-19 | 1997-02-18 | Battery Engineering, Inc. | Thin film solid electrolyte production method |
| CN1317512A (en) * | 2001-05-25 | 2001-10-17 | 复旦大学 | Process for preparing gel-state lithium ion polymer as electrolyte and bettery |
| CN1554698A (en) * | 2003-12-24 | 2004-12-15 | 中国科学院广州化学研究所 | Colloidal polymer electrolyte for lithium ion cell and its preparing method |
| CN102522589A (en) * | 2011-12-16 | 2012-06-27 | 浙江大东南集团有限公司 | Novel gel polymer electrolyte with interpenetrating network structure and preparation method and application thereof |
| CN103772607A (en) * | 2014-01-26 | 2014-05-07 | 郑州大学 | Phosphorus-containing crosslinked gel polymer electrolyte and on-site thermal-polymerization preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116826162A (en) * | 2023-08-28 | 2023-09-29 | 河南新太行电源股份有限公司 | Solid sodium ion battery and preparation method thereof |
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