CN100536048C - Electrolyte of electrochemical capacitor in double electrode layer - Google Patents
Electrolyte of electrochemical capacitor in double electrode layer Download PDFInfo
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- CN100536048C CN100536048C CNB2006100470835A CN200610047083A CN100536048C CN 100536048 C CN100536048 C CN 100536048C CN B2006100470835 A CNB2006100470835 A CN B2006100470835A CN 200610047083 A CN200610047083 A CN 200610047083A CN 100536048 C CN100536048 C CN 100536048C
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- electrode layer
- electrochemical capacitor
- double electrode
- tetrafluoroborate
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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
- Y02E60/13—Energy storage using capacitors
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention is related to electrolyte of electrochemical double electric layer capacitor. Solute is as N including N-alkyl dihalide-1, salt of tetrafluorideborate or salt of phosphofluoric acid, or perchlorate or sulfosalt trifluoromethyl of 4-bicyclo-cis-octane and tetraethyl ammonium tetrafluorideborate. Solvent is aprotonic solvent. At room temperature, density is 0.5mol/l-2.0mol/l; more suitable density is 0.7-1.5mol/l; most suitable density is 0.8-1.2mol/l; and density of tetraethyl ammonium tetrafluorideborate is 0-0.7mol/l. the disclosed electrolyte decides higher capacity and higher voltage characteristic in model of capacitor. The invention is applicable to backup units of memory in PC, source of pulse power for electric motor car or spot welding device, or as load of providing pulse power for battery in hybrid power source.
Description
Technical field
The present invention relates to technology of fine chemicals, be specifically related to a kind of electrolyte of electrochemical capacitor in double electrode layer.
Background technology
The organic electrolyte of protonic solvent and the perchlorate of tetra-allkylammonium, tetrafluoroborate or hexafluorophosphate are widely used among the EDLC.The peculiar advantage that they are compared with aqueous electrolyte is than higher electrochemical stability therefore have than higher operating voltage.Energy stored and voltage is square proportional in the capacitor:
E＝0.5CV
2
Selecting another advantage of protonic solvent is that very wide temperature range is arranged, because normally used organic solvent is liquid in-60 ℃ to+240 ℃ temperature range in EDLC.Yet the dissolubility of tetraalkylammonium salt above-mentioned reduces very soon with temperature in such temperature, and therefore, in practice, the low temperature limit of this electrolyte is normally-20 ℃ to-25 ℃.
In addition, most of salt has single cationic charge, and for example, different ammonium salts, microcosmic salt, pyridiniujm and other salt all are used in the electrochemical capacitor in double electrode layer electrolyte.The cationic salts of double charge and tricharged has been proposed simultaneously.Below shown in aromatic heterocycle have: pyridazine (I), pyrimidine (II), pyrazine (III) and hexa-atomic triazine alkyl growths such as (IV).Yet experiment shows, to such an extent as to these cationic electrochemical stabilities inadequately the organic solution of strong these salt can not use being higher than under the voltage of 2.5-2.8V.On the other hand, in using, use electrochemical capacitor in double electrode layer the cationic idea of double charge as if very attractive, because the increase of ionic charge density will cause the increase of charge inducing density opposite on electrode, and the result, the electric double layer capacity also will increase.
Summary of the invention
At the weak point of the electrolyte of present electrochemical capacitor in double electrode layer (EDLC), the invention provides a kind of electrolyte of electrochemical capacitor in double electrode layer, reach the capacity that improves electrochemical capacitor in double electrode layer and the purpose of voltage performance.
Electrolyte of the present invention is that the tetrafluoroborate of the DRXDACO shown in the general formula (1) or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid are dissolved in a kind of aprotic solvent, or the solution that forms in the mixed solvent of more than one aprotic solvents.Here DRXDACO is meant N, N-two alkylhalide groups-1, and 4-is to the suitable octane of two rings.
X is halogen F, Cl, Br or I; R is C
1～C
4Alkyl, i.e. methyl, ethyl, n-propyl group or n-butyl.Y is BF
4 -Perhaps PF
6 -Or ClO
- 4Perhaps CF
3SO
- 3Anion.
DRXDACO cation of the present invention combines the chemistry and the electrochemical stability of bicyclic system, and some data that DRXDACO electrolyte is obtained are as shown in Fig. 1-3 and table 1,2.Because the DEFDACO of 2-fluoro ethyl growth
2+(BF
4 -)
2Promptly
Demonstrating good dissolubility, electrical conductance and stability.
Aprotic solvent is acetonitrile, propionitrile, 3-methoxypropionitrile, gamma-butyrolacton, gamma-valerolactone, ethylene carbonate, propene carbonate, N, dinethylformamide, 1-Methyl-2-Pyrrolidone, dimethoxy-ethane, methylethylketone and oxolane, sulfolane, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dioxolanes, 1, the mixture of one or more in 4-butane sultone, 1, the 3 propane sultone.
The tetrafluoroborate of DRXDACO or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid are dissolved in aprotic solvent promptly form electrolyte, electrolyte comprises compound in the formula (1) usually as solute.
Electrolyte of the present invention comprises the single compound shown in a kind of following formula (1), yet, the compound that electrolyte preferably of the present invention comprises a kind of formula (1) mixes with tetraethylammonium tetrafluoroborate (TEA), and tetraethylammonium tetrafluoroborate (TEABF4) is the compound that generally uses in the electrochemical capacitor in double electrode layer.When a kind of compound that uses formula (1) mixes with TEA tetrafluoro boric acid salt face, the tetrafluoroborate of DRXDACO or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid and tetraethylammonium tetrafluoroborate are dissolved in aprotic solvent respectively promptly form electrolyte.
To sum up, electrolyte solute of the present invention is N, N-two alkylhalide groups-1,4-is to tetrafluoroborate or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid and the tetraethylammonium tetrafluoroborate of two rings along octane, solvent is an aprotic solvent, it is acetonitrile, propionitrile, the 3-methoxypropionitrile, gamma-butyrolacton, gamma-valerolactone, ethylene carbonate, propene carbonate, N, dinethylformamide, 1-Methyl-2-Pyrrolidone, dimethoxy-ethane, methylethylketone and oxolane, sulfolane, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dioxolanes, 1, the 4-butane sultone, the mixture of one or more in 1, the 3 propane sultone.Electrolyte concentration when room temperature is 0.5mol/l～2.0mol/l, and concentration preferably is 0.7～1.5mol/l, and optimum concentration is 0.8～1.2mol/l.Wherein the concentration of tetraethylammonium tetrafluoroborate is 0～0.7mol/l.
The phosphine dioxane halogen ammonium growth that the present invention proposes a kind of new tetrafluoroborate or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid uses as the supporting electrolyte of electrochemical capacitor in double electrode layer.Said phosphine ammonium salt demonstrates very high dissolubility and varies with temperature very for a short time in-60 ℃ aprotic solvent, this has determined the higher capacity and the higher voltage characteristic of capacitor model.Contain the DRXDACO cation in double charge three spaces and tetrafluoroborate or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid and be dissolved in the electrolyte of the present invention that forms in the aprotic solvent, the electrochemical capacitor in double electrode layer of making of this electrolyte in PC as the backup unit of memory, pulse power supply as electric motor car or spot welding device, load as battery in dissimilar AC-battery power source provides pulse power, or the like.
Description of drawings
Fig. 1 is DEFDACO
2+(BF
4 -)
2Acetonitrile solution (curve 1), gamma-butyrolacton solution (curve 2) and the conductivity of carbonic allyl ester solution (curve 3) and the graph of a relation of concentration.
Fig. 2 is 1M DEFDACO
2+(BF
4 -)
2Acetonitrile solution (curve 1), gamma-butyrolacton solution (curve 2) and the conductivity of carbonic allyl ester solution (curve 3) and the graph of a relation of temperature.
Fig. 3 for example understands 1M DEFDACO
2+(BF
4 -)
2Acetonitrile solution (curve 1) and 1MTEA
+BF
4 -The comparison of electrochemical window of acetonitrile solution (curve 2).
Embodiment
The tetrafluoroborate of DRXDACO of the present invention or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid are from Beijing Inst. of Chemical Reagent, and electrolyte sample provided by the invention has:
N-(2)-chloroethyl-N`-(2)-chloroethyl-1,4-is to the tetrafluoroborate (DEClDACO) of bicyclooctane
2+(BF
4 -)
2Gamma-butyrolacton solution;
N-(2)-fluoro ethyl-N`-(2)-fluoro ethyl-1,4-is to the tetrafluoroborate (DEFDACO) of bicyclooctane
2+(BF
4 -)
2Acetonitrile solution;
N-(2)-fluoro ethyl-N`-(2)-fluoro ethyl-1,4-is to the tetrafluoroborate (DEFDACO) of bicyclooctane
2+(BF
4 -)
2Gamma-butyrolacton solution;
N-(2)-fluoro ethyl-N`-(2)-fluoro ethyl-1,4-is to the tetrafluoroborate (DEFDACO) of bicyclooctane
2+(BF
4 -)
2Carbonic allyl ester solution;
N-(2)-fluoro ethyl-N`-(2)-fluoro ethyl-1,4-is to the tetrafluoroborate (DEFDACO) of bicyclooctane
2+(BF
4 -)
2Propene carbonate (75% volume) and dimethoxy-ethane (25% volume) solution;
N-(2)-fluoro ethyl-N`-(2)-fluoro ethyl-1,4-is to the tetrafluoroborate (DEFDACO) of bicyclooctane
2+(BF
4 -)
2Gamma-butyrolacton (75% volume) and methylethylketone (25% volume) solution;
N-(2)-bromoethyl-N`-(2)-bromoethyl-1,4-is to the hexafluoro borate (DEBrDACO) of bicyclooctane
2+(BF
6 -)
2Acetonitrile solution.
The DEFDACO of different quality
2+(BF
4 -)
2Sample dissolution forms concentration in acetonitrile, gamma-butyrolacton or the propene carbonate of 10ml be 0.5,0.75,1.0,1.25 and the solution of 1.5mol/l, and the conductivity value of measuring these solution in the time of 25 ℃ as shown in Figure 1.
The DEFDACO of different quality
2+(BF
4 -)
2Sample dissolution forms concentration in acetonitrile, gamma-butyrolacton or the propene carbonate of 10ml be the solution of 1.0mol/l, and the conductivity value of measuring these solution in the different temperatures scope of 30 ℃ to-30 ℃ or-40 ℃ as shown in Figure 2.
The DEFDACO of certain mass
2+(BF
4 -)
2Sample dissolution forms concentration in the mixed solvent of the gamma-butyrolacton (75% volume) of 10ml and dimethoxy-ethane (25% volume) be the solution of 1.0mol/l.In the time of 25 ℃, measure the conductivity value of this solution in table 1.
Embodiment 4
The DEFDACO of certain mass
2+(BF
4 -)
2Sample dissolution forms concentration in the mixed solvent of the propene carbonate (75% volume) of 10ml and dimethoxy-ethane (25% volume) be the solution of 1.0mol/l.In the time of 25 ℃, measure the conductivity value of this solution in table 1.
Embodiment 5
The DEBrDACO of certain mass
2+(PF
6 -)
2Sample dissolution forms concentration in the acetonitrile of 10ml be the solution of 1.0mol/l.In the time of 25 ℃, measure the conductivity value of this solution in table 1.
Embodiment 6
The DEClDACO of certain mass
2+(BF
4 -)
2Sample dissolution forms concentration in the gamma-butyrolacton of 10ml be the solution of 0.5mol/l.In the time of 25 ℃, measure the conductivity value of this solution in table 1.
According to the electrolyte of example 1 to 6 preparation their conductivity of test under different concentration and different temperature, the result of measurement is presented in appended drawings 1,2 and the table 1.Here
What Fig. 1 described is the electrolyte of example 1;
What Fig. 2 described is the electrolyte of example 2;
Table 1, first line description be the electrolyte of example 3;
Table 1, second line description be the electrolyte of example 4;
Table 1, what the third line was described is the electrolyte of example 5;
Table 1, what fourth line was described is the electrolyte of example 6;
Table 1
By Fig. 1,2 and table 1 as can be seen, the electrolyte of the present invention design all demonstrates quite high conductivity, the stationarity of this value depends on temperature in different solvents.
Below be the embodiment that electrolyte of the present invention is used.
Embodiment 7
Two work electrodes that the upright EDLC model of group comprises two collector electrodes made by aluminium foil and the 17.7mm that made by activated carbon cloth is long in argon gas and the spacer of making of nonwoven polypropylene that inserts betwixt.Work electrode and spacer all are immersed in 1MDEFDACO
2+(BF
4 -)
2Acetonitrile solution in.Then in the scope of 1.7-3.5V under the condition of constant current (3 or 10mA) this model of loop test, at room temperature determine its capacity and DC internal resistance by charging and discharging curve.These values are listed in the table 2.
Embodiment 8
Two work electrodes that the upright electrochemical capacitor in double electrode layer model of group comprises two collector electrodes made by aluminium foil and the 15.8mm that made by activated carbon cloth is long in argon gas and the spacer of making of nonwoven polypropylene that inserts betwixt.Work electrode and spacer all are immersed in 0.7M DEFDACO
2+(BF
4 -)
2With 0.5M TEA
+BF
4 -Acetonitrile solution in.Then in the scope of 1.7-3.2V under the condition of constant current (3 or 10mA) this model of loop test, at room temperature determine its capacity and DC internal resistance by charging and discharging curve.These values are listed in the table 2.
Embodiment 9
Two work electrodes that the upright electrochemical capacitor in double electrode layer model of group comprises two collector electrodes made by aluminium foil and the 15.8mm that made by activated carbon cloth is long in argon gas and the spacer of making of nonwoven polypropylene that inserts betwixt.Work electrode and spacer all are immersed in 0.3M DEFDACO
2+(BF
4 -)
2With 0.7M TEA
+BF
4 -Acetonitrile solution in.Then in the scope of 1.7-3.2V under the condition of constant current (3 or 10mA) this model of loop test, at room temperature determine its capacity and DC internal resistance by charging and discharging curve.These values are listed in the table 2.
Comprise 24 collector electrodes, 24 the work electrodes parallel spacer of making by aluminium foil with nonwoven polypropylene making that be connected and betwixt insert long with the 15 * 15mm that makes by activated carbon cloth at the electrochemical capacitor in double electrode layer model that group is stood in a specially designed polypropylene battery under the condition of argon gas.Work electrode and spacer all are immersed in 0.7M TEA
+BF
4 -And 0.8MDEFDACO
2+(BF
4 -)
2Acetonitrile solution in.The volume of electrolyte is 480ml, and whole model comprises that the quality of container approximately is 1 kilogram.Model through one macrocyclic seasoned-be 7 weeks of 2.5V first, its voltage progressively rises to 2.8-2.9V then, keeps this voltage more than 13 weeks.The monitoring capacitor parameters, for example its capacity, equivalent series resistance and self discharge, but do not find the variation of outward appearance and the deterioration of capacitor parameters at whole experimental session.
Embodiment 11
Two work electrodes that the upright electrochemical capacitor in double electrode layer model of group comprises two collector electrodes made by aluminium foil and the 15.8mm that made by activated carbon cloth is long in argon gas and the spacer of making of nonwoven polypropylene that inserts betwixt.Work electrode and spacer all are immersed in 1.0M TEA
+BF
4 -Acetonitrile solution in.Then in the scope of 1.7-3.2V under the condition of constant current (3 or 10mA) this model of loop test, at room temperature determine its capacity and DC internal resistance by charging and discharging curve.These values are listed in the table 2.
Should write down be DEFDACO and TEA (analog) tetrafluoroborate electrochemical window record and relatively see Fig. 3.These data are that to measure diameter with cyclic voltammetry be that the glassy carbon electrode of 2mm obtains; Sweep speed is 5mV/s.From figure as can be seen, the electrolyte of DEFDACO is compared the electrochemical window that has than broad with selected analog.The higher operating voltage of ratio of the electrochemical capacitor in double electrode layer device that DEFDACO electrolyte is formed is 3.2～3.5V, if use is that its operating voltage of TEA electrolyte is 2.8～3.2V.The increase of operating voltage will make that energy stored exceeds 20～30% in the electrochemical capacitor in double electrode layer device.
Table 2
Claims (5)
1, a kind of electrolyte of electrochemical capacitor in double electrode layer, solute is N, N-two alkylhalide groups-1,4-is to tetrafluoroborate or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid and the tetraethylammonium tetrafluoroborate of two rings along octane, solvent is an aprotic solvent, concentration of electrolyte is 0.5mol/l～2.0mol/l when room temperature, and wherein the concentration of tetraethylammonium tetrafluoroborate is 0～0.7mol/l.
2, according to the electrolyte of the described electrochemical capacitor in double electrode layer of claim 1, it is characterized in that aprotic solvent is acetonitrile, propionitrile, 3-methoxypropionitrile, gamma-butyrolacton, gamma-valerolactone, ethylene carbonate, propene carbonate, N, dinethylformamide, 1-Methyl-2-Pyrrolidone, dimethoxy-ethane, methylethylketone and oxolane, sulfolane, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, dioxolanes, 1, the mixture of one or more in 4-butane sultone, 1, the 3 propane sultone.
3, according to the electrolyte of the described electrochemical capacitor in double electrode layer of claim 1, it is characterized in that N, N-two alkylhalide groups-1,4-to two rings along the tetrafluoroborate of octane or hexafluorophosphate or perchlorate or trifluoromethyl sulfonic acid general formula is:
X is halogen F, Cl, Br or I; R is C
1～C
4Alkyl, i.e. methyl, ethyl, n-propyl group or n-butyl; Y is BF
4 -Perhaps PF
6 -Or ClO
- 4Perhaps CF
3SO
- 3Anion.
4, according to the electrolyte of the described electrochemical capacitor in double electrode layer of claim 1, it is characterized in that described when room temperature concentration of electrolyte be 0.7～1.5mol/l.
5, according to the electrolyte of claim 1 or 4 described electrochemical capacitor in double electrode layer, it is characterized in that described when room temperature concentration of electrolyte be 0.8～1.2mol/l.
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|---|---|---|---|
| CNB2006100470835A CN100536048C (en) | 2006-06-30 | 2006-06-30 | Electrolyte of electrochemical capacitor in double electrode layer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100470835A CN100536048C (en) | 2006-06-30 | 2006-06-30 | Electrolyte of electrochemical capacitor in double electrode layer |
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|---|---|
| CN1873866A CN1873866A (en) | 2006-12-06 |
| CN100536048C true CN100536048C (en) | 2009-09-02 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101307053B (en) * | 2008-07-04 | 2011-07-06 | 锦州凯美能源有限公司 | Method for preparing antisymmetric N,N'-1-4-dialkyl triethylene diammonium tetrafluoroborate |
| CN101840793A (en) * | 2010-04-29 | 2010-09-22 | 株洲日望电子科技有限公司 | Super capacitor and preparation method thereof |
| CN105070528B (en) * | 2015-07-16 | 2017-12-22 | 湖南中大新能源科技有限公司 | A kind of ultracapacitor electrolyte |
| CN105070530A (en) * | 2015-09-08 | 2015-11-18 | 上海空间电源研究所 | Electrolyte of super capacitor |
| CN110310842B (en) * | 2018-03-20 | 2022-03-18 | 中天超容科技有限公司 | Electrolyte of high-voltage capacitor, preparation method thereof and capacitor device |
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