CN102956373B - Electrolyte and compound method thereof - Google Patents
Electrolyte and compound method thereof Download PDFInfo
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- CN102956373B CN102956373B CN201110238001.6A CN201110238001A CN102956373B CN 102956373 B CN102956373 B CN 102956373B CN 201110238001 A CN201110238001 A CN 201110238001A CN 102956373 B CN102956373 B CN 102956373B
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- acid ester
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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
A kind of electrolyte, comprise methylsulfuric acid ester salt ion liquid and be dissolved in the alkyl silane in described methylsulfuric acid ester salt ion liquid, the mass ratio of described methylsulfuric acid ester salt ion liquid and described alkyl silane is 1: 0.001 ~ 1: 0.05.Above-mentioned electrolyte, by adding alkyl silane, inorganic acids impurity in alkyl silane and methylsulfuric acid ester salt ion liquid reacts, thus the inorganic acids impurity removed in methylsulfuric acid ester salt ion liquid, avoid inorganic acids impurity to corrode the aluminium foil of double layer capacitor, greatly can improve the stability using this methylsulfuric acid ester salt ion liquid to do the double layer capacitor of electrolyte; And the interpolation of alkyl silane can increase the stability of the double layer capacitor using this electrolyte, reduces costs.
Description
[technical field]
The present invention relates to a kind of electrolyte, particularly relate to a kind of electrolyte and the compound method thereof that contain methylsulfuric acid ester salt ion liquid.
[background technology]
Double electric layer capacitor is a kind of novel energy storage device, has the advantages such as high power density, high cycle life, fast charging and discharging performance be good, is widely used in the AC-battery power source etc. of military field, device for mobile communication, computer and electric automobile.As the important component part of double electric layer capacitor, the accumulate performance of electrolyte to double electric layer capacitor has a significant impact, and decides the equivalent internal resistance of capacitor, operating voltage range, accumulate capacity and working temperature and operational environment.
Ionic liquid be room temperature or close to the condition of room temperature under the organic liquid material that is composed entirely of ions.As a kind of novel electrolyte.Ionic liquid, as electrolyte, has the advantages such as electrochemical window is wide, non-volatile, non-combustible, Heat stability is good.Methylsulfuric acid ester salt ion liquid, because cost of material is low, is compare one of il electrolyte with DEVELOPMENT PROSPECT.But containing more inorganic acids impurity in methylsulfuric acid ester salt ion liquid, inorganic acid can corrode the aluminium foil of double layer capacitor, the stability using methylsulfuric acid ester salt ion liquid to make the double electric layer capacitor of electrolyte is caused to reduce.
[summary of the invention]
In view of above-mentioned condition, be necessary that providing a kind of increases electrolyte of the stability of double layer capacitor and preparation method thereof.
A kind of electrolyte, comprise methylsulfuric acid ester salt ion liquid and be dissolved in the alkyl silane in described methylsulfuric acid ester salt ion liquid, the mass ratio of described methylsulfuric acid ester salt ion liquid and described alkyl silane is 1: 0.001 ~ 1: 0.05.
In a preferred embodiment, described alkyl silane is methyl triethyl silicane or trimethyl butyl silane.
In a preferred embodiment, described methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.
In a preferred embodiment, described imidazole salt cation is 1-butyl-3-methyl imidazolium cation, 1-propyl group-3-methyl imidazolium cation or 1-ethyl-3-methylimidazole cation, described quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or thmethylpropyl quaternary ammonium cation, described pyrroles's salt cationoid is butyl methyl pyrroles cation, hydroxypropyl methyl pyrroles cation or ethyl-methyl pyrroles cation, described season, phosphonium salt cationoid was trimethyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season phosphine cation, described pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
A kind of electrolyte, comprises the product that can be obtained by following chemical reaction:
Step one, the methylsulfuric acid ester salt ion liquid providing mass ratio to be 1: 0.001 ~ 1: 0.05 and alkyl silane, containing inevitable impurity in described methylsulfuric acid ester salt ion liquid, described impurity is inorganic acid;
Step 2, in described methylsulfuric acid ester salt ion liquid, add alkyl silane and stirring and dissolving.
In a preferred embodiment, the mass ratio of described methylsulfuric acid ester salt ion liquid and described alkyl silane is 1: 0.01 ~ 1: 0.04.
In a preferred embodiment, described alkyl silane is methyl triethyl silicane or trimethyl butyl silane.
A compound method for electrolyte, comprises the following steps:
Step one, the methylsulfuric acid ester salt ion liquid providing mass ratio to be 1: 0.001 ~ 1: 0.05 and alkyl silane;
Step 2, in described methylsulfuric acid ester salt ion liquid, add described alkyl silane and stirring and dissolving.
In a preferred embodiment, described methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.
In a preferred embodiment, described alkyl silane is methyl triethyl silicane or trimethyl butyl silane.
Above-mentioned electrolyte, by adding alkyl silane, alkyl silane can react with the mineral acid impurities in trifluoroacetic acid salt ionic liquid, thus the mineral acid impurities removed in methylsulfuric acid ester salt ion liquid, avoid inorganic acid to corrode the aluminium foil of double layer capacitor, the stability using this methylsulfuric acid ester salt ion liquid to do the double layer capacitor of electrolyte can be improved; And the interpolation of alkyl silane can increase the stability of the double layer capacitor using this electrolyte, reduces costs.
[accompanying drawing explanation]
Fig. 1 is double layer capacitor and the ratio capacitance value of traditional double layer capacitor under different cycle-index of the electrolyte used in embodiment one.
[embodiment]
Below in conjunction with specific embodiment, electrolyte and compound method thereof are described in further details.
The electrolyte of one execution mode, comprise methylsulfuric acid ester salt ion liquid and be dissolved in the alkyl silane in described methylsulfuric acid ester salt ion liquid, the mass ratio of described methylsulfuric acid ester salt ion liquid and described alkyl silane is 1: 0.001 ~ 1: 0.05.
Methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.Containing inevitable mineral acid impurities in methylsulfuric acid ester salt ion liquid, mineral acid impurities is at least one in sulfuric acid and hydrochloric acid.
Preferably, imidazole salt cation is 1-butyl-3-methyl imidazolium cation, 1-propyl group-3-methyl imidazolium cation or 1-ethyl-3-methylimidazole cation.
Preferably, quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or thmethylpropyl quaternary ammonium cation.
Preferably, pyroles cation is butyl methyl pyrroles cation, hydroxypropyl methyl pyrroles cation or ethyl-methyl pyrroles cation.
Preferably, season phosphonium salt cationoid be trimethyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season phosphine cation.
Preferably, pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
Alkyl silane is preferably methyl triethyl silicane or trimethyl butyl silane.Be appreciated that alkyl silane is not limited to methyl triethyl silicane or trimethyl butyl silane, as long as can react with the mineral acid impurities in methylsulfuric acid ester salt ion liquid.
The mass ratio of methylsulfuric acid ester salt ion liquid and alkyl silane is preferably 1: 0.01 ~ 1: 0.04.
Above-mentioned electrolyte, by adding alkyl silane, mineral acid impurities in alkyl silane and methylsulfuric acid ester salt ion liquid reacts thus removes the inorganic acid in methylsulfuric acid ester salt ion liquid, avoid inorganic acid to corrode the aluminium foil of double layer capacitor, greatly can improve the stability using this methylsulfuric acid ester salt ion liquid to do the double layer capacitor of electrolyte; And the interpolation of alkyl silane can increase the stability of the double layer capacitor using this electrolyte, reduces costs.
The electrolyte of one execution mode, comprises the product that can be obtained by following chemical reaction:
Step one, the methylsulfuric acid ester salt ion liquid providing mass ratio to be 1: 0.001 ~ 1: 0.05 and alkyl silane, containing inevitable impurity in methylsulfuric acid ester salt ion liquid, described impurity is inorganic acid.
Methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.
Preferably, imidazole salt cation is 1-butyl-3-methyl imidazolium cation, 1-propyl group-3-methyl imidazolium cation or 1-ethyl-3-methylimidazole cation.
Preferably, quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or thmethylpropyl quaternary ammonium cation.
Preferably, pyroles cation is butyl methyl pyrroles cation, hydroxypropyl methyl pyrroles cation or ethyl-methyl pyrroles cation.
Preferably, season phosphonium salt cationoid be trimethyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season phosphine cation.
Preferably, pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
Inorganic acid is the one in sulfuric acid and hydrochloric acid.
Alkyl silane is preferably methyl triethyl silicane or trimethyl butyl silane.Be appreciated that alkyl silane is not limited to methyl triethyl silicane or trimethyl butyl silane, as long as can react with the mineral acid impurities in methylsulfuric acid ester salt ion liquid.
The mass ratio of methylsulfuric acid ester salt ion liquid and alkyl silane is preferably 1: 0.01 ~ 1: 0.04.
Step 2, in methylsulfuric acid ester salt ion liquid, add alkyl silane and stirring and dissolving.
Time prepared by above-mentioned electrolyte, by adding alkyl silane in methylsulfuric acid ester salt ion liquid, mineral acid impurities in alkyl silane and methylsulfuric acid ester salt ion liquid occurs thus removes the inorganic acid in methylsulfuric acid ester salt ion liquid, avoid inorganic acid to corrode the aluminium foil of double layer capacitor, greatly can improve the stability using this methylsulfuric acid ester salt ion liquid to do the double layer capacitor of electrolyte; And the interpolation of alkyl silane can increase the stability of the double layer capacitor using this electrolyte, reduces costs.
The compound method of the electrolyte of one execution mode, comprises the following steps:
Step one, the methylsulfuric acid ester salt ion liquid providing mass ratio to be 1: 0.001 ~ 1: 0.05 and alkyl silane.
Methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.Containing inevitable mineral acid impurities in methylsulfuric acid ester salt ion liquid, mineral acid impurities is at least one in sulfuric acid and hydrochloric acid.
Preferably, imidazole salt cation is 1-butyl-3-methyl imidazolium cation, 1-propyl group-3-methyl imidazolium cation or 1-ethyl-3-methylimidazole cation.
Preferably, quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or thmethylpropyl quaternary ammonium cation.
Preferably, pyroles cation is butyl methyl pyrroles cation, hydroxypropyl methyl pyrroles cation or ethyl-methyl pyrroles cation.
Preferably, season phosphonium salt cationoid be trimethyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season phosphine cation.
Preferably, pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
Alkyl silane is preferably methyl triethyl silicane or trimethyl butyl silane.Be appreciated that alkyl silane is not limited to methyl triethyl silicane or trimethyl butyl silane, as long as can react with the mineral acid impurities in methylsulfuric acid ester salt ion liquid.
The mass ratio of methylsulfuric acid ester salt ion liquid and alkyl silane is preferably 1: 0.01 ~ 1: 0.04.
Step 2, in methylsulfuric acid ester salt ion liquid, add alkyl silane and stirring and dissolving.
The compound method of above-mentioned electrolyte, alkyl silane is added in methylsulfuric acid ester salt ion liquid, mineral acid impurities in alkyl silane and methylsulfuric acid ester salt ion liquid occurs thus removes the inorganic acid in methylsulfuric acid ester salt ion liquid, avoid inorganic acid to corrode the aluminium foil of double layer capacitor, greatly can improve the stability using this methylsulfuric acid ester salt ion liquid to do the double layer capacitor of electrolyte; And the interpolation of alkyl silane can increase the stability of the double layer capacitor using this electrolyte, reduces costs.
Be below embodiment part:
Embodiment one
Alkyl silane is added in methylsulfuric acid ester salt ion liquid, be stirred to dissolving and can obtain electrolyte.
In present embodiment, alkyl silane is methyl triethyl silicane, and methylsulfuric acid ester salt ion liquid is 1-ethyl-3-methylimidazole methylsulfuric acid ester salt, and the mass ratio of methylsulfuric acid ester salt ion liquid and alkyl silane is 1: 0.04.
In present embodiment, during preparation electrolyte, carry out in glove box, methyl triethyl silicane is added stirring in 1-ethyl-3-methylimidazole methylsulfuric acid ester salt and within 10 ~ 60 minutes, make methyl triethyl silicane be dissolved in 1-ethyl-3-methylimidazole methylsulfuric acid ester salt.
Above-mentioned electrolyte is applied to double layer capacitor and measures this double layer capacitor stability.
During measuring stability, take Graphene as electrode material, use electrolyte prepared by embodiment one, be assembled into button cell, utilize CHI660A electrochemical workstation to carry out constant current charge-discharge test to it, record its ratio capacitance conservation rate, namely under 30 degrees celsius, in 0 ~ 2.5v window ranges, the ratio capacitance after circulating with the constant current repeated charge 1000 of 1A/g and the ratio of first charge-discharge ratio capacitance.
Refer to Fig. 1, Fig. 1 uses the double layer capacitor of the electrolyte in the present embodiment and uses the methylsulfuric acid ester salt ion liquid not adding methyl triethyl silicane as the ratio capacitance value of double layer capacitor under different cycle-index of electrolyte.As can be seen from Figure 1, the first charge-discharge ratio capacitance of the double layer capacitor of electrolyte using the present embodiment to provide is 108.66F/g, and the ratio capacitance after 1000 times that circulates is 102.48F/g, and its conservation rate is 94.31%; And using the methylsulfuric acid ester salt ion liquid that do not add methyl triethyl silicane to be 108.7F/g as the first charge-discharge ratio capacitance of the double layer capacitor of electrolyte, the ratio capacitance after 1000 times that circulates is 83.03F/g, and its conservation rate is 76.38%; The methylsulfuric acid ester salt ion liquid 1-ethyl-3-methylimidazole methylsulfuric acid ester salt using the ratio capacitance conservation rate of double layer capacitor of the electrolyte of the present embodiment not add methyl triethyl silicane than the use recorded under equal conditions improves 17.93% as the ratio capacitance conservation rate of the double layer capacitor of electrolyte, uses the stability of the double layer capacitor of the electrolyte of the present embodiment to be greatly improved.
Embodiment two to ten eight
In embodiment two to ten eight, alkyl silane is added in methylsulfuric acid ester salt ion liquid, be stirred to dissolving and can obtain electrolyte.During preparation electrolyte, carry out in glove box.
In embodiment two to ten eight, the ratio that the ratio capacitance conservation rate after the proportioning of alkyl silane, methylsulfuric acid ester salt ion liquid, methylsulfuric acid ester salt ion liquid and alkyl silane, mixing time, circulation 1000 times and ratio capacitance conservation rate improve is see table 1.
Table 1 embodiment two to ten eight electrolyte prescription and test result
In embodiment two to ten eight, ratio capacitance conservation rate condition determination is identical with embodiment one; The ratio that ratio capacitance conservation rate improves be the corresponding methylsulfuric acid ester salt ion liquid that uses the ratio capacitance conservation rate of the double layer capacitor of the electrolyte of corresponding embodiment and the use recorded under equal conditions not to add alkyl silane as the double layer capacitor of electrolyte ratio capacitance conservation rate compared with the percentage of raising.
As can be seen from the above table, use the ratio capacitance conservation rate of the double layer capacitor of electrolyte provided by the invention to be greatly improved, use the stability of the double layer capacitor of electrolyte provided by the invention to be improved.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an electrolyte, it is characterized in that: comprise methylsulfuric acid ester salt ion liquid and be dissolved in the alkyl silane in described methylsulfuric acid ester salt ion liquid, the mass ratio of described methylsulfuric acid ester salt ion liquid and described alkyl silane is 1:0.001 ~ 1:0.05.
2. electrolyte as claimed in claim 1, is characterized in that: described alkyl silane is methyl triethyl silicane or trimethyl butyl silane.
3. electrolyte as claimed in claim 1, is characterized in that: described methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternaries cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.
4. electrolyte as claimed in claim 3, it is characterized in that: described imidazole salt cation is 1-butyl-3-methyl imidazolium cation, 1-propyl group-3-methyl imidazolium cation or 1-ethyl-3-methylimidazole cation, described quaternaries cation is methyl triethyl quaternary amine cation, tetraethyl quaternary ammonium cation or thmethylpropyl quaternary ammonium cation, described pyrroles's salt cationoid is butyl methyl pyrroles cation, hydroxypropyl methyl pyrroles cation or ethyl-methyl pyrroles cation, described season, phosphonium salt cationoid was trimethyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season phosphine cation, described pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
5. an electrolyte, is characterized in that, comprises the product that can be obtained by following chemical reaction:
Step one, the methylsulfuric acid ester salt ion liquid providing mass ratio to be 1:0.001 ~ 1:0.05 and alkyl silane, containing inevitable impurity in described methylsulfuric acid ester salt ion liquid, described impurity is inorganic acid;
Step 2, in described methylsulfuric acid ester salt ion liquid, add alkyl silane and stirring and dissolving.
6. electrolyte as claimed in claim 5, is characterized in that: the mass ratio of described methylsulfuric acid ester salt ion liquid and described alkyl silane is 1:0.01 ~ 1:0.04.
7. electrolyte as claimed in claim 5, is characterized in that: described alkyl silane is methyl triethyl silicane or trimethyl butyl silane.
8. a compound method for electrolyte, comprises the following steps:
Step one, the methylsulfuric acid ester salt ion liquid providing mass ratio to be 1:0.001 ~ 1:0.05 and alkyl silane;
Step 2, in described methylsulfuric acid ester salt ion liquid, add described alkyl silane and stirring and dissolving.
9. the compound method of electrolyte as claimed in claim 8, is characterized in that: described methylsulfuric acid ester salt ion liquid by methylsulfuric acid ester anion and imidazole salt cation, quaternaries cation, pyrroles's salt cationoid, season phosphonium salt cationoid or pyridiniujm cationoid form.
10. the compound method of electrolyte as claimed in claim 8, is characterized in that: described alkyl silane is methyl triethyl silicane or trimethyl butyl silane.
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| KR102188220B1 (en) * | 2013-04-01 | 2020-12-08 | 우베 고산 가부시키가이샤 | Nonaqueous electrolyte solution and electricity storage device using same |
| EP2803302B1 (en) * | 2013-05-14 | 2015-12-30 | Eksen Makine Sanayi ve Ticaret A.S. | Chemically stable, stain-, abrasion- and temperature-resistant, easy-to-clean sol-gel coated metalware for use in elevated temperatures |
| JP6651968B2 (en) * | 2016-04-21 | 2020-02-19 | 日清紡ホールディングス株式会社 | Silicon-containing sulfate |
| JP7085139B2 (en) * | 2018-12-18 | 2022-06-16 | トヨタ自動車株式会社 | Electrolyte for lithium secondary battery and lithium secondary battery |
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| JP2003297700A (en) * | 2002-03-29 | 2003-10-17 | Meidensha Corp | Electric double-layer capacitor and its manufacturing method |
| CN1471743A (en) * | 2000-09-07 | 2004-01-28 | ������������ʽ���� | Additive for non-aqueous liquid electrolyte, non-aqueous liquid electrolyte secondary cell and no-aqueous liquid electrolyte electric double layer capacitor |
| CN101284791A (en) * | 2001-03-26 | 2008-10-15 | 日清纺织株式会社 | Electrolytic solution for storage device, and electric double layer capacitor |
| CN102089348A (en) * | 2008-07-11 | 2011-06-08 | 徐光锡 | Organic solvent-dispersible conductive polymer and method for manufacture thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1471743A (en) * | 2000-09-07 | 2004-01-28 | ������������ʽ���� | Additive for non-aqueous liquid electrolyte, non-aqueous liquid electrolyte secondary cell and no-aqueous liquid electrolyte electric double layer capacitor |
| CN101284791A (en) * | 2001-03-26 | 2008-10-15 | 日清纺织株式会社 | Electrolytic solution for storage device, and electric double layer capacitor |
| JP2003297700A (en) * | 2002-03-29 | 2003-10-17 | Meidensha Corp | Electric double-layer capacitor and its manufacturing method |
| CN102089348A (en) * | 2008-07-11 | 2011-06-08 | 徐光锡 | Organic solvent-dispersible conductive polymer and method for manufacture thereof |
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