CN102956372A - Electrolyte and preparation method thereof - Google Patents
Electrolyte and preparation method thereof Download PDFInfo
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- CN102956372A CN102956372A CN2011102379998A CN201110237999A CN102956372A CN 102956372 A CN102956372 A CN 102956372A CN 2011102379998 A CN2011102379998 A CN 2011102379998A CN 201110237999 A CN201110237999 A CN 201110237999A CN 102956372 A CN102956372 A CN 102956372A
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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
Abstract
An electrolyte comprises thiocyanate ionic liquid and an N-Si based compound dissolved in the thiocyanate ionic liquid. The mass ratio of the thiocyanate ionic liquid and the N-Si based compound is 1:(0.001-1):0.05. In the electrolyte, the added N-Si based compound removes water in the thiocyanate ionic liquid by disconnecting an N-Si key and coordinates with thiocyanate radical, and accordingly hydrolysis of the thiocyanate radical is prevented, stability of a double-layer capacitor using the thiocyanate ionic liquid as the electrolyte is improved, the stability of the double-layer capacitor using the electrolyte can be improved by adding the N-Si based compound, and cost is lowered.
Description
[technical field]
The present invention relates to a kind of electrolyte, relate in particular to a kind of electrolyte and compound method thereof that contains thiocyanic acid salt ionic 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 of military field, device for mobile communication, computer and electric automobile etc.As the important component part of double electric layer capacitor, electrolyte has a significant impact the accumulate performance of double electric layer capacitor, is determining the equivalent internal resistance of capacitor, operating voltage range, accumulate capacity and working temperature and operational environment.
Ionic liquid is in room temperature or the organic liquid material that is comprised of ion fully under near the condition of room temperature.As a kind of novel electrolyte.Ionic liquid has the advantages such as electrochemical window is wide, non-volatile, not flammable, Heat stability is good as electrolyte.Thiocyanic acid salt ionic liquid is one of il electrolyte that relatively has DEVELOPMENT PROSPECT because cost of material is low.Yet, contain inevitable impurity (water) in the thiocyanic acid salt ionic liquid, in the electrochemistry cyclic process, thiocyanate radical is unstable, easily hydrolysis, the stability of the double electric layer capacitor that causes using thiocyanic acid salt ionic liquid to do electrolyte reduces.
[summary of the invention]
In view of above-mentioned condition, be necessary to provide electrolyte of a kind of stability that increases double layer capacitor and preparation method thereof.
A kind of electrolyte comprises thiocyanic acid salt ionic liquid and is dissolved in the compound that contains the N-Si base in the described thiocyanic acid salt ionic liquid that the mass ratio of the compound of described thiocyanic acid salt ionic liquid and the described N-Si of containing base is 1: 0.001～1: 0.05.
In a preferred embodiment, the compound of the described N-Si of containing base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.
In a preferred embodiment, described thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.
In a preferred embodiment, described imidazole salt cation is 1-butyl-3-methylimidazole cation, 1-propyl group-3-methylimidazole cation or 1-ethyl-3-methylimidazole cation, described quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or trimethyl propyl group quaternary ammonium cation, described pyrroles's salt cationoid is butyl methyl pyrroles cation, propyl group methylpyrrole cation or ethyl-methyl pyrroles cation, described season, the phosphonium salt cationoid was trimethyl hexyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season the phosphine cation, described pyridiniujm cationoid is the 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 1, mass ratio is provided is 1: 0.001～1: 0.05 thiocyanic acid salt ionic liquid and contain the compound of N-Si base, contains inevitable impurity in the described thiocyanic acid salt ionic liquid, and described impurity is water;
Step 2, add compound and the stirring and dissolving that contains the N-Si base in the described thiocyanic acid salt ionic liquid.
In a preferred embodiment, the mass ratio of the compound of described thiocyanic acid salt ionic liquid and the described N-Si of containing base is 1: 0.008～1: 0.02.
In a preferred embodiment, the compound of the described N-Si of containing base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.
A kind of compound method of electrolyte may further comprise the steps:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 thiocyanic acid salt ionic liquid and contain the compound of N-Si base;
Step 2, add described compound and the stirring and dissolving that contains the N-Si base in the described thiocyanic acid salt ionic liquid.
In a preferred embodiment, described thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.
In a preferred embodiment, the compound of the described N-Si of containing base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.
Above-mentioned electrolyte, the compound that contains the N-Si base by adding, the compound that contains the N-Si base is removed water in the thiocyanic acid salt ionic liquid simultaneously by disconnecting the N-Si key, and with the thiocyanate radical coordination, thereby can prevent the thiocyanate radical hydrolysis, improve the stability of using this thiocyanic acid salt ionic liquid to do the double layer capacitor of electrolyte; And the interpolation that contains the compound of N-Si base can increase the stability of the double layer capacitor that uses this electrolyte, reduces cost.
[description of drawings]
Fig. 1 is the double layer capacitor of the electrolyte among the use embodiment one and the traditional ratio capacitance of double layer capacitor under different cycle-indexes.
[embodiment]
Below in conjunction with specific embodiment electrolyte and compound method thereof are described in further details.
The electrolyte of one execution mode, comprise thiocyanic acid salt ionic liquid and be dissolved in the compound that contains the N-Si base in the described thiocyanic acid salt ionic liquid, the mass ratio of the compound of described thiocyanic acid salt ionic liquid and the described N-Si of containing base is 1: 0.001～1: 0.05.
Thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.Contain inevitable impurity in the thiocyanic acid salt ionic liquid, impurity is water.
Preferably, the imidazole salt cation is 1-butyl-3-methylimidazole cation, 1-propyl group-3-methylimidazole cation or 1-ethyl-3-methylimidazole cation.
Preferably, the quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or trimethyl propyl group quaternary ammonium cation.
Preferably, the pyroles cation is butyl methyl pyrroles cation, propyl group methylpyrrole cation or ethyl-methyl pyrroles cation.
Preferably, season the phosphonium salt cationoid be trimethyl hexyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season the phosphine cation.
Preferably, the pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
The compound that contains the N-Si base is preferably N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.Be appreciated that the compound that contains the N-Si base is not limited to N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane are removed simultaneously water and are got final product with the compound of thiocyanate radical coordination so long as can disconnect the N-Si key.
Thiocyanic acid salt ionic liquid is preferably 1: 0.008 with the mass ratio that contains the compound of N-Si base～and 1: 0.02.
Above-mentioned electrolyte, the compound that contains the N-Si base by adding, the compound that contains the N-Si base is removed water in the thiocyanic acid salt ionic liquid simultaneously by disconnecting the N-Si key, and with the thiocyanate radical coordination, thereby can prevent the thiocyanate radical hydrolysis, improve the stability of using this thiocyanic acid salt ionic liquid to do the double layer capacitor of electrolyte; And the interpolation that contains the compound of N-Si base can increase the stability of the double layer capacitor that uses this electrolyte, reduces cost.
The electrolyte of one execution mode comprises the product that can be obtained by following chemical reaction:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 thiocyanic acid salt ionic liquid and contain the compound of N-Si base, contains inevitable impurity in the thiocyanic acid salt ionic liquid, and impurity is water.
Thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.
Preferably, the imidazole salt cation is 1-butyl-3-methylimidazole cation, 1-propyl group-3-methylimidazole cation or 1-ethyl-3-methylimidazole cation.
Preferably, the quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or trimethyl propyl group quaternary ammonium cation.
Preferably, the pyroles cation is butyl methyl pyrroles cation, propyl group methylpyrrole cation or ethyl-methyl pyrroles cation.
Preferably, season the phosphonium salt cationoid be trimethyl hexyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season the phosphine cation.
Preferably, the pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
The compound that contains the N-Si base is preferably N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.Be appreciated that the compound that contains the N-Si base is not limited to N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane are removed simultaneously water and are got final product with the thiocyanate radical coordination so long as can disconnect the N-Si key.
Thiocyanic acid salt ionic liquid is preferably 1: 0.008 with the mass ratio that contains the compound of N-Si base～and 1: 0.02.
Step 2, add compound and the stirring and dissolving that contains the N-Si base in the thiocyanic acid salt ionic liquid.
When above-mentioned electrolyte prepares, by in thiocyanic acid salt ionic liquid, adding the compound that contains the N-Si base, the compound that contains the N-Si base is removed water in the thiocyanic acid salt ionic liquid simultaneously by disconnecting the N-Si key, and with the thiocyanate radical coordination, thereby can prevent the thiocyanate radical hydrolysis, improve the stability of using this thiocyanic acid salt ionic liquid to do the double layer capacitor of electrolyte; And the interpolation that contains the compound of N-Si base can increase the stability of the double layer capacitor that uses this electrolyte, reduces cost.
The compound method of the electrolyte of one execution mode may further comprise the steps:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 thiocyanic acid salt ionic liquid and contain the compound of N-Si base.
Thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.Contain inevitable impurity in the thiocyanic acid salt ionic liquid, impurity is water.
Preferably, the imidazole salt cation is 1-butyl-3-methylimidazole cation, 1-propyl group-3-methylimidazole cation or 1-ethyl-3-methylimidazole cation.
Preferably, the quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or trimethyl propyl group quaternary ammonium cation.
Preferably, the pyroles cation is butyl methyl pyrroles cation, propyl group methylpyrrole cation or ethyl-methyl pyrroles cation.
Preferably, season the phosphonium salt cationoid be trimethyl hexyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season the phosphine cation.
Preferably, the pyridiniujm cationoid is butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
The compound that contains the N-Si base is preferably N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.Be appreciated that the compound that contains the N-Si base is not limited to N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane are removed simultaneously water and are got final product with the thiocyanate radical coordination so long as can disconnect the N-Si key.
Thiocyanic acid salt ionic liquid is preferably 1: 0.008 with the mass ratio that contains the compound of N-Si base～and 1: 0.02.
Step 2, add compound and the stirring and dissolving that contains the N-Si base in the thiocyanic acid salt ionic liquid.
The compound method of above-mentioned electrolyte, in thiocyanic acid salt ionic liquid, add the compound that contains the N-Si base, the compound that contains the N-Si base is removed water in the thiocyanic acid salt ionic liquid simultaneously by disconnecting the N-Si key, and with the thiocyanate radical coordination, thereby can prevent the thiocyanate radical hydrolysis, can improve the stability of using this thiocyanic acid salt ionic liquid to do the double layer capacitor of electrolyte; And the interpolation that contains the compound of N-Si base can increase the stability of the double layer capacitor that uses this electrolyte, reduces cost.
Below be the embodiment part:
Embodiment one
The compound that will contain the N-Si base adds and to be stirred to dissolving in the thiocyanic acid salt ionic liquid and can to obtain electrolyte.
In the present embodiment, the compound that contains the N-Si base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-, thiocyanic acid salt ionic liquid are 1-ethyl-3-methylimidazole rhodanate, and thiocyanic acid salt ionic liquid is 1: 0.02 with the mass ratio that contains the compound of N-Si base.
In the present embodiment, during preparation electrolyte, in glove box, carry out, with N, N-diethyl-1,1, the trimethyl silicon based amine of 1-adds to stir in the 1-ethyl-3-methylimidazole rhodanate made N in 10～60 minutes, N-diethyl-1,1, the trimethyl silicon based amine of 1-is dissolved in the 1-ethyl-3-methylimidazole rhodanate.
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 the electrolyte of embodiment one preparation, be assembled into button cell, utilize the CHI660A electrochemical workstation that it is carried out the constant current charge-discharge test, record it than electric capacity conservation rate, namely under 30 degrees celsius, in 0～2.5v window ranges, with the ratio electric capacity and the ratio of first charge-discharge than electric capacity after 1000 circulations of constant current repeated charge of 1A/g.
See also Fig. 1, Fig. 1 does not add N for the double layer capacitor that uses the electrolyte in the present embodiment with use, N-diethyl-1,1, the thiocyanic acid salt ionic liquid of the trimethyl silicon based amine of 1-is as the ratio capacitance of double layer capacitor under different cycle-indexes of electrolyte.As can be seen from Figure 1, use the first charge-discharge of the double layer capacitor of the electrolyte that the present embodiment provides to be 108.48F/g than electric capacity, the ratio electric capacity that circulates after 1000 times is 105.67F/g, and its conservation rate is 97.41%; Do not add N and use, N-diethyl-1,1, the thiocyanic acid salt ionic liquid of the trimethyl silicon based amine of 1-is 108.7F/g as the first charge-discharge of the double layer capacitor of electrolyte than electric capacity, the ratio electric capacity that circulates after 1000 times is 83.03F/g, and its conservation rate is 76.38%; Use the present embodiment electrolyte double layer capacitor do not add N than electric capacity conservation rate than the use that records under the equal conditions, N-diethyl-1,1, the thiocyanic acid salt ionic liquid 1-ethyl-3-methylimidazole rhodanate of the trimethyl silicon based amine of 1-has improved 17.93% as the double layer capacitor of electrolyte than electric capacity conservation rate, uses the stability of double layer capacitor of the electrolyte of the present embodiment to be greatly improved.
Embodiment two to 18
Among the embodiment two to 18, the compound that will contain the N-Si base adds in the thiocyanic acid salt ionic liquid, is stirred to dissolving and can obtains electrolyte.During preparation electrolyte, in glove box, carry out.
Among the embodiment two to 18, the ratio that improves than electric capacity conservation rate and than electric capacity conservation rate after the compound, thiocyanic acid salt ionic liquid, thiocyanic acid salt ionic liquid that contains the N-Si base and proportioning, mixing time, the circulation of the compound that contains the N-Si base 1000 times is referring to table 1.
Electrolyte prescription and test data among table 1 embodiment two to 18
Among the embodiment two to 18, than identical among electric capacity conservation rate condition determination and the embodiment one; The ratio that improves than electric capacity conservation rate does not add the compound that contains the N-Si base for the use than recording under electric capacity conservation rate and the equal conditions of the double layer capacitor of the electrolyte that uses corresponding embodiment corresponding thiocyanic acid salt ionic liquid is compared the percentage of raising as the double layer capacitor of electrolyte than electric capacity conservation rate.
As can be seen from the above table, use being greatly improved than electric capacity conservation rate of double layer capacitor of electrolyte provided by the invention, use the stability of the double layer capacitor of electrolyte provided by the invention to be improved.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.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. electrolyte, it is characterized in that: comprise thiocyanic acid salt ionic liquid and be dissolved in the compound that contains the N-Si base in the described thiocyanic acid salt ionic liquid, the mass ratio of the compound of described thiocyanic acid salt ionic liquid and the described N-Si of containing base is 1: 0.001～1: 0.05.
2. electrolyte as claimed in claim 1, it is characterized in that: the compound of the described N-Si of containing base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.
3. electrolyte as claimed in claim 1 is characterized in that: described thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.
4. electrolyte as claimed in claim 3, it is characterized in that: described imidazole salt cation is 1-butyl-3-methylimidazole cation, 1-propyl group-3-methylimidazole cation or 1-ethyl-3-methylimidazole cation, described quaternary ammonium salts cation is methyl triethyl group quaternary ammonium cation, tetraethyl quaternary ammonium cation or trimethyl propyl group quaternary ammonium cation, described pyrroles's salt cationoid is butyl methyl pyrroles cation, propyl group methylpyrrole cation or ethyl-methyl pyrroles cation, described season, the phosphonium salt cationoid was trimethyl hexyl season phosphine cation, triethyl group hexyl season phosphine cation or tri-methyl-amyl season the phosphine cation, described pyridiniujm cationoid is the butyl-pyridinium cation, pentyl pyridine cation or hexyl pyridylium.
5. an electrolyte is characterized in that, comprises the product that is obtained by following chemical reaction:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 thiocyanic acid salt ionic liquid and contain the compound of N-Si base, contains inevitable impurity in the described thiocyanic acid salt ionic liquid, and described impurity is water;
Step 2, add compound and the stirring and dissolving that contains the N-Si base in the described thiocyanic acid salt ionic liquid.
6. electrolyte as claimed in claim 5, it is characterized in that: the mass ratio of the compound of described thiocyanic acid salt ionic liquid and the described N-Si of containing base is 1: 0.008～1: 0.02.
7. electrolyte as claimed in claim 5, it is characterized in that: the compound of the described N-Si of containing base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.
8. the compound method of an electrolyte may further comprise the steps:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 thiocyanic acid salt ionic liquid and contain the compound of N-Si base;
Step 2, add described compound and the stirring and dissolving that contains the N-Si base in the described thiocyanic acid salt ionic liquid.
9. the compound method of electrolyte as claimed in claim 8 is characterized in that: described thiocyanic acid salt ionic liquid by thiocyanate radical anion and imidazole salt cation, quaternary ammonium salts cation, pyrroles's salt cationoid, season the phosphonium salt cationoid or the pyridiniujm cationoid consist of.
10. the compound method of electrolyte as claimed in claim 8, it is characterized in that: the compound of the described N-Si of containing base is N, N-diethyl-1,1, the trimethyl silicon based amine of 1-or hexamethyldisiloxane.
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| CN103467382A (en) * | 2013-09-16 | 2013-12-25 | 浙江丽晶化学有限公司 | Method for preparing thiocyanate-containing ionic liquid and application of ionic liquid in polyacrylonitrile spinning processing |
| CN103730263A (en) * | 2013-12-27 | 2014-04-16 | 深圳新宙邦科技股份有限公司 | Organic electrolytic solution for super capacitor and super capacitor |
| CN108682567A (en) * | 2018-05-09 | 2018-10-19 | 中国科学院兰州化学物理研究所 | A method of constructing high-performance super capacitor by adjusting electrode voltage range |
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Cited By (3)
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| CN103467382A (en) * | 2013-09-16 | 2013-12-25 | 浙江丽晶化学有限公司 | Method for preparing thiocyanate-containing ionic liquid and application of ionic liquid in polyacrylonitrile spinning processing |
| CN103730263A (en) * | 2013-12-27 | 2014-04-16 | 深圳新宙邦科技股份有限公司 | Organic electrolytic solution for super capacitor and super capacitor |
| CN108682567A (en) * | 2018-05-09 | 2018-10-19 | 中国科学院兰州化学物理研究所 | A method of constructing high-performance super capacitor by adjusting electrode voltage range |
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Application publication date: 20130306 |