CN102956369A - Electrolyte and preparation method thereof - Google Patents
Electrolyte and preparation method thereof Download PDFInfo
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- CN102956369A CN102956369A CN2011102379216A CN201110237921A CN102956369A CN 102956369 A CN102956369 A CN 102956369A CN 2011102379216 A CN2011102379216 A CN 2011102379216A CN 201110237921 A CN201110237921 A CN 201110237921A CN 102956369 A CN102956369 A CN 102956369A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
An electrolyte comprises hexafluorophosphate ionic liquid and an alcohol amine compound dissolved in the hexafluorophosphate ionic liquid. The mass ratio of the hexafluorophosphate ionic liquid and the alcohol amine compound is 1 :( 0.001-1):0.05. In the electrolyte, the added alcohol amine compound can suppress hydrolysis and pyrolysis of PF6- in the hexafluorophosphate ionic liquid during electrochemical cycling, and accordingly stability of a double-layer capacitor using the ionic liquid as the electrolyte can be greatly improved. And the invention further provides another electrolyte and a preparation method of the electrolyte.
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 hexafluorophosphoric 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.Hexafluoro phosphonates ionic liquid is because synthetic technology is ripe, cost is low, it is one of at present the most frequently used il electrolyte, yet, in the electrochemistry cyclic process, the hexafluoro phosphonate radical is hydrolysis and pyrolysis easily, causes the poor stability that uses hexafluoro phosphonates ionic liquid to make the double electric layer capacitor of electrolyte.
[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 hexafluorophosphoric acid salt ionic liquid and is dissolved in alcamine compound in the described hexafluorophosphoric acid salt ionic liquid that the mass ratio of described hexafluorophosphoric acid salt ionic liquid and described alcamine compound is 1: 0.001～1: 0.05.
In a preferred embodiment, described alcamine compound is monoethanolamine or Propanolamine.
In a preferred embodiment, described hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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 is characterized in that: comprise the product that can be obtained by following chemical reaction: step 1, mass ratio is provided is 1: 0.001～1: 0.05 hexafluorophosphoric acid salt ionic liquid and alcamine compound; Step 2, add alcamine compound and stirring and dissolving in the described hexafluorophosphoric acid salt ionic liquid.
In a preferred embodiment, described alcamine compound is monoethanolamine or Propanolamine.
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 hexafluorophosphoric acid salt ionic liquid and alcamine compound; Step 2, add alcamine compound and stirring and dissolving in the described hexafluorophosphoric acid salt ionic liquid.
In a preferred embodiment, described alcamine compound is monoethanolamine or Propanolamine.
In a preferred embodiment, described hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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.
Above-mentioned electrolyte, by adding alcamine compound, alcamine compound can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis in the electrochemistry cyclic process and pyrolysis, thus the stability of using this ionic liquid to do the double layer capacitor of electrolyte can greatly be improved.
[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 provided by the invention and compound method thereof are described in further details.
The electrolyte of one execution mode comprises hexafluorophosphoric acid salt ionic liquid and is dissolved in alcamine compound in the hexafluorophosphoric acid salt ionic liquid that the mass ratio of hexafluorophosphoric acid salt ionic liquid and alcamine compound is 1: 0.001～1: 0.05.
Hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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.
Alcamine compound is preferably monoethanolamine or Propanolamine.Alcamine compound is appreciated that alcamine compound is not limited to monoethanolamine or Propanolamine, as long as can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis and pyrolysis get final product in the electrochemistry cyclic process.
The mass ratio of ionic liquid and alcamine compound is preferably 1: 0.03～and 1: 0.05.
Above-mentioned electrolyte, by adding alcamine compound, alcamine compound can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis in the electrochemistry cyclic process and pyrolysis, thus the stability of using this ionic liquid to do the double layer capacitor of electrolyte can greatly be improved; And the interpolation of alcamine compound 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 hexafluorophosphoric acid salt ionic liquid and alcamine compound.
Hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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.
Alcamine compound is monoethanolamine or Propanolamine.Alcamine compound is appreciated that alcamine compound is not limited to monoethanolamine or Propanolamine, as long as can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis and pyrolysis get final product in the electrochemistry cyclic process.
The mass ratio of ionic liquid and alcamine compound is preferably 1: 0.03～and 1: 0.05.
Step 2, add alcamine compound and stirring and dissolving in the described hexafluorophosphoric acid salt ionic liquid.
Above-mentioned electrolyte, by adding alcamine compound, alcamine compound can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis in the electrochemistry cyclic process and pyrolysis, thus the stability of using this ionic liquid to do the double layer capacitor of electrolyte can greatly be improved; And the interpolation of alcamine compound 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 hexafluorophosphoric acid salt ionic liquid and alcamine compound.
Hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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.
Alcamine compound is monoethanolamine or Propanolamine.Alcamine compound is appreciated that alcamine compound is not limited to monoethanolamine or Propanolamine, as long as can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis and pyrolysis get final product in the electrochemistry cyclic process.
The mass ratio of ionic liquid and alcamine compound is preferably 1: 0.03～and 1: 0.05.
Step 2, add alcamine compound and stirring and dissolving in the hexafluorophosphoric acid salt ionic liquid.
The compound method of above-mentioned electrolyte, by adding alcamine compound, alcamine compound can suppress the PF in the hexafluoro phosphonates ionic liquid
6 -Hydrolysis in the electrochemistry cyclic process and pyrolysis, thus the stability of using this ionic liquid to do the double layer capacitor of electrolyte can greatly be improved; While the interpolation of alcamine compound can increase the stability of the double layer capacitor that uses this electrolyte, reduce cost.
Below be the embodiment part:
Embodiment one
Alcamine compound is added in the hexafluoro phosphonates ionic liquid, be stirred to dissolving and can obtain electrolyte.
In the present embodiment, alcamine compound is monoethanolamine, and hexafluoro phosphonates ionic liquid is 1-butyl-3-methylimidazole hexafluoro phosphonate, and the mass ratio of hexafluoro phosphonates ionic liquid and alcamine compound is 1: 0.05.
In the present embodiment, preparation is carried out in glove box during electrolyte, monoethanolamine is added to stir in 1-butyl-3-methylimidazole hexafluoro phosphonate monoethanolamine is dissolved in 1-butyl-3-methylimidazole hexafluoro phosphonate.
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 0～2v 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 the hexafluoro phosphonates ionic liquid of monoethanolamine as the ratio capacitance of double layer capacitor under different cycle-indexes of electrolyte for the double layer capacitor that uses the electrolyte in the present embodiment from use.As can be seen from Figure 1, use the first charge-discharge of the double layer capacitor of the electrolyte that present embodiment provides to be 116.30F/g than electric capacity, the ratio electric capacity that circulates after 1000 times is 102.55F/g, and its conservation rate is 88.18%; And use the hexafluoro phosphonates ionic liquid that do not add monoethanolamine to be 116.62F/g as the first charge-discharge of the double layer capacitor of electrolyte than electric capacity, and the ratio electric capacity that circulates after 1000 times is 81.73F/g, its conservation rate is 70.13%; Use present embodiment electrolyte double layer capacitor than electric capacity conservation rate than the use that records under the equal conditions do not add the 1-butyl of monoethanolamine-3-methylimidazole hexafluoro phosphonate as the double layer capacitor of electrolyte improved 18.05% than electric capacity conservation rate, use the stability of double layer capacitor of the electrolyte of present embodiment to be greatly improved.
Embodiment two to 18
Among the embodiment two to 18, alcamine compound is added in the hexafluoro phosphonates ionic liquid, be stirred to dissolving and can obtain electrolyte.During preparation electrolyte, in glove box, carry out.
Among the embodiment two to 18, seeing table than electric capacity conservation rate and the ratio that improves than electric capacity conservation rate after proportioning, mixing time, the circulation of alcamine compound, hexafluoro phosphonates ionic liquid, hexafluoro phosphonates ionic liquid and alcamine compound 1000 times.
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 alcamine compound 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 hexafluoro phosphonates 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 hexafluorophosphoric acid salt ionic liquid and be dissolved in alcamine compound in the described hexafluorophosphoric acid salt ionic liquid, the mass ratio of described hexafluorophosphoric acid salt ionic liquid and described alcamine compound is 1: 0.001～1: 0.05.
2. electrolyte as claimed in claim 1, it is characterized in that: described alcamine compound is monoethanolamine or Propanolamine.
3. electrolyte as claimed in claim 1 is characterized in that: described hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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. electrolyte is characterized in that: comprise the product that can be obtained by following chemical reaction:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 hexafluorophosphoric acid salt ionic liquid and alcamine compound;
Step 2, add alcamine compound and stirring and dissolving in the described hexafluorophosphoric acid salt ionic liquid.
6. electrolyte as claimed in claim 5, it is characterized in that: described alcamine compound is monoethanolamine or Propanolamine.
7. the compound method of an electrolyte may further comprise the steps:
Step 1, mass ratio is provided is 1: 0.001～1: 0.05 hexafluorophosphoric acid salt ionic liquid and alcamine compound;
Step 2, add alcamine compound and stirring and dissolving in the described hexafluorophosphoric acid salt ionic liquid.
8. the compound method of electrolyte as claimed in claim 7, it is characterized in that: described alcamine compound is monoethanolamine or Propanolamine.
9. the compound method of electrolyte as claimed in claim 7 is characterized in that: described hexafluoro phosphonates ionic liquid by hexafluoro phosphonate 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 9, 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, and described pyrroles's salt cationoid is butyl methyl pyrroles cation, propyl group methylpyrrole cation or ethyl-methyl pyrroles cation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302444A (en) * | 1999-03-23 | 2001-07-04 | 日清纺织株式会社 | Electrolyte composition for electric double layer capacitor, solid polymer electrolyte, composition for polarizable electrode, polarizable electrode |
| CN1343024A (en) * | 2000-09-07 | 2002-04-03 | 默克专利股份有限公司 | Organic amine used as additive in electrochemical battery |
| CN1507669A (en) * | 2001-05-10 | 2004-06-23 | �����֯��ʽ���� | Nonaqueous electrolytic solution, composition for polymer gel electrolyte, polymer gel electrolyte, secondary cell, and electric double-layer capacitor |
| CN101777668A (en) * | 2010-02-05 | 2010-07-14 | 九江天赐高新材料有限公司 | Electrolyte for lithium manganese battery |
-
2011
- 2011-08-18 CN CN2011102379216A patent/CN102956369A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302444A (en) * | 1999-03-23 | 2001-07-04 | 日清纺织株式会社 | Electrolyte composition for electric double layer capacitor, solid polymer electrolyte, composition for polarizable electrode, polarizable electrode |
| CN1343024A (en) * | 2000-09-07 | 2002-04-03 | 默克专利股份有限公司 | Organic amine used as additive in electrochemical battery |
| CN1507669A (en) * | 2001-05-10 | 2004-06-23 | �����֯��ʽ���� | Nonaqueous electrolytic solution, composition for polymer gel electrolyte, polymer gel electrolyte, secondary cell, and electric double-layer capacitor |
| CN101777668A (en) * | 2010-02-05 | 2010-07-14 | 九江天赐高新材料有限公司 | Electrolyte for lithium manganese battery |
Non-Patent Citations (2)
| Title |
|---|
| 左晓希等: "乙醇胺作为电解液添加剂的研究", 《电池》, vol. 35, no. 5, 31 October 2005 (2005-10-31), pages 366 - 367 * |
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Application publication date: 20130306 |