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Pyrrole ionic liquid, and preparation method and application thereof

A technology of ionic liquid and pyrrole, which is applied in the preparation of sulfonic acid amide, the manufacture of hybrid/electric double layer capacitors, electrolytic capacitors, etc., can solve the problems of rising melting point, reducing the stability of ionic liquids, and narrowing the electrochemical window, etc., to achieve The effect of high decomposition voltage, good thermal stability and wide electrochemical window

Active Publication Date: 2014-06-04
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ionic liquid prepared by the two-step method will inevitably introduce halogen elements, and these halogen impurity ions will lead to the disadvantages of reduced stability of the ionic liquid, increased melting point and narrowed electrochemical window.

Method used

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  • Pyrrole ionic liquid, and preparation method and application thereof
  • Pyrrole ionic liquid, and preparation method and application thereof
  • Pyrrole ionic liquid, and preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0038] A preparation method of the above-mentioned pyrrole-based ionic liquid, the preparation process is as follows:

[0039]

[0040] Where MY is N-methyl-bis(trifluoromethanesulfonyl)amine or N-methyl-bis(fluorosulfonyl)amine; R is an alkyl group with 2 to 6 carbon atoms, Y - for (CF 3 SO 2 ) 2 N - or (FSO 2 ) 2 N - .

[0041] Specifically include the following steps:

[0042] Step S1: under the protection of an inert atmosphere, add the pyrrole derivative of the alkyl group and the methylating agent MY in an organic solvent in a molar ratio of 1:1 to 1.2:1, and the ratio of the organic solvent and the pyrrole derivative of the alkyl group is The mass ratio is 0.8:1-1.4:1, and the reaction is stirred and reacted at a temperature of 60°C-80°C for 3 hours-15 hours.

[0043] Wherein, the alkyl group of the pyrrole derivative of the alkyl group is ethylpyrrole, propylpyrrole, butylpyrrole, pentylpyrrole or hexylpyrrole.

[0044] Wherein, the methylating agent MY is...

Embodiment 1

[0068] In a 500mL flask, add 146g chloroform, (104.5g, 1.1mol) ethylpyrrole, (295g, 1.0mol) N-methyl-bis(trifluoromethanesulfonyl)amide, under nitrogen atmosphere, heat up to 70 °C, stirred for 10 hours. Stand to cool, carry out vacuum distillation at a temperature of 130°C and a pressure of 2.5Pa to remove excess reactants, collect the colorless liquid and wash it three times with 50ml of ethyl acetate, then at a temperature of 80°C, vacuum Vacuum drying was carried out under the condition of 0.01 MPa to obtain a colorless liquid 1-ethyl-1-methylpyrrole bis(trifluoromethanesulfonyl)imide salt with a yield of 92%.

[0069] Its hydrogen spectrum data are as follows:

[0070] 1 H NMR (CDCl 3 , 400MHz, ppm): 6.71(d, 2H), 6.45(t, 2H), 3.57(m, 2H), 3.24(s, 3H), 1.52(t, 3H).

[0071] in N 2 (or Ar 2 ) under the protection of atmosphere, take out 10g of 1-ethyl-1-methylpyrrole bis(trifluoromethanesulfonyl)imide salt, then add 30g of acetonitrile therein, and stir and mix it uni...

Embodiment 2

[0073] Add 120g of dichloromethane, (109g, 1.0mol) propylpyrrole, (195g, 1.0mol) N-methyl-bis(fluorosulfonyl)amine into a 500mL flask, and heat up to 60°C under a nitrogen atmosphere , stirred for 3 hours. Stand to cool, carry out vacuum distillation at a temperature of 120°C and a pressure of 1.2Pa to remove excess reactants, collect the colorless liquid and wash it three times with 50ml of ethyl acetate, then at a temperature of 80°C, vacuum Vacuum drying was carried out under the condition of 0.01 MPa to obtain a colorless liquid 1-propyl-1-methylpyrrole bis(fluorosulfonyl)imide salt with a yield of 93%.

[0074] Its hydrogen spectrum data are as follows:

[0075] 1 H NMR (CDCl 3 , 400MHz, ppm): 6.72(d, 2H), 6.47(t, 2H), 3.57(t, 2H), 3.25(s, 3H), 1.52(m, 2H), 0.87(s, 3H).

[0076] in N 2 (or Ar 2 ) under the protection of atmosphere, take out 10g-propyl-1-methylpyrrole bis(fluorosulfonyl)imide salt, then add 50g propylene carbonate therein, and stir and mix it evenly,...

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Abstract

The invention relates to a pyrrole ionic liquid. The chemical structural formula of the ionic liquid is shown as the specification, wherein R is alkyl of C2-C6; Y<-> is (CF3SO2)2N<-> or (FSO2)2N<->. The pyrrole ionic liquid is completely formed by ions at room temperature or under a situation close to the room temperature, has the advantages of high electrical conductivity, low melting point, wide electrochemical window, no volatilization or inflammability, good thermal stability and no halogen impurities or toxicity, and can be applied to the field of preparation of supercapacitors or lithium ionic batteries with high specific capacity. Furthermore, the invention also relates to a preparation method and application of the pyrrole ionic liquid.

Description

【Technical field】 [0001] The invention relates to the field of capacitor electrolyte, in particular to a pyrrole-based ionic liquid and a preparation method thereof, and also relates to an electrolyte using the pyrrole-based ionic liquid, a preparation method thereof, and a supercapacitor. 【Background technique】 [0002] Supercapacitor is a new type of energy device between rechargeable batteries and capacitors. It has the advantages of small size, large capacity, fast charging speed, long cycle life, high discharge efficiency, wide operating temperature range, good reliability, pollution-free and maintenance-free It is a new type, efficient and practical energy storage device, so it is widely used in military fields, mobile communication devices, computers, and hybrid power sources for electric vehicles. The energy stored in a supercapacitor is proportional to the square of the applied voltage, therefore, increasing the applied voltage can greatly increase the specific ener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/323C07C311/48C07C303/40H01G9/035
CPCC07D207/323H01G11/62H01G11/84Y02E60/13
Inventor 周明杰刘大喜袁新生王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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