Cyclic quaternary ammonium salt electrolyte, preparation method and application therefor

A quaternary ammonium salt and electrolyte technology, which is used in the manufacture of hybrid capacitor electrolytes and hybrid/electric double layer capacitors, etc., can solve the problems of small processing capacity of chromatography columns, inability to reuse solvents, and low efficiency, and achieve a simple and easy purification method. line, low cost and high efficiency

Active Publication Date: 2016-03-30
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The chromatographic column has a small processing capacity, is easily saturated, and requires frequent replacement or activation treatment, which consumes a large amount of solvent and energy. Therefore, the use of chromatographic columns for purification has the problems of low efficiency and high cost
However, the solvent purified by the ion exchange method cannot be reused, and there is also a problem of high cost.

Method used

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  • Cyclic quaternary ammonium salt electrolyte, preparation method and application therefor
  • Cyclic quaternary ammonium salt electrolyte, preparation method and application therefor
  • Cyclic quaternary ammonium salt electrolyte, preparation method and application therefor

Examples

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Effect test

Embodiment 1

[0037] 1: Preparation of N,N-dimethylpyrrolidinium tetrafluoroborate

[0038] (1), first add 200g of sodium hydroxide to 1333g of high-purity water to prepare a 13% sodium hydroxide aqueous solution, and inhale in a 5L stainless steel high-pressure reactor, then inhale 630g of 1,4 dichlorobutane under stirring , and finally 236.5 g of dimethylamine was introduced; the reaction solution was stirred for 30 minutes until it was uniform, and the electric heating was turned on to raise the temperature to 90°C for 10 hours of reaction.

[0039] (2) The above synthesis reaction solution was vacuum dehydrated on a rotary evaporator at 110°C to a powder solid mixture of 968g;

[0040] (3) Add 968 g of absolute ethanol to the above solid mixture, stir for 60 minutes, and then filter to obtain 1600 g of an ethanol solution of N,N-dimethylpyrrolidinium chloride salt;

[0041] (4) Add 525 g of ammonium tetrafluoroborate to the above-mentioned ethanol solution of N,N-dimethylpyrrolidinium ...

Embodiment 2

[0052] 1: Preparation of N-ethyl-N-methylpyrrolidinium tetrafluoroborate

[0053] (1), first add 280g of potassium hydroxide to 2154g of high-purity water to prepare a concentration of 11.5% potassium hydroxide aqueous solution, and inhale in a 5L stainless steel autoclave, then inhale 1,4 dibromobutane 1070g under stirring , and finally 310g of N-ethylmethylamine was introduced; the reaction solution was stirred for 30 minutes until uniform, and the electric heating was turned on to raise the temperature to 80°C for 8 hours. During the reaction, the pressure was controlled at 0.1MPa~1.0MPa; Liquid 3800g;

[0054] (2) The above synthesis reaction solution was vacuum dehydrated on a rotary evaporator at 110° C. to 1335 g of a powder solid mixture;

[0055] (3), add 1335g of anhydrous acetonitrile to the above solid mixture, after stirring for 60min, filter to obtain 2300g of acetonitrile solution of N-ethyl-N-methylpyrrolidinium bromide;

[0056] (4) Add 525 g of ammonium tet...

Embodiment 3

[0067] 1: Preparation of N-propyl-N-methylpiperidinium tetrafluoroborate

[0068] (1), first adding 345g of salt of wormwood to 1916g of high-purity water and being mixed with the potassium carbonate aqueous solution of 15% concentration, and inhaling in the 5L stainless steel autoclave, then inhaling 1,5 dichloropentane 700g under the state of stirring, finally Pass in 383g of N-methyl n-propylamine; stir the reaction solution for 30min until uniform, turn on the electric heating and raise the temperature to 100°C for 8 hours, and control the pressure at 0.1MPa~1.0MPa during the reaction process; release 3200g of synthetic reaction solution after returning to normal temperature;

[0069] (2) The above synthetic reaction solution was vacuum dehydrated on a rotary evaporator at 110°C to 1257g of a powder solid mixture;

[0070] (3), add 1257g of anhydrous ethyl acetate to the above solid mixture, after stirring for 60min, filter to obtain 2300g of ethyl acetate solution of N-pr...

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Abstract

The invention relates to a cyclic quaternary ammonium salt electrolyte, a preparation method and an application therefor. The preparation method comprises the steps of enabling an inorganic aqueous alkali, organic secondary amine and alkyl dihalide to react to obtain halogenated cyclic quaternary ammonium salt reacting liquid; dehydrating the halogenated cyclic quaternary ammonium salt reacting liquid to obtain a solid powder mixture; dissolving the solid powder mixture into anhydrous organic solvent, and filtering to obtain an organic solution of the halogenated cyclic quaternary ammonium salt; adding ammonium salt of high purity acid into the organic solution of the halogenated cyclic quaternary ammonium salt, performing a backflow reaction, and then performing filtering, recrystallization, filtering, and vacuum drying to obtain the cyclic quaternary ammonium salt electrolyte. The preparation method is low in cost of the raw materials, and high in cyclization selectivity; the purifying method is simple and easy to implement, high in efficiency and low in cost; in addition, the preparation method has low requirement on equipment, and the industrial production of the cyclic quaternary ammonium salt electrolyte can be achieved easily; and in addition, the prepared cyclic quaternary ammonium salt electrolyte is low in content of halogen, the purity can reach more than 99%, and the yield can reach more than 90%.

Description

technical field [0001] The invention specifically relates to a cyclic quaternary ammonium salt electrolyte, its preparation method and application. Background technique [0002] Supercapacitor is a new type of green and environmentally friendly physical energy storage device between traditional capacitors and batteries that has emerged with the breakthrough of material science in recent years. It is the most promising technical device in physical energy storage. A good complement to other electrochemical energy storage technologies. Its biggest advantage is that it can output high power in a short time, the power density is much higher than that of lithium batteries, the number of charge and discharge cycles can reach more than 500,000 times, the life span can reach more than 10 years, the charging time is short, and it can charge and discharge with high current. Widely used in new energy vehicles, new energy power generation, construction machinery, rail transit, lifting e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/84H01G11/62
CPCY02E60/13H01G11/84H01G11/62
Inventor 邹凯何永刚熊鲲任齐都蒋桥龙李建中
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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