A kind of preparation method of tetrafluoroborate spirocyclic ammonium salt

A tetrafluoroborate spiro and spiro quaternary ammonium salt technology, applied in the direction of organic chemistry, can solve the problems of accelerating the capacity decay of supercapacitors, affecting, reducing the initial capacity and cycle life of supercapacitors, and achieving mild reaction conditions and energy consumption. low effect

Active Publication Date: 2018-09-14
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

The existence of impurity ions and free acids is the main cause of self-discharge; at the same time, moisture not only affects self-discharge, but also accelerates the capacity decay of supercapacitors
Therefore, the presence of impurity ions, free acids, and moisture greatly reduces the initial capacity and cycle life of supercapacitors

Method used

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  • A kind of preparation method of tetrafluoroborate spirocyclic ammonium salt

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Experimental program
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Effect test

Embodiment 1

[0028] In the 2000mL reaction kettle 1, 1000mL of acetonitrile solvent, 194.3g of potassium carbonate, 16.8g of potassium bromide were sequentially added under stirring, and 100.0g of tetrahydropyrrole and 178.6g of 1,4-dichlorobutane were slowly added in sequence under nitrogen protection , stirred and refluxed at 85°C for 12h, cooled and filtered to obtain a chlorinated spirocyclic quaternary ammonium salt solution. Add 265.5g of potassium tetrafluoroborate to the chlorospiroquaternary ammonium salt solution, stir at 25°C for 12 hours for ion exchange, filter, add 5.0g of potassium carbonate to the mother liquor, stir, filter, and distill under reduced pressure to obtain spiroquaternary tetrafluoroborate Crude salt. The crude spirocyclic ammonium salt of tetrafluoroborate was extracted three times with ethyl acetate / water with a volume ratio of 1:1, and the water phase was collected; vacuum distillation, removal of water, heating and dissolving with ethanol, stirring at -5°C...

Embodiment 2

[0035]In a 2000mL reaction kettle 1, 1000mL of acetonitrile solvent, 291.5g of potassium carbonate, 22.7g of tetrabutylammonium bromide were successively added under stirring, and 100.0g of tetrahydropyrrole and 214.2g of 1,4 -Dichlorobutane, stirred and refluxed at 80°C for 10h, cooled and filtered to obtain a chlorospirocyclic quaternary ammonium salt solution. Add 221.3g of potassium tetrafluoroborate to the chlorospiroquaternary ammonium salt solution, stir at 25°C for 12 hours for ion exchange, filter, add 3.0g of potassium carbonate to the mother liquor, stir, filter, and distill under reduced pressure to obtain spiroquaternary tetrafluoroborate Crude salt. The crude spirocyclic ammonium salt of tetrafluoroborate was extracted 3 times with ethyl acetate / water with a volume ratio of 1:1, and the water phase was collected; vacuum distillation, removal of water, heating and dissolving with ethanol, stirring at -10°C Recrystallization, the obtained solid was heated and diss...

Embodiment 3

[0038] In a 2000mL reaction kettle 1, 1000mL of acetonitrile solvent, 388.7g of potassium carbonate, 45.3g of tetrabutylammonium bromide were sequentially added under stirring, and 100.0g of tetrahydropyrrole and 214.2g of 1,4 -Dichlorobutane, stirred and refluxed at 75°C for 12h, cooled and filtered to obtain a chlorospirocyclic quaternary ammonium salt solution. Add 221.3g potassium tetrafluoroborate to the chlorospiroquaternary ammonium salt solution, stir at 20°C for 10h for ion exchange, filter, add 6.0g sodium carbonate to the mother liquor, stir, filter, and distill under reduced pressure to obtain spiroquaternary tetrafluoroborate Crude salt. The crude product of spirocyclic quaternary ammonium tetrafluoroborate was extracted three times with ethyl acetate / water at a volume ratio of 1:1, and the aqueous phase was collected; distilled under reduced pressure to remove water, dissolved by heating with ethanol, and stirred again at 0°C. Crystallization, the obtained solid...

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Abstract

The invention discloses a preparation method of spiro quaternary ammonium tetrafluoroborate. The method comprises steps as follows: (1) an acetonitrile solvent, carbonate, a bromine catalyst, pyrrolidine and 1,4-dichlorobutane are added to a reaction kettle to have a reaction, and a chlorinated spiro quaternary ammonium salt solution is obtained; potassium tetrafluoroborate is added to an acetonitrile solution of chlorinated spiro quaternary ammonium salt, the mixture has a reaction and then is subjected to ion exchange and filtration, carbonate is added to a filtrate, the mixture is stirred, filtered and subjected to reduced-pressure distillation, and a crude spiro quaternary ammonium tetrafluoroborate product is obtained; (2) high-purity spiro quaternary ammonium tetrafluoroborate is obtained with a series of purification methods such as extraction, reduced-pressure distillation, recrystallization, drying and the like. The yield and the purity of spiro quaternary ammonium tetrafluoroborate prepared with the method are relatively high, the content of halide ions and water is low, and spiro quaternary ammonium tetrafluoroborate has the remarkable performance advantage when used as a supercapacitor electrolyte.

Description

technical field [0001] The invention relates to the field of preparation of supercapacitor electrolytes, in particular to a preparation method of tetrafluoroborate spirocyclic quaternary ammonium salt. technical background [0002] Due to the advantages of very high power density, long life and good high and low temperature performance, supercapacitors are regarded as a new energy storage device with great development prospects. They are used in hybrid vehicles, wind power generation, cranes, rail transit and other fields Has a wide range of applications. As an important part of the supercapacitor, the electrolyte is one of the key factors affecting the performance of the capacitor. There are mainly two types of aqueous electrolyte and non-aqueous electrolyte. Supercapacitors with aqueous electrolytes have low energy density, while supercapacitors with non-aqueous electrolytes have higher energy density, but have the disadvantage of low working voltage. Since supercapacito...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/10
CPCC07D487/10
Inventor 邹志群余意马姗仲淑彬何凤荣
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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