Preparation method of spiro quaternary ammonium tetrafluoroborate
A spiro-tetrafluoroborate and spiro-ring quaternary ammonium salt technology, which is applied in organic chemistry and other fields, can solve the problems of accelerating supercapacitor capacity attenuation, impact, and reducing the initial capacity and cycle life of supercapacitors, and achieves mild reaction conditions and low energy consumption. low effect
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Embodiment 1
[0028] In the 2000mL reaction kettle 1, 1000mL of acetonitrile solvent, 194.3g of potassium carbonate, 16.8g of potassium bromide were successively added under stirring, and under the protection of nitrogen, 100.0g of tetrahydropyrrole and 178.6g of 1,4-dichlorobutane were slowly added in sequence , stirred and refluxed at 85°C for 12h, cooled and filtered to obtain a chlorinated spirocyclic quaternary ammonium salt solution. Add 265.5g potassium tetrafluoroborate to the chlorospiroquaternary ammonium salt solution, stir at 25°C for 12 hours for ion exchange, filter, add 5.0g 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 aqueous phase was collected; vacuum distillation, removal of water, heating and dissolving with ethanol, and stirring at ...
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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