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A kind of preparation method of tetrafluoroborate spirocyclic ammonium salt

A technology of spiro tetrafluoroborate and fluoroborate, applied in organic chemistry and other directions, can solve problems such as unreported purification methods, affecting electrolyte performance, etc., and achieve the effects of convenient recycling and application, improving quality and performance, and reducing three wastes.

Active Publication Date: 2017-06-06
QUZHOU CHEMSPEC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the above-mentioned patent, this method has obvious progress, less waste water, simple reaction, but no purification method is reported, even the electrolyte obtained by filtration is a mixture, containing metal ions and unreacted raw and auxiliary materials, which will greatly affect the performance of the electrolyte

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  • A kind of preparation method of tetrafluoroborate spirocyclic ammonium salt
  • A kind of preparation method of tetrafluoroborate spirocyclic ammonium salt
  • A kind of preparation method of tetrafluoroborate spirocyclic ammonium salt

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[0038] The present invention provides a kind of preparation method of tetrafluoroboric acid spirocyclic quaternary ammonium salt, comprising the following steps:

[0039] 1) Put the alkali, fluoroborate, dihaloalkane, and cyclic amine in the reaction solvent, react at 50-90°C, cool down and filter after the reaction is completed, and remove the solvent from the filtrate;

[0040] In the preparation method of the spirocyclic quaternary ammonium tetrafluoroborate provided by the present invention, the base is preferably an inorganic base, more preferably one of lithium carbonate, sodium carbonate, potassium carbonate, lithium hydroxide, sodium hydroxide, and potassium hydroxide. one or more combinations. The molar ratio of cyclic amine to base is preferably 1:0.9 to 1:2, more preferably 1:1 to 1:1.1.

[0041] In the preparation method of the spirocyclic quaternary ammonium tetrafluoroborate provided by the present invention, the fluoroborate is preferably one or more combinatio...

Embodiment 1

[0062] Example 1: (tetrafluoroboric acid spiro-1,1-dipyrrolidinium salt)

[0063] In a 2000mL reactor, 500g of acetonitrile, 193.5g (1.4mol) of potassium carbonate, 146.8g (1.4mol) of ammonium fluoroborate, 177.8g (1.4mol) of 1,4-dichlorobutane, 100g (1.4mol) of ) Tetrahydropyrrole. Heat to 60-70°C and keep it warm for 50 hours. Cool down to room temperature, filter with suction, rinse the filter cake with 50 g of acetonitrile, and combine the filtrates to obtain an acetonitrile solution of the product. The filtrate was concentrated under reduced pressure, 600 g of ethanol and 1.0 g of 18-crown-6 were added for recrystallization, filtered, and vacuum-dried to obtain 229 g of the product. Melting point: 189.2 to 189.7. 1 H NMR (300MHz,D 2 O): δ=2.08~2.09(m,8H), 3.38~3.43(m,8H). 13 C NMR (75MHz, D 2 O): δ=21.67(CH 2 ),62.78(CH 2 ). 19 F NMR (376MHz, CDCl 3 ): δ=-151.95.

Embodiment 2

[0064] Example 2: (tetrafluoroborate spiro-1,1-dipyrrolidinium salt)

[0065] In a 2000mL reactor, 500g of acetonitrile, 193.5g (1.4mol) of potassium carbonate, 146.8g (1.4mol) of ammonium fluoroborate, 177.8g (1.4mol) of 1,4-dichlorobutane, 100g (1.4mol) of ) Tetrahydropyrrole. Heat to 60-70°C and keep it warm for 50 hours. Cool down to room temperature, filter with suction, rinse the filter cake with 50 g of acetonitrile, and combine the filtrates to obtain an acetonitrile solution of the product. The filtrate was concentrated under reduced pressure, and 600 g of ethanol was added for recrystallization, filtered, and vacuum-dried to obtain 230 g of the product.

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Abstract

The invention relates to the field of preparation of electrolyte of a super-capacitor, and particularly relates to a preparation method and application of tetrafluoroboric acid volution quaternary ammonium salt. The preparation method of the tetrafluoroboric acid volution quaternary ammonium salt comprises the following steps of: (1) placing alkali, fluoroborate, alkyl dihalide and cyclamine into a reaction solvent, reacting at 50-90 DEG C; reducing temperature and filtering after the reaction is finished, and removing the solvent contained in filter liquor; (2) adding a recrystallization solvent and a metal ion remover to a product obtained from the step (1) for recrystallization to obtain a tetrafluoroboric acid volution quaternary ammonium salt product. The preparation method disclosed by the invention is easy to operate by adopting one-pot reaction without separating an intermediate, is less in three wastes by adopting a nonaqueous system and economical and practical by conveniently recovering and reusing the solvent and can be used for enhancing the quality and property of the tetrafluoroboric acid volution quaternary ammonium salt by removing the corresponding metal ion contained in a system by adopting crown ether during post-processing.

Description

technical field [0001] The invention relates to the field of preparation of supercapacitor electrolytes, in particular to a preparation method and application of tetrafluoroborate spirocyclic ammonium salt. Background technique [0002] Due to the characteristics of good power characteristics, long cycle life and less environmental pollution, supercapacitors have attracted extensive attention in recent years. Electrolyte, an important part of supercapacitors, is one of the key factors affecting the performance of capacitors. According to the different electrolytes used, supercapacitors can be divided into two types: aqueous electrolyte supercapacitors and non-aqueous electrolyte supercapacitors. Supercapacitors with aqueous electrolytes have low energy density, while supercapacitors with non-aqueous electrolytes have higher energy density. However, the performance of the non-aqueous electrolyte is limited by the decomposition voltage of the electrolyte. At present, the act...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/10
CPCC07D487/10
Inventor 何立杨东刘辉孙元健袁云龙彭勇焦海华胡向兵梁新章
Owner QUZHOU CHEMSPEC CORP