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Preparation method of spiro-quaternary ammonium salt electrolyte

A technology of spirocyclic quaternary ammonium salts and electrolytes, which is applied in hybrid capacitor electrolytes, organic chemistry, etc., can solve the problems of difficulty in meeting the requirements of electrochemical products, large residual halogen ions, and low synthesis yields, and achieve product yields High, high purity, good selectivity

Active Publication Date: 2015-03-04
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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Problems solved by technology

In this case, in order to improve its low-temperature performance, electrical conductivity and capacity, it is known to use spirocyclic quaternary ammonium salt as a new type of electrolyte for electrolyte, in patent documents (CN201010594705, CN201210475201, CN200680040555, US6469888 ) describes the nucleophilic substitution reaction between a cyclic amine and a dihalogenated hydrocarbon, first synthesizing the corresponding halogenated salt or diol disulfonic acid ester, and then preparing the synthetic process of the spirocyclic quaternary ammonium salt by ion exchange. This method synthesizes The yield is low, and there are halogen ions in the preparation process, and the residual amount of halogen ions in the recrystallization process is large, which seriously affects its use in electrochemical energy storage components, and it is difficult to meet the requirements of electrochemical products

Method used

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  • Preparation method of spiro-quaternary ammonium salt electrolyte
  • Preparation method of spiro-quaternary ammonium salt electrolyte
  • Preparation method of spiro-quaternary ammonium salt electrolyte

Examples

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Embodiment 1

[0030] Embodiment 1: Preparation of tetrafluoroborate spiro 1,1'-bispyrrole quaternary ammonium salt

[0031] In a 2L tetrafluoro autoclave, add inert solvent acetonitrile (328g, 8mol), tetrahydropyrrole (71g, 1mol), 1,4 butanediol (75g, 0.83mol), composite catalyst (0.046 g deoxidation type palladium catalyst; 1.375g styrene series strongly acidic cation exchange resin), then slowly add 45% concentration of tetrafluoroboric acid aqueous solution (179g, containing tetrafluoroboric acid 81g), be warming up to 150 ℃ of reaction 8 hours. The above reaction solution was lowered to room temperature, filtered under reduced pressure, and concentrated to a semi-solid state under vacuum at 120°C. After the concentrated solution was cooled to 60°C, an appropriate amount of ethanol was added to produce a large amount of white crystals, and the crude product of spiro 1,1'-bispyrrole quaternary ammonium tetrafluoroborate was obtained by filtration, which was then recrystallized and dried w...

Embodiment 2

[0036] Embodiment 2: Preparation of spiropyrrole-1,1'-piperidine quaternary ammonium tetrafluoroborate

[0037] In a 2L tetrafluoro autoclave, add inert solvent acetonitrile (328g, 8mol), hexahydropyridine (85g, 1mol), 1,4 butanediol (75g, 0.83mol), composite catalyst (0.055 g deoxidation type palladium catalyst; 1.65g styrene series strongly acidic cation exchange resin), then slowly add 45% concentration of tetrafluoroboric acid aqueous solution (179g, containing tetrafluoroboric acid 81g), be warming up to 150 ℃ of reaction 8 hours. The above reaction solution was lowered to room temperature, filtered under reduced pressure, and concentrated to a semi-solid state under vacuum at 120°C. After the concentrated solution was cooled to 60°C, an appropriate amount of ethanol was added to produce a large amount of white crystals, and the crude product of spiropyrrole-1,1'-piperidine quaternary ammonium tetrafluoroborate was obtained by filtration, and then recrystallized and dried...

Embodiment 3

[0041] Embodiment 3: Preparation of tetrafluoroborate spiro 1,1'-bispiperidine quaternary ammonium salt

[0042] In the 2L tetrafluoro autoclave, add inert solvent acetonitrile (328g, 8mol) successively under stirring state, hexahydropyridine (85g, 1mol), 1,5 pentanediols (86.5g, 0.83mol), composite catalyst ( 0.055g deoxidation type palladium catalyst; 1.65g styrene series strongly acidic cation exchange resin), then slowly add 45% concentration of tetrafluoroboric acid aqueous solution (179g, containing tetrafluoroboric acid 81g), be warming up to 155 ℃ and react for 8 hours. The above reaction solution was lowered to room temperature, filtered under reduced pressure, and concentrated to a semi-solid state under vacuum at 120°C. After the concentrated solution was cooled to 60°C, an appropriate amount of ethanol was added to produce a large amount of white crystals, and the crude product of spiro 1,1'-bispiperidine quaternary ammonium tetrafluoroborate was obtained by filtra...

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Abstract

The invention relates to a preparation method of a spiro-quaternary ammonium salt electrolyte. The preparation method is characterized by subjecting a cyclic amine, diol and a strong acid to condensation reaction at 120-180 DEG C for 8-16 hours in a polar organic solvent in the presence of a catalyst, and then purifying the reactant, thus obtaining the spiro-quaternary ammonium salt electrolyte, wherein the cyclic amine is any one of pyrrolidone, piperidine and morpholine; diol is 1,4-butanediol or 1,5-pentanediol; the strong acid is any one of tetrafluoroboric acid, trifluoromethanesulfonic acid and bis(trifluoromethanesulfonyl)imidic acid; the feed mole ratio of the cyclic amine to diol to the strong acid is 1 to (0.7-0.9) to (0.8-1). The preparation method has the advantages that the raw materials are cheap; the whole synthetic reaction is good in selectivity; the product has high yield and high purity; no halide ions are introduced in the reaction process, and the content of halogen in the obtained target product is less than 1ppm, so that the preparation method can meet the requirements of electrochemical energy storage electrolytes and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of a spirocyclic quaternary ammonium salt electrolyte. Background technique [0002] Because electrochemical energy storage devices, especially supercapacitors, have excellent pulse charge-discharge performance and large-capacity energy storage performance that traditional physical capacitors do not have, their applications in high-energy pulsed lasers have attracted widespread attention. At the same time, it is used as a backup power supply for computer systems and wireless communication equipment because of its large storage energy, light weight, and multiple charge and discharge. With the rise of research on environmentally friendly electric vehicles, electrochemical capacitors are used in conjunction with lead-acid batteries and other batteries to form composite batteries, which are used in the power starting system of electric vehicles to pr...

Claims

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Application Information

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IPC IPC(8): C07D487/10C07D498/10C07D471/10H01G11/62
CPCY02E60/13C07D487/10C07D471/10C07D498/10H01G11/62
Inventor 邹凯何永刚熊鲲施苏萍闻立新郭军关士友李建中
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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