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Preparation method of high-purity conductive salt for super capacitor

A technology of quaternary ammonium salt cation and general formula, applied in the field of preparation of tetrafluoroborate alkyl quaternary ammonium salt, can solve the problems of easy agglomeration of dried products, reduced product yield, difficult removal of water, etc., and achieves low water content. , The effect of maintaining high yield and avoiding environmental pollution

Active Publication Date: 2011-03-23
岳阳凯门科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above-mentioned method fails to avoid the pollution of halogen anion from raw material source, and the yield of product also all reduces after removing halogen anion with recrystallization, and the moisture contained in the product is difficult to remove, and dry product is easy to agglomerate, and high-temperature drying will make Decomposition of quaternary ammonium salts

Method used

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  • Preparation method of high-purity conductive salt for super capacitor
  • Preparation method of high-purity conductive salt for super capacitor
  • Preparation method of high-purity conductive salt for super capacitor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: the synthesis of methyltriethylammonium tetrafluoroborate

[0028] In a 250mL stainless steel reaction kettle, add 38g (0.38mol) of triethylamine, 53g (0.59mol) of dimethyl carbonate, and 70mL of methanol in sequence, react at 130°C for 24 hours, cool to room temperature, open the reaction kettle, and collect the product solution , detected by gas chromatography, the conversion rate of triethylamine was 95%. After the collected product solution was evaporated under reduced pressure at 50° C. to remove the solvent, it was dried under reduced pressure at 50° C. and 133 Pa to obtain 65 g of solid (yield 90%). The reaction process of this step is shown in formula (9) .

[0029] In the 250mL three-neck round bottom flask, add 100mL methanol successively, the solid 38.3g (0.20mol) that last step obtains, ammonium fluoride (NH 4 F) 7.4g (0.20mol), install the reflux condenser, under continuous nitrogen flow, 50 ℃, under stirring condition, react for 10 hours, f...

Embodiment 2

[0035] Embodiment 2: comparative example

[0036] In a 250mL stainless steel reaction kettle, add 38g (0.38mol) of triethylamine, 53g (0.59mol) of dimethyl carbonate, and 70mL of methanol in sequence, react at 130°C for 24 hours, cool to room temperature, open the reaction kettle, and collect the product solution , detected by gas chromatography, the conversion rate of triethylamine was 95%. The collected product solution was evaporated to remove the solvent under reduced pressure at 50° C., and then dried under reduced pressure at 50° C. and 133 Pa pressure to obtain 65 g of solid (yield 90%).

[0037] In a 500mL PTFE round bottom flask, add 250mL of methanol solution containing 76.5g (0.4mol) of methyltriethylammonium-monomethyl carbonate, and slowly drop in 42% tetrafluoroboric acid at 0°C under electromagnetic stirring (HBF 4 ) aqueous solution 85mL, after the dropwise addition, continue at room temperature for 30min., stop stirring, and the pH of the solution is 6.0. A...

Embodiment 3

[0039] The final products obtained in Example 1 and Example 2 were compared in quality, and the results are shown in Table 1.

[0040] Table 1 The quality analysis results of methyltriethylammonium tetrafluoroborate obtained by different preparation methods

[0041]

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Abstract

The invention relates to a preparation method of quaternary alkylammonium salt tetrafluoroborate of which the structure is expressed by general formula (1), wherein QA+ represents quaternary ammonium salt positive ions. The preparation method is characterized in that monomethyl carbonic ester of which the structure is expressed by (QA+)(CH3OCO2-) reacts with ammonium fluoride, and then the mixture reacts with a complex compound formed by boron trifluoride and Louis basic organic solvent after being filtered, and the obtained solid product is dried and recrystallized, so as to obtain the quaternary alkylammonium salt tetrafluoroborate of which the structure is expressed by the general formula (1). In preparation method provided by the invention, the operation step is simple, the productivity is high, the purity of the products can reach more than 99.9 percent, the moisture of the products is low, the content of halogen negative ions is less than 5ppm, and no pollution of foreign ions such as BF3OH-, BF2(OH)2-, BF(OH)3- and the like generates. The quaternary alkylammonium salt tetrafluoroborate prepared by the method is used for preparing electrolyte, thus the obtained super capacitor has high capacity, low internal resistance and low capacity attenuation at high temperature. The formula (1) is shown in specification.

Description

technical field [0001] The invention relates to a preparation method of a conductive salt used for a supercapacitor, in particular to a preparation method of a high-purity tetrafluoroborated alkyl quaternary ammonium salt. Background technique [0002] Supercapacitors (Supercapacitors), also known as Electrochemical Capacitors, are a new type of energy storage device that combines the characteristics of traditional flat-panel capacitors and secondary lithium batteries. It can not only provide higher specific energy than ordinary flat-panel capacitors, It also has higher specific power and longer cycle life than secondary batteries. Therefore, supercapacitors are considered to be an efficient and practical new type of clean energy. At present, as a backup power supply, they have been widely used in electronic and electrical products such as cameras, video recorders, mobile phones, and computers. Moreover, with the society's demand for low-emission and zero-emission vehicles,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07D233/58C07D233/06C07D295/037C07D263/04
CPCC01B35/063C07C209/20H01G11/62Y02E60/13
Inventor 周志彬郑文钺杨朝辉张正波
Owner 岳阳凯门科技有限公司
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