Preparation method of high-purity alkylammonium tetrafluoroborate for super capacitor

A technology of supercapacitor and tetrafluoroboric acid, which is applied in capacitors, electrolytic capacitors, chemical instruments and methods, etc., to achieve the effects of high conversion rate, small internal resistance and high yield

Active Publication Date: 2012-05-02
锦州凯美能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method fails to avoid the introduction of halide ions from the source of raw materials

Method used

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  • Preparation method of high-purity alkylammonium tetrafluoroborate for super capacitor
  • Preparation method of high-purity alkylammonium tetrafluoroborate for super capacitor
  • Preparation method of high-purity alkylammonium tetrafluoroborate for super capacitor

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Experimental program
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Effect test

Embodiment 1

[0036] Preparation of triethylmethylammonium tetrafluoroborate

[0037] Under a nitrogen atmosphere, triethoxonium tetrafluoroborate (47.5 g, 0.25 mol) was added to a solution containing N,N-diethyl-N-methylamine (26.1 g, 0.3 mol) and 150 ml of dichloro methane in a 500 ml reaction flask and stirred at room temperature for 15 hours. After filtration, the filtrate was concentrated to obtain the crude product of triethylmethylammonium tetrafluoroborate. Dissolve in ethanol, add activated carbon, heat to reflux for 30 minutes, filter, and cool the filtrate to obtain 46.6 g of white crystals of triethylmethylammonium tetrafluoroborate, with a yield of 92%.

[0038] Detected by ion chromatography: Na: 2.1ppm, K: 3.5ppm, Fe: 1.6ppm, Mg: 1.0ppm, Ca: 2.5ppm, no halogen ions.

Embodiment 2

[0040] Preparation of triethylmethylammonium tetrafluoroborate

[0041] Under a nitrogen atmosphere, trimethoxonium tetrafluoroborate (29.6 g, 0.2 mol) was added to a solution containing N,N-diethyl-N-methylamine (20.9 g, 0.24 mol) and 150 ml of dichloromethane In a 250 ml reaction flask, react at 40°C for 8 hours. After filtration, the filtrate was concentrated to obtain the crude product of triethylmethylammonium tetrafluoroborate. Dissolve in methanol, add activated carbon, heat to reflux for 30 minutes, filter, and cool the filtrate to obtain 38.2 g of white crystals of triethylmethylammonium tetrafluoroborate, with a yield of 94%.

[0042] Detected by ion chromatography: Na: 2.2ppm, K: 2.6ppm, Fe: 1.6ppm, Mg: 1.6ppm, Ca: 2.4ppm, no halide ions were seen.

Embodiment 3

[0044] Preparation of Tetraethylammonium Tetrafluoroborate

[0045] Under a nitrogen atmosphere, triethoxonium tetrafluoroborate (47.5 g, 0.25 mol) was added to a 500 mL reaction flask containing triethylamine (28.3 g, 0.28 mol) and 200 mL of chloroform, 60 °C for 10 hours. Filtration, the filtrate was concentrated to obtain the crude product of tetraethylammonium tetrafluoroborate, dissolved in methanol, added activated carbon, heated to reflux for 30 minutes, filtered, and the filtrate was cooled to obtain 47.7 grams of white crystals of tetraethylammonium tetrafluoroborate. The yield was 88%.

[0046] Detected by ion chromatography: Na: 1.8ppm, K: 2.8ppm, Fe: 1.5ppm, Mg: 2.4ppm, Ca: 3.2ppm, no halogen ions.

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Abstract

The invention discloses a preparation method of high-purity alkylammonium tetrafluoroborate for a super capacitor, characterized by reacting tertiary amine with tetrafluoroborate alcoxylonium salt at a certain temperature to obtain corresponding alkylammonium tetrafluoroborate, and purifying to obtain the high-purity alkylammonium tetrafluoroborate. The method has the advantages of simple operation steps, good selectivity, high conversion rate, high product purity, and no halogen ions, and can satisfy the requirements of a high performance super capacitor. The use of the prepared alkylammonium tetrafluoroborate as an electrolyte in the super capacitor can achieve the advantages of high product capacity, low internal resistance, and reduced capacity fade at a high temperature.

Description

technical field [0001] The invention belongs to the field of synthesis methods of organic electrolytes for supercapacitors, and in particular relates to a method for preparing high-purity quaternary ammonium tetrafluoroborate. Background technique [0002] Supercapacitor (electric double layer capacitor) is a high-energy electric energy storage element developed in recent years. It has the advantages of high power density, high cycle life, fast charging and discharging, and no pollution to the environment. It is widely used in motor regulators Clean energy systems such as sensors, backup power supplies for microcomputer memory, starting devices for motor vehicles, wind power generation and solar power generation systems have attracted attention. Quaternary ammonium salts, as non-aqueous electrolytes for supercapacitors, can be used as supporting electrolytes for chemical batteries for energy storage devices or high-energy capacitors. [0003] As a high-purity tetrafluorobor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/20C07C217/08C07C213/00C07D207/04C07D233/58C07D233/60C07D295/037H01G9/035
CPCY02E60/13
Inventor 王道林金振兴
Owner 锦州凯美能源有限公司
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