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A kind of simple preparation method of tetraethylammonium tetrafluoroborate

A technology of tetraethylammonium tetrafluoroborate and tetraethylammonium chloride is applied in the preparation of amino compounds from amines, organic chemistry and other directions, which can solve the problems of serious environmental pollution and long production cycle, and achieve high purity and production efficiency. The effect of short cycle and simple steps

Active Publication Date: 2019-09-10
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method takes 16-26 hours to prepare once, the production cycle is too long, and long-term stirring and large-scale use of organic solvents are required, causing serious environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dissolve commercially available tetraethylammonium chloride and commercially available sodium fluoroborate in water to form 3mol / L solutions respectively. After mixing 100 mL each of the two solutions, a precipitate was formed in the solution, and about 11 g of the precipitate was obtained by filtration. The main component was tetraethylammonium tetrafluoroborate after testing.

Embodiment 2

[0024] Dissolve commercially available tetraethylammonium chloride and sodium tetrafluoroborate in water respectively to make 100mL of 6mol / L solutions, and drop the tetraethylammonium chloride solution into the sodium tetrafluoroborate solution under stirring at room temperature. As the addition proceeded, the solution gradually changed from clear to cloudy. After the dropwise addition was completed, it was filtered under reduced pressure and washed with a small amount of ice water to obtain 103 g of a wet salt-like solid. Tested by silver nitrate turbidimetric method, the content of chloride ions is relatively high, indicating that a certain amount of sodium chloride is mixed in the crude product.

Embodiment 3

[0026] Dissolve commercially available tetraethylammonium chloride and sodium tetrafluoroborate in water respectively to make 100mL of 6mol / L solutions, and drop the tetraethylammonium chloride solution into the sodium tetrafluoroborate solution under stirring at room temperature. As the addition proceeded, the solution gradually changed from clear to cloudy. When the solution was added dropwise to 40 mL, filter under reduced pressure, and after the filtrate was collected, 20 mL of tetraethylammonium chloride solution was added dropwise, and the resulting solid was suction-filtered again. The above steps were repeated until all the 100mL tetraethylammonium chloride solution was added dropwise. The solids filtered each time were washed with a small amount of ice water and stored separately, and tested by silver nitrate turbidimetry. The solids obtained by the last two filtrations had obvious chloride ions.

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PUM

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Abstract

The invention discloses a method for preparing electrolyte salt tetraethylammonium tetrafluoroborate for an electronic power supply. Sold tetraethylammonium chloride and sodium tetrafluoroborate are adopted as synthesis raw materials, water is adopted as a solvent, feeding is carried out according to the molar ratio of tetraethylammonium chloride to sodium tetrafluoroborate being (0.2-1):1, solidsare collected after stirring and reacting are carried out, and crude tetraethylammonium tetrafluoroborate is obtained; the obtained crude product is intensely stirred and dispersed with a small amount of water for 10 min to 60 min at room temperature, and filtering is carried out; then the solids obtained through filtering are washed with ethyl alcohol of the temperature of -10 DEG C to 0 DEG C,and tetraethylammonium tetrafluoroborate is obtained after drying is carried out. According to the method, the crude product can be obtained through direct filtering after feeding, a high-purity product can be obtained through one step of simple purification, the steps are simple, the production period is short, and the purity is high; only a small amount of ethyl alcohol for washing is used as anorganic solvent in the whole process, environmental pollution is avoided, the requirement for equipment is extremely low, vacuum, corrosion prevention and heating are not needed in the synthesis process, and the energy consumption and the cost are remarkably reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of tetraethylammonium tetrafluoroborate, an electrolyte salt for electronic power sources. Background technique [0002] Tetraethylammonium tetrafluoroborate ((C 2 h 5 ) 4 N=BF 4 - ) is often used as the electrolyte salt of organic supercapacitors. Traditional methods often use quaternary ammonium bases or quaternary ammonium salts as raw materials to react with fluoroboric acid to prepare tetraethylammonium tetrafluoroborate. Yet, when adopting quaternary ammonium base as raw material, often can have a lot of metal ions such as potassium, sodium in the product, influence the purity of product; Problems such as high cost and environmental pollution caused by difficult recycling. [0003] Patent document CN1768979A discloses a method for synthesizing tetraethylammonium tetrafluoroborate by using fluoboric acid and tetraethylammoniu...

Claims

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Application Information

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IPC IPC(8): C07C209/68C07C211/63
Inventor 陈果王红郭小峰
Owner WUHAN UNIV
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