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Method for synthesizing tetraethylammonium tetrafluoroborate through using micro-channel reactor

A technology of tetraethylammonium tetrafluoroborate and microchannel reactor, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve problems such as low conversion rate and long reaction time, and achieve production cost Low cost, less waste, high safety performance

Active Publication Date: 2017-04-19
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for synthesizing tetraethylammonium tetrafluoroborate using a microchannel reactor, thereby solving the problems of low conversion rate and long reaction time of the existing preparation method

Method used

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  • Method for synthesizing tetraethylammonium tetrafluoroborate through using micro-channel reactor
  • Method for synthesizing tetraethylammonium tetrafluoroborate through using micro-channel reactor
  • Method for synthesizing tetraethylammonium tetrafluoroborate through using micro-channel reactor

Examples

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Embodiment 1

[0026] The method for utilizing the microchannel reactor of the present embodiment to synthesize tetraethylammonium tetrafluoroborate comprises: 150g fluoroboric acid solution (mass concentration is 25%) and 270g tetraethylammonium hydroxide solution (mass concentration is 40%) Pass it into a microchannel reactor, the volume flow ratio of fluoboric acid solution and tetraethylammonium hydroxide solution is 1:2, stay at 40°C for 3min to obtain tetraethylammonium tetrafluoroborate solution, evaporate, concentrate and crystallize to obtain Tetraethylammonium tetrafluoroborate crude product and mother liquor, the mother liquor is used to prepare fluoboric acid solution.

[0027] The purification process of tetraethylammonium tetrafluoroborate crude product is as Figure 4 As shown, the crude product of tetraethylammonium tetrafluoroborate and deionized water twice its mass were mixed in a reaction kettle, heated and boiled, cooled and crystallized, and solid-liquid separator was u...

Embodiment 2

[0030] The method for utilizing the microchannel reactor of the present embodiment to synthesize tetraethylammonium tetrafluoroborate comprises: 150g fluoroboric acid solution (mass concentration is 20%) and 270g tetraethylammonium hydroxide solution (mass concentration is 10%) Pass it into a microchannel reactor, the volume flow ratio of fluoboric acid solution and tetraethylammonium hydroxide solution is 1:5, stay at 20°C for 3min, obtain tetraethylammonium tetrafluoroborate solution, evaporate, concentrate and crystallize to obtain Tetraethylammonium tetrafluoroborate crude product and mother liquor, the mother liquor is used to prepare fluoboric acid solution.

[0031] The purification process of the tetraethylammonium tetrafluoroborate crude product is the same as in Example 1.

[0032] The conversion rate of the product obtained in this embodiment is 99.76%, and the yield rate is 93.72%.

Embodiment 3

[0034] The method for utilizing the microchannel reactor of the present embodiment to synthesize tetraethylammonium tetrafluoroborate comprises: 150g fluoroboric acid solution (mass concentration is 30%) and 270g tetraethylammonium hydroxide solution (mass concentration is 15%) Pass it into the microchannel reactor, the volume flow ratio of fluoboric acid solution and tetraethylammonium hydroxide solution is 1:5, stay at 50°C for 30s, obtain tetraethylammonium tetrafluoroborate solution, evaporate, concentrate and crystallize to obtain Tetraethylammonium tetrafluoroborate crude product and mother liquor, the mother liquor is used to prepare fluoboric acid solution.

[0035] The purification process of the tetraethylammonium tetrafluoroborate crude product is the same as in Example 1.

[0036] The conversion rate of the product obtained in this embodiment is 99.88%, and the yield rate is 93.82%.

[0037] The technical indicators of tetraethylammonium tetrafluoroborate obtained...

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Abstract

The invention relates to a method for synthesizing tetraethylammonium tetrafluoroborate through using a micro-channel reactor. The method comprises the following steps: introducing a tetraethylammonium hydroxide solution and an excess amount of a fluorboric acid solution to the micro-channel reactor, carrying out a reaction at 10-60 DEG C for 30 s to 50 min to obtain a tetraethylammonium tetrafluoroborate solution, and crystallizing the tetraethylammonium tetrafluoroborate solution to obtain crude tetraethylammonium tetrafluoroborate. The crude tetraethylammonium tetrafluoroborate is prepared through the reaction of the tetraethylammonium hydroxide solution and the fluorboric acid solution in the micro-channel reactor. Compared with production technologies adopting routing reactors, the method disclosed in the invention has the advantages of uniform heat and mass transfer process, no amplified reaction, and realization of increase of the raw material conversion rate through effectively reducing side reactions by adopting above reaction conditions. The method also has the characteristics of great shortening of the reaction time, realization of continuous production of the tetraethylammonium tetrafluoroborate, production efficiency increase and production cost reduction.

Description

technical field [0001] The invention belongs to the field of preparation of organic quaternary ammonium tetrafluoroborate, and in particular relates to a method for synthesizing tetraethylammonium tetrafluoroborate by using a microchannel reactor. Background technique [0002] Supercapacitors have the characteristics of high energy density, high power density, and large specific capacity, and have great application prospects in the fields of electric vehicles, mobile communications, and national defense. Since tetraethylammonium tetrafluoroborate (Et 4 N + BF 4 - ) has high electrical conductivity, good thermal stability and high-voltage resistance, and has been widely used as an electrolyte salt for supercapacitor electrolyte systems. [0003] The patent with publication number CN1762979A discloses a preparation method of tetraethylammonium tetrafluoroborate, which utilizes tetraethylammonium halide salt and fluoboric acid to carry out exchange reaction in the presence ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/63C07C209/84
CPCC07C209/00C07C209/84C07C211/63
Inventor 薛旭金侯红军刘海霞张照坡司腾飞于洋杨明霞薛峰峰王永勤王鹏杰辛婉婉
Owner DO FLUORIDE CHEM CO LTD