Tetraethylammonium tetrafluoroborate synthesis
- Product Name:Tetraethylammonium tetrafluoroborate
- CAS Number:429-06-1
- Molecular formula:C8H20BF4N
- Molecular Weight:217.06
Yield:429-06-1 65.8%
Reaction Conditions:
at 20;Temperature;
Steps:
1-5; 1-2; 4-7 (1) Synthesis of tetraethylammonium tetrafluoroborate
85mL 6mol / L tetraethylammonium chloride solution was added dropwise to 100mL 6mol / L sodium tetrafluoroborate solution under stirring at room temperature As the addition progressed, the solution gradually changed from clear to cloudy. After the completion of the dropwise addition, the mixture was filtered under reduced pressure, and the solid was washed with a small portion of ice water to obtain a crude salty product (92 g). The sodium chloride content was less than 1% by silver nitrate turbidimetry. (2) Purification of tetraethylammonium The step (1) to give a wet salt of the crude product 50g dispersed in the procedure of Example 4, (2) the obtained filtrate A to give a crude dispersion, at room temperature with vigorous stirring the dispersion for 15 minutes, the solid was collected by filtration under reduced pressure, the filtrate was collected standby (filtrate B), the solid was washed with ice water, -10 ° C - 0 ° C ethanol, and drained as much as possible. Then the product was placed in a vacuum drying oven at a pressure of 0.001 MPa and gradually increased from room temperature to 60 ° C in 12 hours. Vacuum drying, finally obtained 40g of white tetraethylammonium tetrafluoroborate solid, from the commercially available tetraethylammonium chloride raw material to the final product, the total yield is 65.8%, the detection purity is greater than 99.95%, the chloride ion content is less than 90ppm, sodium The ion content is less than 100 ppm. Repeated experiments have shown that the filtrate can replace the pure water as a dispersion to effectively increase the overall yield. This substitution can be repeated. Use at least 5 times without affecting product purity.
References:
CN108586263,2018,A Location in patent:Paragraph 0021-0042; 0045-0052
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