A kind of preparation method of potassium hexafluorophosphate
A technology of potassium hexafluorophosphate and potassium hydrogen fluoride, applied in chemical instruments and methods, sodium/potassium compounds, inorganic chemistry, etc., can solve the problems of increasing the difficulty of control, easily causing danger, etc., achieving easy control, reducing risk, The effect of responsiveness
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Embodiment 1
[0035] A preparation method of potassium hexafluorophosphate, comprising the following steps:
[0036] (1) Add 150 g of anhydrous hydrogen fluoride to 78 g of dried potassium hydrogen fluoride solid at 0-8°C;
[0037] (2) Adjust the temperature to -5°C, turn on the vacuum pump and adjust the vacuum degree to 0.5Pa, make the reaction condition a slight negative pressure, slowly add 160g of phosphorus oxychloride dropwise, and control the dropping rate so that the temperature does not exceed -2°C After the dropwise addition is completed, continue to stir and react for 30 minutes;
[0038] (3) Adjust the temperature to 80°C and keep it warm for 30 minutes; adjust the vacuum to 0.7Pa, extract the residual hydrogen fluoride gas and the generated hydrochloric acid gas, and neutralize it with the lye;
[0039] (4) Slowly add 50% potassium hydroxide solution to the reaction, and adjust the pH value to 7;
[0040] (5) The reacted material is cooled to room temperature, and 181g of po...
Embodiment 2
[0045] A preparation method of potassium hexafluorophosphate, comprising the following steps:
[0046] (1) Add 160 g of anhydrous hydrogen fluoride to 78 g of dried potassium hydrogen fluoride solid at 0-8°C;
[0047] (2) Adjust the temperature to -5°C, turn on the vacuum pump and adjust the vacuum degree to 0.5Pa, make the reaction condition a slight negative pressure, slowly add 163g of phosphorus oxychloride dropwise, and control the dropping rate so that the temperature does not exceed -2°C After the dropwise addition is completed, continue to stir and react for 30 minutes;
[0048] (3) Adjust the temperature to 80°C and keep it warm for 30 minutes; adjust the vacuum to 0.7Pa, extract the residual hydrogen fluoride gas and the generated hydrochloric acid gas, and neutralize it with the lye;
[0049] (4) Slowly add 50% potassium hydroxide solution to the reaction, and adjust the pH value to 7;
[0050] (5) The reacted material is cooled to room temperature, and the 182g p...
Embodiment 3
[0055] (1) Add 167g of anhydrous hydrogen fluoride to 78g of dry potassium hydrogen fluoride solid at 0-8°C;
[0056] (2) Adjust the temperature to -5°C, turn on the vacuum pump and adjust the vacuum to 0.5Pa, make the reaction condition a slight negative pressure, slowly add 165g of phosphorus oxychloride dropwise, and control the dropping rate so that the temperature does not exceed -2°C After the dropwise addition is completed, continue to stir and react for 30 minutes;
[0057] (3) Adjust the temperature to 80°C and keep it warm for 30 minutes; adjust the vacuum to 0.8Pa, extract the residual hydrogen fluoride gas and the generated hydrochloric acid gas, and neutralize it with the lye;
[0058](4) Slowly add 50% potassium hydroxide solution to the reaction, and adjust the pH value to 7;
[0059] (5) The reacted material was cooled to room temperature, and 183.7g of potassium hexafluorophosphate crude product was obtained after centrifugation;
[0060] (6) Add 300ml of wa...
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