Preparation and purification method of lithium hexafluorophosphate
A technology of lithium hexafluorophosphate and purification method, which is applied in the field of preparation and purification of electrolyte salt lithium hexafluorophosphate, can solve problems such as affecting battery safety, increasing battery internal resistance, reducing moisture content, etc., and achieves the effects of shortening production cycle, reducing moisture and improving efficiency
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Embodiment 1
[0047] A preparation method of lithium hexafluorophosphate, comprising the following steps:
[0048] (1) Preparation of lithium fluoride solution
[0049] Take 1000kg of anhydrous hydrogen fluoride and add it to the synthesis reaction kettle, then add 50kg of high-purity lithium fluoride through an automatic closed feeder, stir well, and control the temperature at around -5°C.
[0050] (2)PF 5 Preparation and purification:
[0051] Add 405kg of phosphorus pentachloride to the stainless steel reactor using a vacuum feeder, and add 195kg of anhydrous hydrogen fluoride into the reactor through an automatic regulating valve. The product is PF 5 , hydrogen chloride, the mixed gas contains a small amount of unreacted hydrogen fluoride, which exists in gaseous form; the mixed gas enters the precision gas filter (filter accuracy 0.1 μm), that is, high-purity PF is prepared 5 Mixed gas with hydrogen chloride.
[0052] (3) After purification, it enters the reaction kettle added wit...
Embodiment 2
[0059] A preparation method of lithium hexafluorophosphate, comprising the following steps:
[0060] (1) Slowly feed fluorine gas and nitrogen gas into the mother liquor after crystallization separation and mix 1kg (F 2 : N 2 =1:4), while stirring, the process lasted for 30 minutes to remove trace moisture in the mother liquor. (F 2 +H 2 O=HF+HFO)
[0061] (2) Return 550kg of all the mother liquors after the removal of impurities in the reactor, then add 500kg of hydrogen fluoride raw material, then add 37kg of lithium fluoride, fully stir, and control the temperature at around -5°C;
[0062] (3) Add 300kg of phosphorus pentachloride to the stainless steel reactor using a vacuum feeder, and add 150kg of anhydrous hydrogen fluoride into the reactor through an automatic regulating valve. MPa, the reaction product is PF 5 , hydrogen chloride, the mixed gas contains a small amount of unreacted hydrogen fluoride, which exists in gaseous form; the mixed gas enters the precisio...
Embodiment 3
[0068] A preparation method of lithium hexafluorophosphate, comprising the following steps:
[0069] (1) Preparation of lithium fluoride solution
[0070] Take 1000kg of anhydrous hydrogen fluoride and add it to the synthesis reaction kettle, then add 50kg of high-purity lithium fluoride through an automatic closed feeder, stir well, and control the temperature at around -5°C.
[0071] (2)PF 5 Preparation and purification:
[0072] Add 405kg of phosphorus pentachloride to the stainless steel reactor using a vacuum feeder, and add 195kg of anhydrous hydrogen fluoride into the reactor through an automatic regulating valve. The temperature of the reaction process is controlled at about 150°C, the pressure is controlled at 0.05MPa, and the reaction product is PF. 5 , hydrogen chloride, the mixed gas contains a small amount of unreacted hydrogen fluoride, which exists in gaseous form; the mixed gas enters the precision gas filter (filter accuracy 0.1 μm), that is, high-purity PF ...
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