A kind of molten salt deoxidation method using nitrogen trifluoride as fluorinating agent
A technology of nitrogen trifluoride and fluorinating agent, which is applied in chemical instruments and methods, fluoride preparation, alkali metal fluoride, etc., and can solve problems such as high cost, equipment corrosion, and poor process safety
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Embodiment 1
[0040] Example 1KF-ZrF 4 Molten salt system deoxidation
[0041] (1) 2000gKF-ZrF 4 (58-42mol%) is placed in the reactor, the lid of the kettle is covered, and the atmosphere in the reactor is replaced with pure argon.
[0042](2) Heating the reactor to raise the temperature from room temperature to 200°C, and keep it warm for 3 hours; at the end of the heat preservation, replace the atmosphere in the reactor with pure argon; heat the reactor again, and raise the temperature from 200°C to 350°C, keep it warm 3h; at the end of the heat preservation, replace the atmosphere in the reactor with pure argon to remove the water generated during the heating process. Continue to heat the reactor to make the temperature reach 600°C; keep it warm for 3 hours until the molten salt is completely melted, and pass the mixed gas of nitrogen trifluoride and argon (NF 3 The volume fraction is 10%), and the flow rate is 1L / min to carry out purification and deoxidation.
[0043] (3) Stop feedi...
Embodiment 2
[0045] Example 2NaF-ZrF 4 Molten salt system deoxidation
[0046] (1) 1000g NaF-ZrF 4 (59.5-40.5mol%) is placed in the reactor, the lid of the kettle is covered, and the atmosphere in the reactor is replaced with pure argon.
[0047] (2) Heating the reactor to raise the temperature from room temperature to 250°C, and keep it warm for 2 hours; at the end of the heat preservation, replace the atmosphere in the reactor with pure argon; heat the reactor again, and raise the temperature from 250°C to 400°C, then keep it warm 2h; at the end of the heat preservation, replace the atmosphere in the reactor with pure argon to remove the water generated during the heating process. Continue to heat the reactor to make the temperature reach 700°C; keep it warm for 5 hours until the molten salt is completely melted, and pass the mixed gas of nitrogen trifluoride and argon (NF 3 The volume fraction is 20%), and the flow rate is 0.5L / min to carry out purification and deoxidation.
[0048]...
Embodiment 3
[0050] Example 3LiF-BeF 2 Molten salt system deoxidation
[0051] (1) 5kg LiF-BeF 2 (67-33mol%) is placed in the reactor, the lid of the kettle is covered, and the atmosphere in the reactor is replaced with pure argon.
[0052] (2) Heating the reactor to raise the temperature from room temperature to 200°C, and keep it warm for 2 hours; replace the atmosphere in the reactor with pure argon at the end of the heat preservation; heat the reactor again, and raise the temperature from 200°C to 400°C, keep it warm 2h; at the end of the heat preservation, replace the atmosphere in the reactor with pure argon to remove the water generated during the heating process. Continue to heat the reactor to make the temperature reach 500°C; keep warm for 10 hours until the molten salt is completely melted, and feed a mixed gas of nitrogen trifluoride and argon into the molten fluoride salt in the reactor through a mass flow meter (the volume fraction of NF3 is 50%), the flow rate is 2L / min, ...
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