Method for purifying fluorine compound
一种氟化合物、精制方法的技术,应用在氟化物制备、卤化硼化合物、稀土金属氟化物等方向,能够解决氟气危险等问题
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Embodiment 1
[0039] First, 300 g of ethylmethylimidazolium BF containing 500 ppm of water as an impurity 4 Put in a fluororesin bottle connected with suction and exhaust cocks.
[0040] Then, open the suction cock and fill with N with a water content of 1ppm or less. 2 50 vol% COF diluted with gas 2 After the gas, close the cock. makes COF 2 The usage-amount of gas is 5 times equivalent with respect to the oxygen atom of the said water|moisture content.
[0041] Furthermore, the fluororesin bottle was immersed in an oil bath and heated so that the internal temperature was 100°C. Then, the fluororesin bottle was taken out from the oil bath, and the bottle was shaken and stirred for 1 minute. Then, the bottle was returned to the oil bath and immersed for about 5 minutes until the internal temperature reached 100° C., the bottle was taken out from the oil bath again, and the bottle was shaken and stirred for 1 minute. This operation was repeated for 30 minutes.
[0042] Then, the fluor...
Embodiment 2
[0053] Concentration 50% by weight hydrofluoric acid is added in this calcium hydroxide in the mode that reaches 1.03 times of equivalent with respect to calcium hydroxide and is stirred, makes calcium fluoride (CaF 2 ) suspension. This calcium fluoride suspension was filtered and washed to obtain 900 g of calcium fluoride containing 45% by weight of water.
[0054] Then, calcium fluoride was dried in air at a temperature of 105° C. for 8 hours. The content of oxygen atoms in the dried calcium fluoride was measured and found to be 1500 ppm.
[0055] The dry calcium fluoride in N 2 Baking at 500° C. for 8 hours in air flow. Then, it was cooled to room temperature, and the oxygen atom content was measured again, and it was 880 ppm.
[0056] 200 g of calcined calcium fluoride was charged into a fluororesin bottle connected with a cock for air intake and exhaust. Then, open the suction cock and fill with N with a water content of 1ppm or less. 2 30 vol% COF diluted with gas ...
Embodiment 3
[0060] Concentration 50% by weight hydrofluoric acid is added in this calcium hydroxide in the mode that reaches 1.03 times of equivalent with respect to calcium hydroxide and is stirred, makes calcium fluoride (CaF 2 ) suspension. This calcium fluoride suspension was filtered and washed to obtain 900 g of calcium fluoride containing 45% by weight of water.
[0061] Then, calcium fluoride was dried in air at a temperature of 105° C. for 8 hours. The content of oxygen atoms in the dried calcium fluoride was measured and found to be 1500 ppm.
[0062] The dry calcium fluoride in N 2 Baking at 500° C. for 8 hours in air flow. Then, it was cooled to room temperature, and the oxygen atom content was measured again, and it was 880 ppm.
[0063] 200 g of calcined calcium fluoride was charged into a fluororesin bottle connected with a cock for air intake and exhaust. Then, open the suction cock and fill with 40% by volume COF diluted with HF gas with a moisture content of 5ppm or...
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