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

Inactive Publication Date: 2009-10-14
STELLA CHEMIFA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the fluorine gas used in this method is very dangerous and requires close attention and experience
Moreover, this method has problems in that it is limited to the case where the fluorine compound is a powder, and it is limited to implementation at room temperature or higher.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

Provided is a process for purifying a fluorine compound capable of yielding a highly pure fluorine compound by removing at least oxygen from a fluorine compound containing an oxygen compound as an impurity. In a process according to the present invention for purifying a fluorine compound, the following is brought into contact with the fluorine compound, which contains an oxygen compound as an impurity, thereby removing at least oxygen: carbonyl fluoride in an amount of a 0.1-fold equivalent or more and a 100-fold equivalent or less of oxygen atoms in the fluorine compound.

Description

technical field [0001] The present invention relates to a method for purifying fluorine compounds into high-purity fluorine compounds by simply removing oxygen compound impurities contained in fluorine compounds. Background technique [0002] Conventionally, as a method for purifying a fluorine compound by removing an oxygen compound as an impurity present in a fluorine compound, a method of adding anhydrous hydrogen fluoride solution to a fluorine compound and repeating crystallization, solid-liquid separation, and drying steps several times (e.g. , refer to Patent Documents 1 and 2). However, the anhydrous hydrogen fluoride solution used in the above method is very dangerous, requires close attention and experience, and thus has poor operability. Also, in this method, there is a problem that the manufacturing cost and the number of steps increase. [0003] In addition, a method of reducing oxygen components and carbon components present in fluorine compounds with fluorin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B9/08C07C209/84C07C211/63C07D233/58
CPCC01F11/22C01B7/195C07D233/58C01F17/0062C01B35/065C01P2006/82C01B25/10C01P2006/80C01F17/265C01B9/08C07C7/148
Inventor 胁雅秀酒井大辅樱井稔久
Owner STELLA CHEMIFA CORP
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