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Highly purified fluoride fused salt and preparation method thereof

A fluoride salt and fluoride technology, applied in the field of high-purity fluoride molten salt and its preparation, can solve the problems of difficult preparation, long preparation period and the like

Inactive Publication Date: 2013-07-24
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation cycle of this method is very long, and the molten molten salt needs to be converted into high-purity anhydrous HF and H 2 Alternate treatment for more than 48 hours, and high-purity anhydrous HF (water content less than 15ppm) is difficult to prepare, HF and H 2 There is also a higher risk of using

Method used

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  • Highly purified fluoride fused salt and preparation method thereof
  • Highly purified fluoride fused salt and preparation method thereof

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preparation example Construction

[0091] In the present invention, the preparation method steps of preferred molten salt are as follows:

[0092] (i) providing ammonium bifluoride-fluoride salt mixture, wherein said mixture contains fluoride salts LiF, NaF and KF and ammonium bifluoride, wherein said ammonium bifluoride has a purity ≥ 99.9wt%;

[0093] (ii) heating and melting the ammonium bifluoride-fluoride salt mixture to form a high-purity fluoride salt melt; wherein, the oxides in the fluoride salt react with hydrogen fluoride released by the decomposition of ammonium bifluoride to generate water, and the water vapor venting; and

[0094] (iii) Cooling said high-purity fluoride salt melt, thereby fluoride molten salt.

[0095] Wherein, step (i) includes: providing a fluoride salt mixture, wherein the fluoride salt includes LiF, NaF and KF; and adding ammonium bifluoride with a purity ≥ 99.9wt% to the fluoride salt mixture, thereby obtaining ammonium bifluoride-fluoride salt mixture; and / or

[0096] Pro...

Embodiment 1

[0119] Preparation and detection of embodiment 1 high-purity ammonium bifluoride

[0120] Raw materials: 99% ammonium bifluoride (purchased from Shanghai Wujiaoxing Technology Co., Ltd.), wherein the chloride ion content is 322ppm, the nitrate is 10ppm, the phosphate is 20ppm, and the sulfate is 60ppm. Deionized water that has been treated by itself, and absolute ethanol after treatment.

[0121] Add 1L of deionized water to a 2L PTFE reactor, heat it in a water bath to 80 degrees, slowly add 1.2kg of ammonium bifluoride, and after it is completely dissolved, filter it with a PTFE membrane while it is still hot, and wait for slow cooling to crystallize. The crystals were filtered out, washed with ethanol for 5 times, crushed, and dried in a vacuum oven at 80°C.

[0122] The content of ammonium bifluoride obtained by the method is greater than 99.9%, the chloride ion content is lower than 85ppm, the nitrate radical is lower than 10ppm, the phosphate radical is lower than 20ppm...

Embodiment 2

[0123] The preparation of embodiment 2LiF-NaF-KF molten salt (No.1)

[0124] Using LiF, NaF and KF as raw materials, the content of LiF and NaF is 99.9%, and the content of KF is 99.97%. The above raw materials are all treated in a vacuum oven at 300-400°C for 4 hours, and then the molar percentage is LiF:NaF:KF =46.5:11.5:42 ratio weighing, a total of 20kg. Add 3.0 kg of high-purity ammonium bifluoride with a mass ratio of 15% as a fluorination reagent, seal and mix. Transfer the mixed fluoride salt mixture to the graphite crucible of the vacuum induction melting furnace, seal it, evacuate it to below 10Pa, and remove water under high vacuum for 1 hour. Fill high-purity N2 to normal pressure, heat and melt according to the set program: heating from room temperature to 300°C takes 1 hour; heating from 300°C to 450°C takes 2 hours; heating from 450°C to 700°C takes 1 hour; 700 ° C for 2 hours, a total of 6 hours. Then it is cooled to about 600°C, and the crucible is rotated ...

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Abstract

The invention provides a highly purified fluoride fused salt and a preparation method thereof. Specifically, the method comprises the following steps of: (i) providing a ammonium bifluoride-fluoride salt mixture, wherein the mixture contains the components of fluoride salts LiF, NaF, KF and ammonium bifluoride, and the purity of the ammonium bifluoride is not less than 99.9wt%; (ii) heating and fusing the ammonium bifluoride-fluoride salt mixture so as to obtain a highly purified fluoride salt melt; and (iii) cooling the high purified fluoride salt melt so as to obtain the fluoride fused salt. The fused slat is few in impurity, high in purity, stable in physicochemical property, and suitable for the wide preparation and application in the nuclear industry.

Description

technical field [0001] The invention belongs to the field of nuclear energy industry technology and chemical technology, and in particular relates to a high-purity molten fluoride salt and a preparation method thereof. Background technique [0002] The molten salt nuclear reactor is a reactor commonly used in nuclear power generation technology. Molten salt nuclear reactors are liquid nuclear fuels obtained by directly dissolving nuclear fuel into molten salt, such as liquid thorium fluoride reactors and uranium tetrafluoride reactors. Because the molten salt nuclear reactor has extremely high economic efficiency, the direct heat exchange method of its fuel makes it have the advantage of miniaturization, so it has a bright prospect for providing power for ships and aircraft. [0003] Molten salt in molten state is used as a solvent and coolant in molten salt nuclear reactors. The molten salt commonly used in such nuclear reactors is a molten salt mixture of fluorinated sal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G21C15/28
CPCY02E30/30
Inventor 肖吉昌宗国强王荣荣董群安陈博张龙陈伟
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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