CN112891973B - Method for reducing oxygen content in halide molten salt - Google Patents
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- CN112891973B CN112891973B CN202110055209.8A CN202110055209A CN112891973B CN 112891973 B CN112891973 B CN 112891973B CN 202110055209 A CN202110055209 A CN 202110055209A CN 112891973 B CN112891973 B CN 112891973B
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Abstract
The invention discloses a method for reducing the oxygen content in halide molten salt. The method comprises the following steps: distilling the halide fused salt under a vacuum condition; wherein the vacuum degree under vacuum condition is 10 ‑5 ～10 3 Pa; in the distillation treatment, the distillation temperature is at least 200 ℃ higher than the condensation temperature, and the distillation temperature is 400-1200 ℃. The method for reducing the oxygen content in the halide molten salt can effectively reduce the oxygen content in the halide molten salt by more than 70 percent; the oxygen content in the treated distillation product can be as low as 560mg/Kg or less, and even can be as low as 200mg/Kg or less; and has high treatment efficiency and weak corrosion to equipment.
Description
Technical Field
The invention relates to a method for reducing the oxygen content in halide molten salt.
Background
The fused salt energy storage technology can be combined with a photo-thermal power generation system to meet the peak regulation requirement of a power grid. Among them, the halide molten salt has a certain application potential. For example, chloride molten salt is cheap and has large phase change latent heat; the fluoride fused salt has high melting point and large fusion latent heat, and has good heat transfer performance. However, the halide may absorb water during production to deliquesce to generate oxygen or may be contaminated with oxygen during storage, so that oxygen is inevitably contained in the halide molten salt, and the corrosiveness of the halide molten salt having a high oxygen content is significantly enhanced.
In the research of nuclear reactors, the dry post-treatment technology using molten salt as a medium has the advantages of radiation resistance, compact equipment, low critical risk, nuclear diffusion resistance, less radioactive waste amount and the like, and can be used for treating the spent fuel of the reactor, wherein the high-temperature molten salt electrolysis technology mainly uses halide molten salt as a medium to carry out electrolysis treatment on fuel elements at high temperature. In the electrolytic process, if the oxygen content of the molten salt medium is too high, the electrolytic efficiency of the electrolytic process is affected, and meanwhile, alkaline earth fission products or rare earth fission products are also converted into corresponding oxides or oxyhalides, so that the electrolytic purification and recovery cannot be realized.
The halide molten salt system can also be used as a nuclear fuel carrier and a coolant of a molten salt reactor, if the oxygen content in the carrier salt is too high, part of fission products generated by nuclear fuel fission can be converted into oxygen-containing compounds with low solubility, so that precipitation is generated in the molten salt reactor, a fixed-point heat release source and a radiation source are formed, the operation safety of the reactor is threatened, and the difficulty of reactor maintenance is increased.
Therefore, the oxygen content in the halide molten salt is effectively reduced, and the application of the halide molten salt is facilitated.
At present, the method for reducing the oxygen content in the halide molten salt comprises H 2 A hydrogen halide process, an electrochemical process or a transpiration process. Wherein H 2 The hydrogen halide method can remove water, oxides and the like in the molten salt, but has longer treatment time, and meanwhile, hydrogen halide has certain danger and stronger corrosivity to equipment in the operation process, and particularly when the hydrogen halide molten salt with higher oxygen content is treated, the treatment time is longer, and the corrosivity to the equipment is more serious; compared with H 2 The hydrogen halide method, although the electrochemical method can treat molten salt with low oxygen content level and slightly relieves the corrosiveness of equipment, has small treatment amount in unit time and low treatment efficiency; the transpiration method is simple in treatment process, and can treat the halide molten salt with high oxygen content, but the treatment method is long in time consumption and low in treatment efficiency due to the fact that the halide molten salt is heated under normal pressure.
Therefore, it is highly desirable to provide a method for efficiently reducing the oxygen content in the halide molten salt and achieving high treatment efficiency.
Disclosure of Invention
The invention provides a method for reducing the oxygen content in halide molten salt, aiming at solving the problems that the method for reducing the oxygen content in the halide molten salt in the prior art has strong corrosion to equipment and low treatment efficiency, and particularly takes a long time when the halide molten salt with high oxygen content is treated. The method for reducing the oxygen content in the halide molten salt can effectively reduce the oxygen content in the halide molten salt, has high treatment efficiency and weak corrosion to equipment.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for reducing the oxygen content in a halide molten salt comprises the following steps: distilling the halide fused salt under a vacuum condition to obtain a distilled product;
wherein, in the vacuum condition, the vacuum degree is 10 -5 ～10 3 Pa; in the distillation treatment, the distillation temperature is at least 200 ℃ higher than the condensation temperature, and is 400-1200 ℃.
In the present invention, the halide molten salt may be a halide molten salt conventionally used in the field of molten salt energy storage or the field of nuclear power reactors, and includes at least a halide. The halide molten salt can be derived from a halide molten salt used by a molten salt battery, a halide molten salt fuel carrier, a halide molten salt used by a molten salt reactor, or waste salt generated in a dry post-treatment process of reactor spent fuel. Among them, the dry post-treatment of the reactor spent fuel may be conventional in the art, such as a high temperature electrochemical treatment process or a fission product separation process.
The oxygen content in the halide fused salt can be 500-40000 mg/Kg, preferably 500-15000 mg/Kg, such as 1000-15000 mg/Kg, and further such as 1370mg/Kg or 10000 mg/Kg.
The oxygen content in the halide molten salt refers to the content of oxygen in the halide molten salt in the form of an oxide or oxyhalide.
Wherein, the halide generally refers to one or more of fluoride, chloride, bromide and iodide, and is preferably fluoride or chloride.
Wherein, theSaid fluoride may be LiF, NaF, KF and BeF 2 One or more of (a).
The fluoride is preferably LiF.
The fluoride is preferably LiF and BeF 2 (ii) a More preferably 67 mol% LiF and 33 mol% BeF 2 。
The fluoride is preferably LiF, NaF and KF; more preferably 46.5 mol% LiF, 11.5 mol% NaF and 42 mol% KF.
Wherein the chloride can be LiCl, NaCl, KCl and BeCl 2 One or more of (a).
The chloride is preferably LiCl.
The chloride is preferably NaCl.
The chloride is preferably KCl.
The chloride is preferably LiCl and KCl.
The chloride is preferably NaCl and KCl.
When two halides are included in the halide molten salt, the ratio of the mole percentages of the two halides can be any ratio, such as (1-2): 1. The halogen atoms in the two halides may be the same or different, preferably the same halogen atom.
When three halides are included in the halide molten salt, the ratio of the mole percentages of the three halides may be any ratio, such as 1: (3-4): (4-5), and further example 1: 3.65: 4. the halogen atoms in the three halides may be the same or different, preferably the same halogen atom.
In the invention, the distillation product is the halide molten salt after distillation treatment. Wherein, the oxygen content in the distillation product can be below 560mg/Kg, such as 100-480 mg/Kg, and further such as 180mg/Kg, 190mg/Kg, 320mg/Kg, 450mg/Kg or 560 mg/Kg.
In the present invention, the degree of vacuum is preferably 10 -2 ～10 3 Pa, more preferably 10 -1 ～10 3 Pa, for example, 5 to 15Pa or 90 to 110 Pa.
In the present invention, the distillation treatment is preferably performed under an inert atmosphere.
In the distillation treatment, the temperature difference between the distillation temperature and the condensation temperature is preferably 200 to 500 ℃, for example 230 ℃ or 300 ℃.
The distillation temperature is preferably 400 to 1200 ℃, more preferably 700 to 1000 ℃, such as 730 ℃, 900 ℃ or 950 ℃.
The time of the distillation treatment can be 0.5 to 5 hours, preferably 1 to 4 hours, for example 3 hours.
The amount of the distillation treatment may be 5 to 500g, preferably 10 to 350g, and more preferably 100g or 200 g.
The distillation treatment equipment may be conventional in the art, and generally comprises an evaporation unit, a condensation unit and a collection unit; preferably also an inert atmosphere unit. The inert atmosphere unit is used for providing an inert environment for the distillation process so as to ensure that halide molten salt in the distillation treatment and a distillation product after the distillation treatment are not polluted by atmosphere with high oxygen content again; meanwhile, the inert atmosphere unit can also provide inert gas required for restoring the distillation treatment equipment to normal pressure.
Wherein, the evaporation unit can comprise an evaporation furnace body and an evaporation container. The evaporation container can be arranged in a furnace cavity of the evaporation furnace body. The evaporation vessel may be an evaporation crucible. The size of the evaporation crucible may be conventional in the art, for example
The collection unit may be a collection crucible.
In a preferred embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt comprises the following steps: distilling the halide molten salt under inert atmosphere and vacuum condition to obtain a distilled product;
wherein the halides in the halide molten salt are 67 mol% LiF and 33 mol% BeF 2 (ii) a The oxygen content in the halide molten salt is 500-12000 mg/Kg;
in the vacuum condition, the vacuum degree is 5-30 Pa;
in the distillation treatment, the distillation temperature and the condensation temperature are respectively 800-1000 ℃ and 500-700 ℃; the temperature difference between the distillation temperature and the condensation temperature is 250-350 ℃,
the oxygen content in the distillation product is less than 480 mg/Kg.
In the preferred embodiment, the time for the distillation treatment is preferably 2 to 5 hours. The amount of the distillation treatment is preferably 100 to 400 g.
In a preferred embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt comprises the following steps: distilling the halide fused salt under inert atmosphere and vacuum condition to obtain a distilled product;
wherein the halide in the halide molten salt is lithium halide, preferably LiCl or LiF; the oxygen content in the halide molten salt is 1000-15000 mg/Kg;
in the vacuum condition, the vacuum degree is 5-150 Pa;
in the distillation treatment, the distillation temperature and the condensation temperature are respectively 700-1000 ℃ and 500-800 ℃; the temperature difference between the distillation temperature and the condensation temperature is 200-350 ℃,
the oxygen content in the distillation product is below 400 mg/Kg.
In the preferred embodiment, the time for the distillation treatment is preferably 0.5 to 4 hours. The amount of the distillation treatment is preferably 50 to 200 g.
In a preferred embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt comprises the following steps: distilling the halide molten salt under inert atmosphere and vacuum condition to obtain a distilled product;
wherein the halides in the halide molten salt are 46.5 mol% LiF, 11.5 mol% NaF and 42 mol% KF; the oxygen content in the halide molten salt is 30000-40000 mg/Kg;
in the vacuum condition, the vacuum degree is 5-30 Pa;
in the distillation treatment, the distillation temperature and the condensation temperature are respectively 800-1000 ℃ and 500-700 ℃; the temperature difference between the distillation temperature and the condensation temperature is 200-350 ℃,
the oxygen content in the distillation product is below 560 mg/Kg.
In the preferred embodiment, the time for the distillation treatment is preferably 0.5 to 2 hours. The amount of the distillation treatment is preferably 50 to 200 g.
In one embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt preferably comprises the following steps:
(1) filling inert gas in a furnace chamber of the evaporation furnace body under inert atmosphere, placing halide fused salt in an evaporation container of the distillation equipment, and sealing;
wherein the oxygen content in the halide molten salt is 600 mg/Kg; the halides in the halide molten salt are 67 mol% LiF and 33 mol% BeF 2 (ii) a The treatment amount of the halide molten salt is 200 g;
(2) setting the vacuum degree of the distillation equipment to be 10 Pa;
(3) setting the distillation temperature and the condensation temperature of the distillation equipment to be 950 ℃ and 650 ℃ respectively, and carrying out distillation treatment on the halide;
wherein the time of the distillation treatment is 3 h;
(4) after the distillation treatment is finished, the oxygen-containing impurities are left in the distillation container, and a distillation product is obtained in a collection unit;
wherein the oxygen content in the distillation product is 180 mg/Kg.
In one embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt preferably comprises the following steps:
(1) under the inert atmosphere, filling inert gas into a furnace chamber of the evaporation furnace body, placing halide fused salt into an evaporation container of the distillation equipment, and sealing;
wherein the oxygen content in the halide molten salt is 1370 mg/Kg; the halide in the halide molten salt is LiCl; the treatment amount of the halide molten salt is 10 g;
(2) setting the vacuum degree of the distillation equipment to be 100 Pa;
(3) setting the distillation temperature and the condensation temperature of the distillation equipment to be 730 ℃ and 500 ℃ respectively, and carrying out distillation treatment on the halide;
wherein the time of the distillation treatment is 1 h;
(4) after the distillation treatment is finished, the oxygen-containing impurities are left in the distillation container, and a distillation product is obtained in a collection unit;
wherein the oxygen content in the distillation product is 320 mg/Kg.
In one embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt preferably comprises the following steps:
(1) filling inert gas in a furnace chamber of the evaporation furnace body under inert atmosphere, placing halide fused salt in an evaporation container of the distillation equipment, and sealing;
wherein the oxygen content in the halide molten salt is 10000 mg/Kg; the halide in the halide molten salt is LiF; the treatment amount of the halide molten salt is 100 g;
(2) setting the vacuum degree of the distillation equipment to be 10 Pa;
(3) setting the distillation temperature and the condensation temperature of the distillation equipment to be 950 ℃ and 650 ℃ respectively, and carrying out distillation treatment on the halide;
wherein the time of the distillation treatment is 3 h;
(4) after the distillation treatment is finished, the oxygen-containing impurities are left in the distillation container, and a distillation product is obtained in a collection unit;
wherein the oxygen content in the distillation product is 190 mg/Kg.
In one embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt preferably comprises the following steps:
(1) under the inert atmosphere, filling inert gas into a furnace chamber of the evaporation furnace body, placing halide fused salt into an evaporation container of the distillation equipment, and sealing;
wherein the oxygen content in the halide molten salt is 40000 mg/Kg; the halides in the halide molten salt are 46.5 mol% LiF, 11.5 mol% NaF and 42 mol% KF; the treatment amount of the halide molten salt is 100 g;
(2) setting the vacuum degree of the distillation equipment to be 10 Pa;
(3) setting the distillation temperature and the condensation temperature of the distillation equipment to be 900 ℃ and 600 ℃, and carrying out distillation treatment on the halide;
wherein the time of the distillation treatment is 1 h;
(4) after the distillation treatment is finished, the oxygen-containing impurities are remained in the distillation container, and a distillation product is obtained in a collection unit;
wherein the oxygen content in the distillation product is 560 mg/Kg.
In one embodiment of the present invention, the method for reducing the oxygen content in the halide molten salt preferably comprises the following steps:
(1) under the inert atmosphere, filling inert gas into a furnace chamber of the evaporation furnace body, placing halide fused salt into an evaporation container of the distillation equipment, and sealing;
wherein the oxygen content in the halide molten salt is 10000 mg/Kg; the halides in the halide molten salt are 67 mol% LiF and 33 mol% BeF 2 (ii) a The treatment amount of the halide molten salt is 350 g;
(2) setting the vacuum degree of the distillation equipment to be 10 Pa;
(3) setting the distillation temperature and the condensation temperature of the distillation equipment to be 950 ℃ and 650 ℃ respectively, and carrying out distillation treatment on the halide;
wherein the time of the distillation treatment is 5 h;
(4) after the distillation treatment is finished, the oxygen-containing impurities are left in the distillation container, and a distillation product is obtained in a collection unit;
wherein the oxygen content in the distillation product is 450 mg/Kg.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
1. the method for reducing the oxygen content in the halide molten salt can effectively reduce the oxygen content in the halide molten salt by more than 70 percent, and even can reduce the oxygen content by more than 98 percent; the oxygen content in the treated distillation product can be as low as 560mg/Kg or less, and can even be as low as 200mg/Kg or less.
2. The method for reducing the oxygen content in the halide molten salt has high treatment efficiency, wherein the evaporation ratio of the halide molten salt is up to more than 99%, and the evaporation recovery rate is up to more than 80%.
3. Meanwhile, the method for reducing the oxygen content in the halide molten salt is weak in equipment corrosion.
Drawings
FIG. 1 is a photograph showing the appearance of a distilled product obtained by distilling the molten halide salt of example 1;
FIG. 2 is a photograph of an internal cross section (cut) of a distilled product obtained after the molten halide salt of example 1 was subjected to distillation treatment;
FIG. 3 is a photograph of oxygen-containing impurities remaining in a distillation vessel after the molten halide salt of example 1 was subjected to distillation treatment.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the invention thereto. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Examples 1 to 5
The halide molten salt in examples 1, 3 and 4 is a self-made simulated molten salt reactor fuel carrier salt; the halide molten salt in example 2 is a halide molten salt for a molten salt battery; the halide molten salt in example 5 is a halide molten salt used for a molten salt pile.
In embodiments 1 to 5, a method for reducing the oxygen content in a halide molten salt includes the steps of:
(1) after the halide fused salt is crushed, filling inert gas into the furnace of the evaporation furnace body in inert atmosphereIn the cavity, the crushed halide fused salt is placed in an evaporation crucible of distillation equipment
In, sealing;
(2) setting the vacuum degree of distillation equipment;
(3) setting the distillation temperature, the condensation temperature and the distillation time of distillation equipment, and distilling the halide molten salt;
(4) after the distillation treatment is finished, the oxygen-containing impurities are left in the evaporation crucible, and the distillation product is collected in the collection crucible;
the parameter conditions in steps (1) to (4) are shown in table 1.
TABLE 1
Effect example 1
(1) After the distillation treatment in example 1 was completed, the distillation product was cooled to room temperature, and a white molten salt product as shown in fig. 1 was obtained in a collection crucible, and the appearance was clean. The molten salt product shown in fig. 1 was cut, and it was seen that its inner section was also white as shown in fig. 2. The remaining product in the evaporation crucible in fig. 3 is an oxide impurity, and is grayish green. It can be seen that the distillation process has separated the oxide impurities from the white molten halide salt.
(2) The evaporation ratio and distillation recovery rate of the halide molten salt in examples 1 to 5 were calculated.
Wherein the evaporation ratio is (m) General assembly -m Remainder of )/m General (1) ×100％；
Evaporation recovery rate m Collecting /(m General assembly -m Remainder of )×100％；
m General assembly The total mass of the halide molten salt to be distilled, namely the halide molten salt treatment amount in the table 1;
m remains of The mass of the residual molten salt in the evaporation crucible after the distillation treatment;
m collecting The quality of the white molten salt product collected from the crucible was collected for distillation treatment.
The results are shown in Table 2.
(3) The oxygen content of the halide molten salt and the oxygen content of the halide molten salt after distillation treatment were measured by an oxygen content analyzer (model 0836) of LECO corporation, and the average values were measured twice.
The results are shown in Table 2.
TABLE 2
As can be seen from the data in table 2, in the method for reducing the oxygen content in the halide molten salt in embodiments 1 to 5, the evaporation ratio of the halide molten salt is as high as 99% or more, the distillation recovery rate can be 80% or more, the oxygen content in the halide molten salt can be effectively reduced by 70% or more, the treatment efficiency is high, and the oxygen content in the treated distillation product can be as low as 560mg/Kg or less, even as low as 200mg/Kg or less; meanwhile, the corrosion to equipment is weak.
Claims (39)
1. A method for reducing the oxygen content in a halide molten salt is characterized by comprising the following steps: distilling the halide molten salt under inert atmosphere and vacuum condition to obtain a distilled product;
wherein, in the vacuum condition, the vacuum degree is 0.1-10 3 Pa; in the distillation treatment, the distillation temperature is at least 200 ℃ higher than the condensation temperature, and the distillation temperature is 730-1200 ℃; the distillation treatment equipment comprises an evaporation unit, a condensation unit and a collection unit; the distillation treatment time is 0.5-5 h; the processing amount of the distillation treatment is 5-500 g.
2. The method for reducing the oxygen content in the halide molten salt according to claim 1, wherein the oxygen content in the halide molten salt is 500-40000 mg/Kg.
3. The method for reducing the oxygen content in the halide molten salt according to claim 2, wherein the oxygen content in the halide molten salt is 500-15000 mg/Kg.
4. The method for reducing the oxygen content in the halide molten salt according to claim 3, wherein the oxygen content in the halide molten salt is 1000-15000 mg/Kg.
5. The method of reducing oxygen content in a molten halide salt according to claim 4, wherein the oxygen content in the molten halide salt is 1370mg/Kg or 10000 mg/Kg.
6. A method of reducing the oxygen content of a halide molten salt as in claim 2 wherein the halide is one or more of fluoride, chloride, bromide and iodide.
7. A method of reducing the oxygen content in a halide molten salt as in claim 6 wherein the halide is a fluoride or chloride.
8. Method for reducing the oxygen content in molten halide salts according to claim 7, characterised in that the fluoride is LiF, NaF, KF and BeF 2 One or more of (a).
9. A method of reducing the oxygen content in a molten halide salt as in claim 8 where the fluoride is LiF.
10. The method of reducing oxygen content in a molten halide salt of claim 8 wherein the fluoride is LiF and BeF 2 。
11. The halide-reducing molten salt of claim 10A method of moderate oxygen content, characterized in that when said fluoride is LiF or BeF 2 When the fluoride is 67 mol% LiF and 33 mol% BeF 2 。
12. A method of reducing the oxygen content in molten halide salts as claimed in claim 8 where the fluoride is LiF, NaF and KF.
13. A method of reducing the oxygen content in a molten halide salt as claimed in claim 12 where the fluoride is 46.5 mol% LiF, 11.5 mol% NaF and 42 mol% KF when the fluoride is LiF, NaF and KF.
14. A method of reducing the oxygen content in halide molten salts as claimed in claim 7 where the chlorides are LiCl, NaCl, KCl and BeCl 2 One or more of (a).
15. A method of reducing the oxygen content in a halide molten salt as claimed in claim 14 where the chloride is LiCl.
16. The method of reducing the oxygen content in a halide molten salt of claim 14 wherein the chloride is NaCl.
17. A method of reducing the oxygen content in a halide molten salt as claimed in claim 14 where the chloride is KCl.
18. A method of reducing the oxygen content in a halide molten salt as claimed in claim 14 where the chlorides are LiCl and KCl.
19. A method of reducing the oxygen content in halide molten salt as claimed in claim 14, characterised in that the chlorides are NaCl and KCl.
20. The method of reducing oxygen content in a halide molten salt as claimed in claim 1 wherein when two halides are included in the halide molten salt, the ratio of the mole percent of the two halides is arbitrary;
alternatively, when three halides are included in the halide molten salt, the ratio of the mole percentages of the three halides is arbitrary.
21. The method for reducing oxygen content in a halide molten salt as claimed in claim 20, wherein when two halides are included in the halide molten salt, the ratio of the mole percentages of the two halides is (1-2): 1;
or, when three halides are included in the halide molten salt, the ratio of the mole percentages of the three halides is 1: (3-4): (4-5).
22. A method of reducing the oxygen content in a halide molten salt as claimed in claim 21, wherein when two halides are included in the halide molten salt, the halogen atoms in the two halides are the same halogen atom;
or, when three halides are included in the halide molten salt, the halogen atoms in the three halides are the same halogen atom.
23. A method of reducing the oxygen content in a halide molten salt as claimed in any one of claims 1 to 22 wherein the oxygen content in the distillation product is 560mg/Kg or less.
24. A method of reducing the oxygen content in a molten halide salt as claimed in claim 23 wherein the oxygen content in the distilled product is 100 to 480 mg/Kg.
25. A method of reducing the oxygen content in a molten halide salt as claimed in claim 24 where the oxygen content in the distilled product is 180mg/Kg, 190mg/Kg, 320mg/Kg, 450mg/Kg or 560 mg/Kg.
26. The method for reducing the oxygen content in a halide molten salt according to any one of claims 1 to 22, wherein in the distillation treatment, the temperature difference between the distillation temperature and the condensation temperature is 200 to 500 ℃.
27. A method of reducing the oxygen content in a halide molten salt as claimed in claim 26 where in the distillation process the temperature difference between the distillation temperature and the condensation temperature is 230 ℃ or 300 ℃.
28. The method of reducing oxygen content in a halide molten salt as in any one of claims 1 to 9, wherein the distillation temperature is 730 ℃, 900 ℃ or 950 ℃.
29. A method for reducing the oxygen content in a halide molten salt as claimed in any one of claims 1 to 22, wherein the distillation treatment time is 1 to 4 hours.
30. A method for reducing the oxygen content in a halide molten salt as claimed in claim 29 where the distillation treatment time is 3 hours.
31. A method for reducing the oxygen content in a halide molten salt as claimed in any one of claims 1 to 22, wherein the distillation treatment is carried out at a throughput of 10 to 350 g.
32. A method of reducing the oxygen content in a halide molten salt as claimed in claim 31 where the distillation process throughput is 100g or 200 g.
33. The method for reducing the oxygen content in the halide molten salt according to any one of claims 1 to 22, wherein the distillation treatment equipment comprises an inert atmosphere unit.
34. A method for reducing the oxygen content in halide molten salt as claimed in any one of claims 1 to 22, wherein the evaporation unit comprises an evaporation furnace body and an evaporation vessel.
35. A method of reducing the oxygen content of halide molten salt as claimed in claim 34 where the evaporation vessel is an evaporation crucible.
36. A method of reducing the oxygen content in halide molten salt as claimed in claim 35, characterised in that the evaporation crucible has dimensions of
37. A method for reducing the oxygen content in a halide molten salt as claimed in any one of claims 1 to 22 wherein the collection unit is a collection crucible.
38. A method of reducing the oxygen content in a halide molten salt as claimed in any one of claims 1 to 22 comprising the steps of:
distilling the halide fused salt under inert atmosphere and vacuum condition to obtain a distilled product; wherein the halides in the halide molten salt are 67 mol% LiF and 33 mol% BeF 2 ；
In the vacuum condition, the vacuum degree is 5-30 Pa;
in the distillation treatment, the distillation temperature and the condensation temperature are respectively 800-1000 ℃ and 500-700 ℃; the temperature difference between the distillation temperature and the condensation temperature is 250-350 ℃,
the oxygen content in the distillation product is below 480 mg/Kg;
the distillation treatment time is 2-5 h;
the treatment capacity of the distillation treatment is 100-400 g;
alternatively, the method for reducing the oxygen content in the halide molten salt comprises the following steps:
distilling the halide molten salt under inert atmosphere and vacuum condition to obtain a distilled product; wherein the halide in the halide molten salt is lithium halide;
in the vacuum condition, the vacuum degree is 5-150 Pa;
in the distillation treatment, the distillation temperature and the condensation temperature are 700-1000 ℃ and 500-800 ℃ respectively; the temperature difference between the distillation temperature and the condensation temperature is 200-350 ℃,
the oxygen content in the distillation product is below 400 mg/Kg;
the distillation treatment time is 0.5-4 h;
the treatment capacity of the distillation treatment is 50-200 g;
alternatively, the method for reducing the oxygen content in the halide molten salt comprises the following steps:
distilling the halide molten salt under inert atmosphere and vacuum condition to obtain a distilled product; wherein the halides in the halide molten salt are 46.5 mol% LiF, 11.5 mol% NaF and 42 mol% KF;
in the vacuum condition, the vacuum degree is 5-30 Pa;
in the distillation treatment, the distillation temperature and the condensation temperature are respectively 800-1000 ℃ and 500-700 ℃; the temperature difference between the distillation temperature and the condensation temperature is 200-350 ℃,
the oxygen content in the distillation product is below 560 mg/Kg;
the distillation treatment time is 0.5-2 h;
the processing amount of the distillation treatment is 50-200 g.
39. A method of reducing the oxygen content in a molten halide salt according to claim 38, wherein the method of reducing the oxygen content in a molten halide salt comprises the steps of:
distilling the halide molten salt under inert atmosphere and vacuum condition to obtain a distilled product; wherein the lithium halide is LiCl or LiF.
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