CN106621429B - The method and distilling apparatus of closed distillation fused salt - Google Patents

The method and distilling apparatus of closed distillation fused salt Download PDF

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CN106621429B
CN106621429B CN201510427482.3A CN201510427482A CN106621429B CN 106621429 B CN106621429 B CN 106621429B CN 201510427482 A CN201510427482 A CN 201510427482A CN 106621429 B CN106621429 B CN 106621429B
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distillation
flange
collection
crucible
baculum
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CN106621429A (en
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杨洋
窦强
付海英
王子豪
耿俊霞
李晴暖
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Shanghai Institute of Applied Physics of CAS
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Shanghai Institute of Applied Physics of CAS
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Abstract

The invention discloses the methods and distilling apparatus of a kind of closed distillation fused salt, this method is realized by a kind of distilling apparatus, distilling apparatus includes distillation still, airtight cavity is formed in the distillation still, the left end of the airtight cavity is evaporating area, and top, the bottom of the right-hand end of the airtight cavity are respectively condensing zone and collecting region.The present invention increases due to the vapour pressure of fused salt with temperature raising, it is heated under conditions of closed and the different parts of cooling vacuum distillation still can form biggish vapour pressure gradient to drive fused salt to distill, the shortcomings that overcoming the low prior art rate of recovery, product dispersion, pollution and corrosion of the fused salt for vacuum system are effectively prevented, product recoveries are improved.

Description

The method and distilling apparatus of closed distillation fused salt
Technical field
The present invention relates to the methods and distilling apparatus of a kind of closed distillation fused salt.
Background technique
Fused salt is molten mass composed by metal cation and metalloid anion.It common are alkali or alkaline earth metal Halide, silicate, carbonate, nitrate and phosphate.Fused salt has good high-temperature stability, in wide temperature range The characteristics such as interior low-vapor pressure, low viscosity, good electric conductivity and high heat capacity, can be used as the electrolysis of electroextraction metal Matter and the fuel solvent and the heat transfer medium that are used as fusedsalt reactor in nuclear industry etc..
The distillation of fused salt is to utilize the volatility difference between supporting electrolyte and fission product, corrosion product, Lai Shixian carrier The recycling of fused salt and the removal of impurity.The temperature as needed for evaporation fused salt is very high (generally 800 DEG C~1200 DEG C), Er Qierong Salt vapour pressure is very low, such as LiF, and vapour pressure is only 70Pa at 1000 DEG C.Therefore, it is necessary at higher temperature and vacuum degree Fused salt is distilled, impurity is separated.
Meanwhile needing ceaselessly to be evacuated in the common vacuum distillation method course of work to maintain the vacuum degree in distillation still, Drive fused salt evaporation, condensation.Such distillation mode can accelerate the distillation of fused salt, improve distilling rate.But due to part Condensation collection system can be discharged in salt with pumping, so that the rate of recovery of fused salt is not usually high, and product disperses, while salt fog can It can enter vacuum system to pollute and corrode.
Summary of the invention
The technical problem to be solved by the present invention is in order to overcome it is in the prior art it is traditional overcome it is traditional in the prior art Fused salt distillating method in the fused salt rate of recovery is low, product dispersion, more, the easy to pollute and corrosion vacuum system of loss of material etc. lack It falls into, the method and distilling apparatus of a kind of closed distillation fused salt is provided.
The present invention is to solve above-mentioned technical problem by following technical proposals:
A kind of method of closed distillation fused salt, it is characterized in that, use a distilling apparatus to realize, the distilling apparatus packet Distillation still is included, an airtight cavity is formed in the distillation still, the left end of the airtight cavity is evaporating area, the airtight cavity Top, the bottom of right-hand end are respectively condensing zone and collecting region, the distilling apparatus further include: the evaporation being set in the evaporating area Crucible, the collection crucible being set in the collecting region and the cooling device being set in the collection crucible, this method specifically include Following steps:
S1, airtight cavity is vacuumized, while opening cooling device;
S2, temperature of the heating fused salt to be evaporated to needed for melting;
S3, be reduced to 10 when the intracorporal vacuum degree of the closed chamber-2Pa-10-4When Pa, the closed airtight cavity simultaneously stops to this Airtight cavity vacuumizes;
S4, when continuing the temperature in heating evaporation area to 900 DEG C -1000 DEG C, while adjusting the temperature of the condensing zone lower than should The temperature of evaporating area, by cooling so that the temperature of flange baculum and collection baculum is lower than 100 DEG C;
S5, distillation process judged by the intracorporal air pressure change of closed chamber.
In the present solution, heating process vacuumizes, vacuum pump is out of service when distillation starts, and vacuum is formed in distillation still Airtight cavity, since the vapour pressure of fused salt increases as temperature increases, the different parts of heating and cooling distillation still, and make With kettle internal cooling system, biggish temperature gradient is formed, to form biggish vapour pressure gradient driving fused salt distillation.
Meanwhile air pressure changes as the evaporation and condensation of fused salt are continuous in airtight cavity, since airtight cavity can not be intuitive Judgement distill process, can by the air pressure of airtight cavity and temperature judgement distillation terminal, consequently facilitating judge whether need Heater power source is closed, so as to avoid the waste of the energy.
The present invention also provides a kind of distilling apparatus, including distillation still, it is formed with an airtight cavity in the distillation still, this is close The left end of closed chamber body is evaporating area, and top, the bottom of the right-hand end of the airtight cavity are respectively condensing zone and collecting region, Feature is, the distilling apparatus further include:
Evaporator crucible, for placing fused salt to be evaporated, and the evaporator crucible is set in the evaporating area;
Crucible is collected, for collecting through pervaporation and condensed fused salt, which is set in the collecting region, and It is extended in the condensing zone at the top of the collection crucible;
Cooling device is set in the collection crucible and reduces the temperature of the collection crucible neighboring area for being passed through coolant Degree.
In the present solution, collection device and cooling device structure setting form so that by water cooling realize condensing zone in Cool, while increasing the condensation area of salt steam, increase the temperature gradient of airtight cavity, improve the distillation of salt Rate helps to improve the collection rate of high-temperature molten salt vacuum distillation, improves product recoveries.
Preferably, the distillation still includes:
Shell is distilled, the evaporator crucible is provided in the distillation shell, and the shape of the distillation shell is in " 7 font ";
Upper flange extends radially outwardly from the outer surface of the bottom of the distillation shell;
Lower flange, be removably attachable to the bottom end of the upper flange and with the upper flange be tightly connected, and the lower flange with The upper flange, distillation shell are provided with the collection crucible around the airtight cavity is formed on the lower flange.
In the present solution, form using the above structure, so that the evaporating area of high temperature is located at the most remote areas far from lower flange. The temperature of flange is further decreased using water cooling simultaneously, realizes the room temperature sealing of upper flange and lower flange, air-tightness is up to standard.Together When, there is bigger temperature gradient compared to the distillation shell of vertically or horizontally shape using the distillation shell of " 7 font ".
Preferably, the middle part of the lower flange is equipped with a flange baculum, this is extended at the top of the flange baculum In condensing zone, it is formed with a chamber resettling in the flange baculum, the cooling device is equipped in the chamber resettling;
The collection crucible is cylinder, and the bottom of the collection crucible is equipped with hollow collection baculum, and the collection is rodlike Protrusion is sleeved on the outer surface of the flange baculum, and the bottom of the collection baculum is located in the collecting region, the collection It is extended at the top of baculum in the condensing zone.
It is being linked in the outer surface of flange baculum in the present solution, collecting baculum and can be adjacent to, flange is rodlike prominent Internal logical circulating coolant is played, collection baculum can be cooled down, meanwhile, the design for collecting baculum increases salt steam Condensation area increases the temperature gradient of airtight cavity, improves the distilling rate of salt.
Preferably, being provided with wedge-shape diversion plate on inner wall on the right side of the distillation shell, the bottom end of the wedge-shape diversion plate is goed deep into In the collection crucible, the exhaust tube being connected with the collecting region, and the pumping are provided in the one side wall of the bottom of the distillation shell Tracheae is located at the lower section of the wedge-shape diversion plate.
In the present solution, distillation shell lower end be connected with for be evacuated with the pipeline of air inlet, before distillation starts to cavity into Row pumping, starts closing when distillation, airtight cavity can be made to keep condition of high vacuum degree while high temperature.Meanwhile exhaust tube is set It sets below deflector, bleeding point is covered by wedge-shape diversion plate and the side wall for collecting crucible, prevents salt steam from flowing into exhaust tube.
Preferably, the outer surface of the distillation shell is equipped at least two heaters, the covering of the wherein at least one heater In outside the evaporating area, and at least another heater is covered in outside the condensing zone.
In the present solution, using subsection heater.Can be sectional temperature-controlled, so that airtight cavity is capable of forming biggish temperature Spend gradient.
Preferably, the distillation shell, collection crucible, wedge-shape diversion plate, upper flange and lower flange are closed by refractory metal Golden material is made.
In the present solution, the distilling apparatus of form using the above structure, high temperature resistant, high intensity and material out-gassing rate are low, Be conducive to obtain higher vacuum degree and temperature.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention Example.
The positive effect of the present invention is that:
The present invention is condensed using cooling device, is overcome existing by heating distillation fused salt in the airtight cavity of vacuum The shortcomings that technology rate of recovery is low, product disperses, effectively prevents pollution and corrosion of the fused salt for vacuum system, improves product The rate of recovery.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the distilling apparatus of present pre-ferred embodiments.
Description of symbols:
Distillation still: 1
Distill shell: 11 upper flanges: 12 lower flanges: 13
Flange baculum: 131 chamber resettling: 132 evaporating areas: 14
Condensing zone: 15 collecting regions: 16 O-rings: 17
Bleeding point: 18 exhaust tubes: 19
Resistance heater: 2,3,4
Insulating layer: 5
Evaporator crucible: 6
Collection crucible: 7
Collect baculum: 71 annular horizontal portions: 72 annular vertical portions: 73
Annular collection chamber: 74
Cooling device: 8
Wedge-shape diversion plate: 9
Specific embodiment
A preferred embodiment is named, and completely illustrates the present invention in conjunction with attached drawing to become apparent from.
In the description of the present invention, it is to be understood that, term " on ", "lower", "front", "rear", "left", "right", " perpendicular Directly ", the orientation or positional relationship of the instructions such as "horizontal", "top", "bottom" "inner", "outside" is orientation based on the figure or position Relationship is merely for convenience of description of the present invention and simplification of the description, rather than the device or element of indication or suggestion meaning must have There is specific orientation, be constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
Fig. 1 shows a kind of distilling apparatus, which includes distillation still 1, is formed with a closed chamber in the distillation still 1 Body.The left end of the airtight cavity is evaporating area 14, and top, the bottom of the right-hand end of the airtight cavity are respectively condensing zone 15 With collecting region 16.
Wherein, which includes: distillation shell 11, upper flange 12 and lower flange 13.The shape of the distillation shell 11 is in " 7 font ".Meanwhile left and right two parts of the distillation shell 11 are cylinder, the top surface of the distillation shell 11 is track type.And The distillation shell 11 is formed with the evaporating area 14, condensing zone 15 and collecting region 16.The wall thickness of the distillation shell 11 is 12mm.
Certainly, in the actual use process, which is located at the horizontal component of " 7 font ", condensing zone 15 and receipts Collection area 16 is located at the top and bottom of the vertical portion of " 7 font ".Enable in this way the airtight cavity evaporate simultaneously with it is cold Solidifying fused salt, and biggish temperature gradient can be formed in evaporating area 14 and condensing zone 15, improve the recovery efficiency of fused salt.
In addition, upper flange 12 extends radially outwardly from the outer surface of the bottom of the distillation shell 11;Lower flange 13 passes through spiral shell Bolt is removably attachable to the bottom end of the upper flange 12 and is tightly connected with the upper flange 12.And the lower flange 13 and the upper flange 12, distillation shell 11, which surrounds, is formed with the airtight cavity.It is located at the evaporating area 14 of high temperature far from lower flange 13 most Far region.The temperature of flange is further decreased using water cooling simultaneously, realizes the room temperature sealing of upper flange 12 and lower flange 13, it is airtight Property is up to standard.
In the present embodiment, it is tightly connected between upper flange and lower flange by an O-ring 17, and the material of the O-ring 17 Matter is metal.Make to be metal sealing between upper flange and lower flange in this way, because metal sealing leak rate is 10-10Pa.L/s, from And improve the leakproofness of airtight cavity.
In addition, offering an exhaust tube 19 in the one side wall of the bottom of the distillation shell 11.It uses one end of the exhaust tube 19 Yu Yuyi vacuum pump is connected, and is disposed with vacuum meter and valve on the exhaust tube 19, before distillation starts to cavity into Row pumping, starts closing when distillation, airtight cavity can be made to keep condition of high vacuum degree while high temperature.And vacuum meter is convenient for real The person of testing observes the intracorporal pressure of closed chamber, consequently facilitating judging whether evaporation terminates.
Further, the outer surface of the distillation shell is set there are three concatenated resistance heater 2,3,4, wherein first electricity Resistance heater 2 is covered in outside the evaporating area 14, and second resistance heater 3 is covered in outside the condensing zone 15, and third should Resistance heater 4 is covered in outside the collecting region 16.In the present embodiment, a heat preservation is provided with outside those resistance heaters 2,3,4 Layer 5.
Please understood according to Fig. 1, the distilling apparatus further include: evaporator crucible 6 collects crucible 7 and cooling device.Evaporation Crucible 6 is for placing fused salt to be evaporated, and the evaporator crucible 6 is set in the evaporating area 14.In the present embodiment, evaporator crucible 6 be cylinder.And evaporator crucible 6 can be picked and placed by opening lower flange 13, convenient disassembly.The cooling device is water cooling tube.
Wherein, crucible 7 is collected for collecting through pervaporation and condensed fused salt, which is set to the collection In area 16, and the top of the collection crucible 7 extends in the condensing zone 15.The setting of the collection crucible is convenient for collection liquid state Fused salt.
In addition, the middle part of the lower flange 13 is equipped with a flange baculum 131, the top of the flange baculum 131 is prolonged It extends in the condensing zone 15.A chamber resettling 132 is formed in the flange baculum 131, it is cold which is equipped with this But device 8, and the top of the cooling device 8 extends to the top of the chamber resettling 132.In the actual use process, the stick Shape protrusion 131 is cylinder hollow club shaped structure.And the cooling device plugs in the baculum 131 at the middle part of the lower flange 13 Portion.
Meanwhile the collection crucible 7 is cylinder, and the bottom of the collection crucible is equipped with a hollow collection baculum 71, which is sleeved on the outer surface of the flange baculum 131, and the bottom position of the collection baculum 71 In in the collecting region 16, the top of the collection baculum 71 is extended in the condensing zone 15.
In the present embodiment, the outer surface for being linked in flange baculum 131, flange can be adjacent to by collecting baculum 71 Lead to circulating coolant inside baculum 131, can cool down and collect baculum 71, meanwhile, collect the design of baculum 71 The condensation area for increasing salt steam increases the temperature gradient of airtight cavity, improves the distilling rate of salt.
Wherein, which includes: annular horizontal portion 72 and annular vertical portion 73.The inner circumferential in the annular horizontal portion 72 Edge is welded in the outer surface of the bottom of the collection baculum 71;The annular vertical portion 73 is set to the outer of the annular horizontal portion 72 Periphery and extending axially upward along the collection baculum 71, and the annular vertical portion 73 and the collection baculum 71 is outer An annular collection chamber 74 is formed between surface.
Further, it is provided with wedge-shape diversion plate 9 on the inner wall of the bottom of the distillation shell 11, the wedge-shape diversion plate 9 Bottom end is goed deep into the annular collection chamber 74, and exhaust tube 19 is located at the lower section of the wedge-shape diversion plate 9.Exhaust tube 19 is arranged in water conservancy diversion Below plate, bleeding point 18 is covered by wedge-shape diversion plate 9 and the side wall for collecting crucible, prevents salt steam from flowing into exhaust tube 19.
Further, the distillation shell 11, evaporator crucible 6, collect crucible 7, wedge-shape diversion plate 9, upper flange 12 and under Flange 13 is made of metal alloy compositions.
In use, the evaporator crucible 6 equipped with fused salt to be evaporated is put into the steaming of airtight cavity from lower ending opening Send out in area 14, will collect after crucible and lower flange 13 assemble and be put into the collecting region 16 of airtight cavity, by lower flange 13 with it is upper The sealing of flange 12 installs.Bleeding point 18 is sequentially connected valve, vent valve, filter and vacuum pump.
The present invention also provides a kind of methods of closed distillation fused salt, use distilling apparatus as described above, the party Method specifically includes the following steps:
Step 100 closes valve, vent valve, opens vacuum pump.
Step 101 is slowly opened the valve and is opened to maximum, the intracorporal gas of the closed chamber is discharged, when this is closed When the intracorporal vacuum degree of chamber is reduced to 10Pa or less, cooling device is opened.Lower flange 13 can be cooled down in this way and is collected rodlike prominent Play 71.
Step 102 opens heater power source, heats temperature (such as 600 DEG C) of the fused salt to be evaporated to needed for melting.Its In, during heating, vacuum pump works always.
Step 103 is reduced to 10 when the intracorporal vacuum degree of the closed chamber-2Pa-10-4When Pa, the valve is successively closed, it is close It closes the airtight cavity and closes the vacuum pump.
Step 104, when continuing to heat the temperature of the evaporating area 14 to 900 DEG C -1000 DEG C, meanwhile, adjust the condensing zone 15 Temperature be lower than the evaporating area 14 temperature, by water cooling make flange baculum 131 and collect baculum 71 temperature Lower than 100 DEG C.
In the actual use process, when the temperature of the evaporating area 14 is heated to 1000 DEG C simultaneously, the condensing zone is adjusted 15 temperature is lower than 1000 DEG C, the formation temperature gradient inside airtight cavity.Through supercooling, makes lower flange 13 and collect rodlike prominent The temperature for playing 71 is lower than 100 DEG C, and the leak rate of lower flange 13 is lower than 10-7Pa.L/s.Evaporation of the fused salt in vacuum and high temperature in this way Area 14 is evaporated, and since 15 temperature of condensing zone is lower, the vapour pressure of salt is relatively low, therefore low temperature cold coagulation zone will be flowed into after steam generation 15 and 71 surface condensation of collection baculum at middle part collect.
Air pressure changes as the evaporation and condensation of fused salt are continuous in airtight cavity, since airtight cavity can not intuitively judge Distillation process, can be by the Origin And Destination of the air pressure of airtight cavity and temperature judgement distillation, consequently facilitating judging whether to need Heater power source is closed, so as to avoid the waste of the energy.
In conclusion the present invention distills fused salt by heating in the airtight cavity of vacuum, and use improved cooling Device condensation overcomes the shortcomings that prior art rate of recovery is low, product disperses, effectively prevents dirt of the fused salt for vacuum system Dye and corrosion, improve product recoveries.
Although specific embodiments of the present invention have been described above, it will be appreciated by those of skill in the art that this is only For example, protection scope of the present invention is to be defined by the appended claims.Those skilled in the art without departing substantially from Under the premise of the principle and substance of the present invention, many changes and modifications may be made, but these change and Modification each falls within protection scope of the present invention.

Claims (5)

1. a kind of method of closed distillation fused salt, which is characterized in that it uses a distilling apparatus to realize, which includes Distillation still, an airtight cavity is formed in the distillation still, and the left end of the airtight cavity is evaporating area, the right side of the airtight cavity Top, the bottom of side end are respectively condensing zone and collecting region, the distilling apparatus further include: the evaporation earthenware being set in the evaporating area Crucible, the collection crucible being set in the collecting region and the cooling device being set in the collection crucible;
The distillation still includes:
Shell is distilled, the evaporator crucible is provided in the distillation shell, and the shape of the distillation shell is in " 7 font ", the distillation Wedge-shape diversion plate is provided on inner wall on the right side of shell, the bottom end of the wedge-shape diversion plate is protruded into the collection crucible, the distillation shell The exhaust tube being connected with the collecting region is provided in the one side wall of the bottom of body, and the exhaust tube is located at the wedge-shape diversion plate Lower section;
Upper flange extends radially outwardly from the outer surface of the bottom of the distillation shell;
Lower flange is removably attachable to the bottom end of the upper flange and is tightly connected with the upper flange, and on the lower flange and this Flange, distillation shell are provided with the collection crucible around the airtight cavity is formed on the lower flange;
The middle part of the lower flange is equipped with a flange baculum, extends in the condensing zone at the top of the flange baculum;
The bottom of the collection crucible is equipped with hollow collection baculum, which is sleeved on the flange baculum Outer surface, and the bottom of the collection baculum is located in the collecting region, and it is cold to extend to this at the top of the collection baculum In coagulation zone;
This method specifically includes the following steps:
S1, airtight cavity is vacuumized, while opening cooling device;
S2, temperature of the heating fused salt to be evaporated to needed for melting;
S3, be reduced to 10 when the intracorporal vacuum degree of the closed chamber-2Pa-10-4When Pa, the closed airtight cavity simultaneously stops closed to this Cavity vacuumizes;
S4, when continuing the temperature in heating evaporation area to 900 DEG C -1000 DEG C, while adjusting the temperature of the condensing zone lower than the evaporating area Temperature, by cooling so that flange baculum and collecting the temperature of baculum and being lower than 100 DEG C;
S5, distillation process judged by the intracorporal air pressure change of closed chamber.
2. a kind of distilling apparatus, including distillation still, an airtight cavity, the left end of the airtight cavity are formed in the distillation still For evaporating area, top, the bottom of the right-hand end of the airtight cavity are respectively condensing zone and collecting region, which is characterized in that the distillation Device further include:
Evaporator crucible, for placing fused salt to be evaporated, and the evaporator crucible is set in the evaporating area;
Crucible is collected, for collecting through pervaporation and condensed fused salt, which is set in the collecting region, and the receipts It is extended in the condensing zone at the top of collection crucible;
Cooling device is set in the collection crucible and reduces the temperature of the collection crucible neighboring area for being passed through coolant;
The distillation still includes:
Shell is distilled, the evaporator crucible is provided in the distillation shell, and the shape of the distillation shell is in " 7 font ", the distillation Wedge-shape diversion plate is provided on inner wall on the right side of shell, the bottom end of the wedge-shape diversion plate is protruded into the collection crucible, the distillation shell The exhaust tube being connected with the collecting region is provided in the one side wall of the bottom of body, and the exhaust tube is located at the wedge-shape diversion plate Lower section;
Upper flange extends radially outwardly from the outer surface of the bottom of the distillation shell;
Lower flange is removably attachable to the bottom end of the upper flange and is tightly connected with the upper flange, and on the lower flange and this Flange, distillation shell are provided with the collection crucible around the airtight cavity is formed on the lower flange;
The middle part of the lower flange is equipped with a flange baculum, extends in the condensing zone at the top of the flange baculum, should It is formed with a chamber resettling in flange baculum, the cooling device is equipped in the chamber resettling.
3. distilling apparatus as claimed in claim 2, which is characterized in that the collection crucible is cylinder, the bottom of the collection crucible Portion is equipped with hollow collection baculum, which is sleeved on the outer surface of the flange baculum, and the collection The bottom of baculum is located in the collecting region, extends in the condensing zone at the top of the collection baculum.
4. distilling apparatus as claimed in claim 2 or claim 3, which is characterized in that the outer surface of the distillation shell is equipped at least two Heater, the wherein at least one heater are covered in outside the evaporating area, and at least to be covered in this cold for another heater Outside coagulation zone.
5. distilling apparatus as claimed in claim 2 or claim 3, which is characterized in that the distillation shell, collect crucible, wedge-shape diversion plate, Upper flange and lower flange are made of refractory metal alloy material.
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WO2021092401A1 (en) 2019-11-08 2021-05-14 Abilene Christian University Identifying and quantifying components in a high-melting-point liquid
CN111249761B (en) * 2020-03-04 2022-01-28 中国科学院上海应用物理研究所 Molten salt distillation purification method and equipment
CN113444895B (en) * 2020-03-27 2023-06-30 核工业理化工程研究院 Alkaline metal evaporation and filtration device and method
CN111485113B (en) * 2020-04-16 2021-09-14 中国原子能科学研究院 Alkali metal impurity pretreatment device
CN112891973B (en) * 2021-01-15 2022-09-13 中国科学院上海应用物理研究所 Method for reducing oxygen content in halide molten salt

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US4584015A (en) * 1983-09-26 1986-04-22 Fried. Krupp Gesellschaft Mit Beschrankter Haftung Process and system for the production of very pure alloys
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