CN109207128A - A kind of preparation method and applications of high-purity molten chloride - Google Patents
A kind of preparation method and applications of high-purity molten chloride Download PDFInfo
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Abstract
The present invention relates to the preparation methods of high-purity molten chloride, comprising: provides the untreated molten chloride of purity >=95%；The untreated molten chloride is heated to liquid, obtains fused chloride fused salt；It is stood after active metal is added in fused chloride fused salt, make water and oxidative impurities in active metal and untreated molten chloride that redox reaction occur respectively and generates precipitating, active metal includes at least one of lithium, potassium, calcium, sodium, magnesium, aluminium, zinc and iron, and oxidative impurities include OH‑、SO4 2‑、NO3 ‑、PO4 3‑And NO2 ‑At least one of；Remaining solid active metal and the precipitating being filtered to remove in fused chloride fused salt, obtain high-purity molten chloride, wherein the active metal containing dissolution.The invention further relates to the applications of high-purity molten chloride.High-purity molten chloride preparation method provided by the invention is simple, safety, and solves the problems, such as that structural material is perishable in fused salt and restricts molten chloride and applies in industrial-scale.
Description
Technical field
The invention belongs to fused salt fields, and in particular to a kind of preparation method and applications of high-purity molten chloride.
Background technique
Molten chloride is by metal cation and anion (Cl-) what is formed is in the compound of molten state at high temperature.
Molten chloride has wider operating temperature, viscosity low, and electric conductivity is good, and Ion transfer and diffusion rate are higher, specific heat capacity
Height, while the material capabilities such as dissolution metal, nuclear fuel are also equipped with, thus in molten-salt electrolysis, fused salt refining, Molten Salt Electroplating, fuel
Battery, battery, solar energy optical-thermal, molten salt reactor and energy storage field have a wide range of applications.Molten chloride type is more, price just
It preferably, is a kind of very potential high temperature heat transfer heat storage medium.But molten chloride, which easily absorbs water, causes water suction afterchlorinate object molten
Salt has aggressive, causes container material or structural material to generate corrosion and embrittlement, directly affects the peace of equipment or system
Entirely, thus to a certain extent the large-scale application of molten chloride is restricted.
University of Illinois of the U.S. prepares molten chloride using vacuum and high-pure anhydrous HCl, this method reaction time
Long (> 48h), in addition the characteristics such as the low boiling point of HCl gas, volatile, easy to moisture absorption require pipe material harsh.Masschusetts, U.S.A
The Institute of Technology is passed through Cl in fused chloride fused salt2, it is passed through inert atmosphere again later to prepare molten chloride.This method pair
Equipment material requires height, and in addition research discovery is when temperature is raised to 740 DEG C, Cl2Oxidisability can be lost and no longer have purifying chlorine
The ability of compound fused salt.Brookhaven National Laboratory of the U.S. takes in low pressure (< 0.03Torr), vacuum and inert atmosphere
Under the conditions of respectively continuous heating prepare and purification of chlorinated object fused salt.This method clean-up effect is unobvious, and manufacturing cycle is very long
(manufacturing cycle > 48h).U.S.'s Argonne National Laboratory comes fused salt and Cd-Mg alloy under 550~600 DEG C of inert atmosphere
Prepare molten chloride.Cd is a kind of rare metal, and the content in the earth's crust is less, and price is high, and Cd has with its compound
There is certain toxicity, the air harm to the human body polluted by Cd is serious.Fused salt is prepared using the method, it is not only at high cost, and to ring
The health of border and the mankind cause certain harm.Ceskoslovenska Akademie Ved uses CCl4Steam prepares molten chloride,
But this method control is difficult, is easy to pollute the environment.Above method generates greatly limitation to molten chloride application.
Summary of the invention
Complicated for high-purity molten chloride preparation method at present, dangerous and structural material is perishable in fused salt
And molten chloride is restricted the problem of industrial-scale is applied, the present invention provides a kind of preparation method of high-purity molten chloride
And its application.
The preparation method of a kind of high-purity molten chloride provided according to the present invention, comprising the following steps: P1 is provided pure
The untreated molten chloride is heated to liquid by the untreated molten chloride of degree >=95%, P2, and it is molten to obtain fused chloride
Salt；P3 is stood after active metal is added in fused chloride fused salt, so that in the active metal and untreated molten chloride
Water and oxidative impurities occur respectively redox reaction generate precipitating, wherein active metal include lithium, potassium, calcium, sodium, magnesium,
At least one of aluminium, zinc and iron, oxidative impurities include OH-、SO4 2-、NO3 -、PO4 3-And NO2 -At least one of；P4, mistake
Remaining solid active metal and the precipitating in fused chloride fused salt are filtered out, high-purity molten chloride is obtained, wherein should
Active metal containing dissolution in high-purity molten chloride.
The present invention carries out redox reaction using water in active metal and molten chloride and oxidative impurities, to go
Except high-purity molten chloride is made in water and oxidative impurities in molten chloride.The preparation method is simple, safe, using this method
Contain active metal in high-purity molten chloride obtained, external environment can be alleviated to a certain extent to structural material in fused salt
Middle corrupting influence.
Preferably, which includes NaCl, KCl, MgCl2And CaCl2At least one of.
Preferably, P2 specifically: keep constant temperature after untreated molten chloride is heated to the first temperature, continue to heat
Constant temperature is kept after being increased to second temperature, obtains fused chloride fused salt；Wherein, the 100 DEG C≤first untreated chlorination of temperature <
Object fused salt fusing point < second temperature.To remove Free water present in fused salt by way of heating.
Preferably, the retention time of constant temperature at the first temperature is 2-4h.To, allow in fused chloride fused salt from
It is eliminated as much as by water.
Preferably, step P1 includes carrying out testing preceding pretreatment to crucible, is then packed into untreated molten chloride
It is heated in pretreated crucible；The crucible is graphite crucible or corundum crucible.
Preferably, pretreated step before being tested to crucible specifically: cleaned with deionized water, the earthenware that will have been cleaned
Crucible is placed in baking oven and dries to remove its Free water, obtains dry crucible, takes out dry crucible, puts it into covering inertia
In >=700 DEG C of high-temperature calcinations in the high temperature resistance furnace of atmosphere, to remove combination water therein.
Preferably, the time of repose in step P3 is 4-24h.To allow in active metal and fused chloride fused salt
Water or oxidative impurities sufficient redox reaction occurs.
The present invention also provides the application for high-purity molten chloride that above-mentioned preparation method obtains, high-purity molten chloride with
Structural material carries out static corrosion.
High-purity molten chloride preparation method provided by the invention is simple, safety, and solves structural material in fused salt
It is perishable and restrict molten chloride industrial-scale application the problem of.
In short, the preparation method that the present invention provides a kind of high-purity molten chloride overcomes one or more in the prior art
It is insufficient.The preparation method simple process safety, suitable application area simple to operate are wide.The molten chloride prepared using this method
Purity is high, performance stablize that pass heat storage performance good, and the corrosion to structural material can be effectively reduced, can effectively extending structure material make
Use the service life.The preparation method simple possible, easily operated control is at low cost, and safety and environmental protection will not cause damages to human environment.With
Other preparation methods are compared, the high-purity molten chloride short preparation period prepared using this method, simple process safety, operation letter
Just suitable application area is wide for folk prescription, is suitble to the production of extensive molten chloride.The molten chloride purity is high of this method preparation, passes and stores
Hot property is excellent, and can alleviate to a certain extent external environment dissolved with a certain amount of active metal in fused salt and exist to structural material
The influence of fused salt corrosion can significantly reduce the corrosion rate of nickel-base alloy and stainless steel in molten chloride, effectively inhibit
Their grain boundary corrosion improves service life of the stainless steel in molten chloride.Conjunction used in molten chloride is widened
The selection range of gold reduces the manufacture and processing cost of structural material in fused salt practical application, has pushed molten chloride in
The large-scale application in high temperature energy-storage field, academic and engineer application are significant.
Detailed description of the invention
Fig. 1 a is for nickel-base alloy Haynes-230 in embodiment 1 in untreated NaCl-KCl-CaCl under the conditions of 800 DEG C2
SEM photograph in fused salt after static immersing 100h；
Fig. 1 b is for nickel-base alloy Haynes-230 in embodiment 1 in high-purity N aCl-KCl-CaCl under the conditions of 800 DEG C2It is molten
SEM photograph in salt after static immersing 100h；
Fig. 2 a is for 316H stainless steel in embodiment 2 in untreated NaCl-KCl-MgCl under the conditions of 730 DEG C of temperature2Fused salt
SEM photograph after middle static immersing 400h；
Fig. 2 b is for 316H stainless steel in embodiment 2 in high-purity N aCl-KCl-MgCl under the conditions of 730 DEG C of temperature2In fused salt
SEM photograph after static immersing 400h；
Fig. 2 c is for 316 stainless steels in embodiment 2 in untreated NaCl-KCl-MgCl under the conditions of 730 DEG C of temperature2Fused salt
SEM photograph after middle static immersing 400h；
Fig. 2 d is for 316 stainless steels in embodiment 2 in high-purity N aCl-KCl-MgCl under the conditions of 730 DEG C of temperature2It is quiet in fused salt
State impregnates the SEM photograph after 400h.
Specific embodiment
Below in conjunction with attached drawing and a specific embodiment of the invention, technical solution of the present invention is carried out specifically
It is bright, but following examples are only that and cannot limit the present invention to understand the present invention, in the embodiment and embodiment in the present invention
Feature can be combined with each other, the invention can be implmented in many different forms as is defined and embodied by the claims.
Preparation of samples:
Molten chloride is bought, and they are stored in the reagent cabinet of low temperature drying, in case stand-by；
By high temperature resistance furnace debugging to optimum state, it is ensured that its burner hearth, bell clean dried, in case stand-by.Ensure high temperature
The cold water function of resistance furnace works normally and the deionized water of the cooling-water machine is in ordinary water level, in case stand-by；
Ensure electronic balance (precision 0.01g), graphite crucible or corundum crucible, active metal (lithium, potassium, calcium, sodium, magnesium,
Aluminium, zinc, iron), filter screen, dress salt container, crucible tongs, the dried and cleans such as tweezers, in case stand-by.
Embodiment 1
1.1 high-purity N aCl-KCl-CaCl2The preparation characterization of fused salt
A kind of preparation method of the high-purity molten chloride provided according to the present invention, comprising the following steps:
1) crucible pre-processes: graphite crucible deionized water is cleaned 10~15min, repeated washing in ultrasonic instrument
Graphite crucible is three times.Cleaned graphite crucible is placed in baking oven in 100 DEG C of dryings of > to remove its Free water, drying is obtained
Graphite crucible.Take out graphite crucible, put it into covering inert atmosphere high temperature resistance furnace in >=700 DEG C of high-temperature calcinations >=
10h, to remove combination water therein.Spare in glove box, water, oxygen content difference in glove box are stored into after being cooled to room temperature
Less than 5ppm.
2) the untreated chlorate of accurate weighing: NaCl (84.10g), KCl (15.00g) and CaCl2(201.00g) will claim
It has measured chlorate to be uniformly mixed, has formed untreated molten chloride.Untreated molten chloride is packed into pretreated graphite
In crucible, it is placed in the high temperature resistance furnace of covering inert atmosphere.
3) high temperature resistance furnace temperature program(me) is set, untreated molten chloride is heated to 250 DEG C, heats 40min；It is permanent
Temperature is increased to 600 DEG C by 250 DEG C again after warm 120min, heats 60min, 60 min of constant temperature, and then obtain fused chloride
Fused salt.
4) metal Ca is placed in fused chloride fused salt, after standing 4h, fused chloride fused salt is filtered using strainer,
Prepare high-purity molten chloride.In the process, Ca reacts as follows with water generation in fused chloride fused salt: Ca+2H2O=Ca
(OH)2+H2Or Ca+H2O=CaO+H2, to generate precipitating and gas, and then water in fused chloride fused salt is removed.In addition,
Ca occurs redox reaction with oxidative impurities in fused chloride fused salt and generates precipitating, while oxidative impurities being removed.
It is removed using strainer filtering: (1) impurity that untreated molten chloride or crucible itself introduce；(2) water or oxidative impurities
The precipitating generated after reacting with active metal Ca；It (3) is unreacted Ca.
5) high-purity molten chloride is stored in fused salt storage tank, samples after cooling and is ground in glove box.
Table 1 is untreated and high-purity N aCl-KCl-CaCl2Fused salt Positive Ion Content (ug/g)
Table 2 is untreated and high-purity N aCl-KCl-CaCl2Anion-content (ug/g) in fused salt
Using ICP-OES and automatical potentiometric titrimeter to NaCl-KCl-CaCl2It is tested, see Table 1 for details and table 2.From
For table 1 it is found that using impurity content in the molten chloride of this method preparation in ppm magnitude, purity is high-purity grade.In addition, using
Also contain active metal Ca in molten chloride made from this method, sustainable react with water and oxidation impurities of active metal Ca will
It is removed, and then the NaCl-KCl-CaCl of this method preparation2For high-purity grade.
1.2 high-purity and untreated NaCl-KCl-CaCl2The experiment of the static corrosion of fused salt and Haynes-230
1) Haynes-230 is cut into 10mm × 10mm × 2mm size using wire cutting method, by well cutting
Surface is polishing to 2000 mesh with SiC sand paper by Haynes-230 step by step, is successively blown with deionized water and dehydrated alcohol ultrasonic cleaning
It is dry, it is 100 DEG C or more in drying box temperature and dries for 24 hours, obtains Haynes-230 sample.
2) take several crucibles that the untreated chlorination of alumina crucible is added in Haynes-230 sample and molten chloride respectively
Crucible is sealed in object.Above-mentioned assembly and welding process carry out in the glove box of Ar atmosphere protection, and the autoclave body being sealed is put
Enter in Muffle furnace and keeps the temperature 100h in 800 DEG C of constant temperature.
3) sample is cleaned in the glove box of Ar atmosphere protection with deionized water after taking out sample, is seen using scanning electron microscope
Examine the pattern variation of sample corrosion front and back, the microscopic appearance of evaluation corrosion front and back sample.
As shown in Fig. 1 a- Fig. 1 b, Haynes230 sample is 800 DEG C of NaCl-KCl-CaCl in temperature2Corrode in fused salt
After 100h, there is apparent grain boundary corrosion in the Haynes230 in untreated molten chloride, and average corrosion depth is 4 μm.And
Haynes-230 sample is in high-purity N aCl-KCl-CaCl2Fused salt has no signs of corrosion.
Embodiment 2
2.1 high-purity N aCl-KCl-MgCl2The preparation characterization of fused salt
A kind of preparation method of the high-purity molten chloride provided according to the present invention, comprising the following steps:
1) graphite crucible pre-processes: graphite crucible deionized water being cleaned 10~15min in ultrasonic instrument, is repeated
Clean graphite crucible three times.Cleaned graphite crucible is placed in baking oven in 100 DEG C of dryings of > to remove its Free water, is done
Dry graphite crucible.Graphite crucible is taken out, is put it into the high temperature resistance furnace of covering inert atmosphere in >=700 DEG C of high-temperature calcinations
>=10h, to remove combination water therein.Spare in glove box, water, oxygen content point in glove box are stored into after being cooled to room temperature
It little Yu not 5ppm.
2) the non-purified chlorate of accurate weighing: NaCl (65.7g), KCl (55.9g) and MgCl2(178.4g) will be weighed
Chlorate be uniformly mixed, form untreated molten chloride.Untreated molten chloride is packed into pretreated graphite earthenware
In the untreated chloride of crucible, it is placed in the high temperature resistance furnace of covering inert atmosphere.
3) high temperature resistance furnace temperature program(me) is set, untreated molten chloride is heated to 250 DEG C, heats 60min；It is permanent
Temperature is increased to 600 DEG C by 250 DEG C again after warm 240min, heats 80min, constant temperature 60min, and then obtain fused chloride
Fused salt.
4) metal Mg is placed in fused chloride fused salt, after standing for 24 hours, using strainer to fused chloride fused salt mistake
Filter, prepares high-purity molten chloride.In the process, Mg reacts as follows with the water generation in fused chloride fused salt: Mg+2H2O
=Mg (OH)2+H2Or Mg+H2O=MgO+H2, to generate precipitating and gas, and then water in fused chloride fused salt is removed.
In addition, redox reaction occur for oxidative impurities generate to precipitate in Mg and fused chloride fused salt, while by oxidative impurities
Removal.It is removed using strainer filtering: (1) impurity that untreated molten chloride or crucible itself introduce；(2) water or oxidisability
The precipitating that impurity and active metal Mg are generated after reacting；It (3) is unreacted Mg.
5) high-purity molten chloride is stored in fused salt storage tank, samples after cooling and is ground in glove box.
Table 3 is untreated and high-purity N aCl-KCl-MgCl2Fused salt Positive Ion Content (ug/g)
Table 4 is untreated and high-purity N aCl-KCl-MgCl2Anion-content (ug/g) in fused salt
Using ICP-OES and automatical potentiometric titrimeter to NaCl-KCl-MgCl2It is tested, specific value is shown in Table 3 and table
4.As may be known from Table 3 and Table 4, using impurity content in the molten chloride of this method preparation in ppm magnitude, purity is high-purity grade.
In addition, using active metal Mg is also contained in molten chloride made from this method, active metal Mg is sustainable with water and oxidation
Property impurity reaction remove it.
2.2 high-purity and untreated NaCl-KCl-MgCl2The experiment of the static corrosion of fused salt and alloy
1) 316H, 316 stainless steel alloys are cut into the size of the mm of 10mm × 10mm × 2 respectively using wire cutting method,
Surface is polishing to 2000 mesh with SiC sand paper by well cutting sample step by step, is successively cleaned by ultrasonic with deionized water and dehydrated alcohol
Drying is 100 DEG C or more in drying box temperature and dries for 24 hours, obtains alloy corrosion sample.
2) take several crucibles that alumina crucible is added in 316H, 316 stainless steel alloy samples and molten chloride respectively
In and seal.Above-mentioned assembly and welding process carry out in the glove box of Ar atmosphere protection, and seal pot is put into Muffle furnace
400h is kept the temperature in 730 DEG C of constant temperature.
3) sample is cleaned in the glove box of Ar atmosphere protection with deionized water after taking out sample, is seen using scanning electron microscope
Examine the pattern variation of sample corrosion front and back, the microscopic appearance of evaluation corrosion front and back sample.
Fig. 2 a- Fig. 2 d is under the conditions of 730 DEG C of temperature, and 316H and 316 stainless steels are in untreated NaCl-KCl-MgCl2It is molten
Salt (c, e) and high-purity N aCl-KCl-MgCl2Microscopic appearance after fused salt (d, f) static immersing 400h.It can be with from Fig. 2 a- Fig. 2 d
It obtains, 316H stainless steel has obvious grain boundary corrosion in untreated fused salt, and average corrosion depth is 2 μm.In high-purity N aCl-KCl-
MgCl2Surface is smooth in fused salt, has no signs of corrosion.316 stainless steels are in untreated NaCl-KCl-MgCl2Occur in fused salt obvious
Grain boundary corrosion and hole corrode.In high-purity N aCl-KCl-MgCl2316 stainless steel surfaces are smooth in fused salt, no hole and crystal boundary
Corrosion phenomenon.This illustrates high-purity N aCl-KCl-MgCl2It is small to the corrosion of 316 stainless steel alloys, it can slow down to a certain extent pair
The corrosion of 316 stainless steel alloys.
It should be understood that although the untreated molten chloride provided in above-described embodiment is NaCl-KCl-CaCl2Fused salt and
NaCl-KCl-MgCl2Fused salt, but can actually be NaCl, KCl, MgCl2And CaCl2At least one of.Moreover, this is not
Handle molten chloride purity should >=95%, in order to which active metal and water therein and oxidative impurities react,
Oxidative impurities therein include OH-、SO4 2-、 NO3 -、PO4 3-And NO2 -At least one of, this point from table yin from
The reduction of sub- content can obviously be known.
Above-described, only presently preferred embodiments of the present invention, the range being not intended to limit the invention, of the invention is upper
Stating embodiment can also make a variety of changes.Letter made by i.e. all claims and description according to the present invention
Single, equivalent changes and modifications, fall within claims of the invention.The not detailed description of the present invention is conventional skill
Art content.
Claims (8)
1. a kind of preparation method of high-purity molten chloride, which comprises the following steps:
P1 provides the untreated molten chloride of purity >=95%,
The untreated molten chloride is heated to liquid, obtains fused chloride fused salt by P2；
P3 is stood after active metal is added in fused chloride fused salt, so that the active metal and untreated molten chloride
In water and oxidative impurities occur respectively redox reaction generate precipitating, wherein active metal include lithium, potassium, calcium, sodium,
At least one of magnesium, aluminium, zinc and iron, oxidative impurities include OH-、SO4 2-、NO3 -、PO4 3-And NO2 -At least one of；
It is molten to obtain high all-chloride for P4, remaining solid active metal and the precipitating being filtered to remove in fused chloride fused salt
Salt, wherein the active metal containing dissolution in high-purity molten chloride.
2. preparation method according to claim 1, which is characterized in that the untreated molten chloride include NaCl,
KCl、MgCl2And CaCl2At least one of.
3. preparation method according to claim 1, which is characterized in that the P2 specifically: by untreated molten chloride
Constant temperature is kept after being heated to the first temperature, continues to keep constant temperature after heating is increased to second temperature, obtains fused chloride fused salt；
Wherein, the untreated molten chloride fusing point < second temperature of the 100 DEG C≤first temperature <.
4. preparation method according to claim 3, which is characterized in that the retention time of the constant temperature at the first temperature
For 2-4h.
5. preparation method according to claim 1, which is characterized in that the step P1 includes pre- before being tested to crucible
Untreated molten chloride, is then fitted into pretreated crucible and heats by processing；The crucible be graphite crucible or
Corundum crucible.
6. preparation method according to claim 5, which is characterized in that it is described crucible is tested before pretreated step
Specifically: it is cleaned with deionized water, the crucible cleaned is placed in baking oven and is dried to remove its Free water, dry earthenware is obtained
Crucible takes out dry crucible, puts it into >=700 DEG C of high-temperature calcinations in the high temperature resistance furnace of covering inert atmosphere, to remove
Combination water therein.
7. preparation method according to claim 1, which is characterized in that the time of repose in the step P3 is 4-24h.
8. a kind of application for high-purity molten chloride that the preparation method according to any one of right 1-7 obtains, feature
It is, high-purity molten chloride and structural material carry out static corrosion.
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Cited By (6)
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| WO2020168605A1 (en) * | 2019-02-22 | 2020-08-27 | 广州特种承压设备检测研究院 | Modified chloride molten salt, preparation method and application thereof |
| WO2020168604A1 (en) * | 2019-02-22 | 2020-08-27 | 广州特种承压设备检测研究院 | Mixed chloride molten salt having high thermal conductivity, preparation method therefor and application thereof |
| CN113336255A (en) * | 2021-08-05 | 2021-09-03 | 天津包钢稀土研究院有限责任公司 | Purification method of rare earth halide molten salt |
| CN113372886A (en) * | 2021-07-01 | 2021-09-10 | 中国科学院上海应用物理研究所 | Ternary chloride molten salt with high-temperature thermal stability and preparation method thereof |
| CN113732294A (en) * | 2021-09-26 | 2021-12-03 | 中国科学院上海应用物理研究所 | Method for cheap large-scale synthesis of metal clusters through molten salt |
| US11931763B2 (en) | 2019-11-08 | 2024-03-19 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020168605A1 (en) * | 2019-02-22 | 2020-08-27 | 广州特种承压设备检测研究院 | Modified chloride molten salt, preparation method and application thereof |
| WO2020168604A1 (en) * | 2019-02-22 | 2020-08-27 | 广州特种承压设备检测研究院 | Mixed chloride molten salt having high thermal conductivity, preparation method therefor and application thereof |
| US11931763B2 (en) | 2019-11-08 | 2024-03-19 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
| CN113372886A (en) * | 2021-07-01 | 2021-09-10 | 中国科学院上海应用物理研究所 | Ternary chloride molten salt with high-temperature thermal stability and preparation method thereof |
| CN113336255A (en) * | 2021-08-05 | 2021-09-03 | 天津包钢稀土研究院有限责任公司 | Purification method of rare earth halide molten salt |
| CN113336255B (en) * | 2021-08-05 | 2021-10-29 | 天津包钢稀土研究院有限责任公司 | Purification method of rare earth halide molten salt |
| CN113732294A (en) * | 2021-09-26 | 2021-12-03 | 中国科学院上海应用物理研究所 | Method for cheap large-scale synthesis of metal clusters through molten salt |
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