CN106835203A - The purifier and method of a kind of fused salt - Google Patents
The purifier and method of a kind of fused salt Download PDFInfo
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- CN106835203A CN106835203A CN201611218940.3A CN201611218940A CN106835203A CN 106835203 A CN106835203 A CN 106835203A CN 201611218940 A CN201611218940 A CN 201611218940A CN 106835203 A CN106835203 A CN 106835203A
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- storehouse
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- upper lid
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
- C25C3/28—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium of titanium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
Abstract
The invention discloses the purifier and method of a kind of fused salt, the purifier includes the Gas Stirring conduit of electrode storehouse, the reactor with upper lid, crucible and lower end with nozzle；Crucible is placed in reactor；Top cap is connected to fused salt conduit and inert gas/vacuum tube；Upper lid is sealedly connected with liquid metal discharge pipe, cathode mechanism and anode mechanism；Gas Stirring conduit is tightly connected with upper lid, and its lower end passes through upper lid and extends to the lower end of crucible；Electrode storehouse includes anodic gas collecting pipe, negative electrode storehouse and anode storehouse；Anodic gas collecting pipe is tightly connected with upper lid, and lower end connects after passing through upper lid with anode storehouse；Negative electrode storehouse and anode storehouse are placed in the molten salt electrolyte in crucible, are fixedly connected by quartz rod between the two；The upper end in negative electrode storehouse connects with liquid metal discharge pipe.The present invention effectively removes slaine, oxide form impurity in fused salt, and fused salt purification purity is high, can be continuously produced, and then effectively improve the purity of electrolytic titanium.
Description
Technical field
A kind of device the present invention relates to fused salt processing technology field, more particularly to fused salt is purified and method.
Background technology
In common metal, titanium is one of most abundant element of content in the earth's crust, and abundance accounts for the 4th in structural metal,
It is only second to aluminium, iron, magnesium.Titanium is a kind of Rare Metals Materials of superior performance, except superior strength/weight ratio, is suitable as
Beyond space flight spare part, the purposes of many non-space flight is have now been developed, in people such as oil, the energy, traffic, chemical industry, raw doctors
Certain application has also been obtained with field, and its application field is also constantly extending.In recent years, with semiconductor technology, information
The fast development of the high-tech areas such as technology, biomaterial, they to the purity requirement of titanium that is used also more and more higher,
Demand to high purity titanium is also increasing.
The production method of high purity titanium mainly has fused-salt electrolytic refining method, iodide process, electron-beam process.Refined with iodide process
When, speed of separating out is slow, and is intermittent operation, therefore productivity ratio is low.Electron-beam process is to general low-melting-point metal impurity
Element and nonmetalloid C, N, H can remove, but oxygen and heavy metal must use fused salt electrolysis process or iodine before electronic torch melting
Change method is removed.Using fused salt electrolysis process refining titanium not only can effectively remove cause integrated circuit error radioactive element uranium and
Thorium, and produce and can be carried out continuously, productivity ratio is high, and the energy of consumption is small, low production cost.
Fused-salt electrolytic refining prepares the technique of titanium, general to be electrolysed using alkali metal or alkaline-earth halide molten salt system
Matter, electrolyte purity is generally technical pure or analyzes pure, wherein containing certain impurity.During high-temperature electrolysis, metallic impurity elements from
Son such as Fe2+、Cu2+、Ni2+、Cr3+And Mn4+It is metal Deng can be simultaneously reduced electrochemically in negative electrode and titanium ion, significantly reduces
Electrolytic titanium purity.Moisture and metal oxide in electrolyte can pollute electrolytic titanium in molten condition, cause to be electrolysed obtained titanium
Oxygen content raise.
The content of the invention
In view of above-mentioned analysis, an object of the present invention is：A kind of purifier of fused salt is provided, the purifier can
Slaine and oxide form impurity effectively in removal fused salt.
The second object of the present invention is：A kind of purifier method of fused salt is provided, the method can effectively remove fused salt
In slaine and oxide form impurity, so as to improve the purity of electrolytic titanium.
To reach one of above-mentioned purpose, the present invention adopts the following technical scheme that realization：
A kind of purifier of fused salt, the purifier electrode storehouse 11, the reactor 17 with upper lid 6, the and of crucible 16
Gas Stirring conduit 1 of the lower end with nozzle；
The crucible 16 is placed in the reactor 17；
The upper lid 6 is connected with fused salt conduit 2 and inert gas/vacuum tube 3；The lower end of the fused salt conduit 2 passes through institute
State lid 6 and extend to the lower end of the crucible 16；Upper lid 6 described in the lower end of the inert gas/vacuum tube 3 and the reaction
Device 17 is connected；The upper lid 6 is sealedly connected with liquid metal discharge pipe 8, cathode mechanism and anode mechanism；
The lower end of the Gas Stirring conduit 1 passes through the upper lid 6 and extends to the lower end of the crucible 16；
The electrode storehouse 11 includes anodic gas collecting pipe 22, negative electrode storehouse 23 and anode storehouse 24；The anodic gas are collected
Pipe 22 is tightly connected with the upper lid 6, and lower end connects after passing through the upper lid 6 with the anode storehouse 24；The He of negative electrode storehouse 23
Anode storehouse 24 is placed in the molten salt electrolyte 13 in the crucible 16, is fixedly connected by quartz rod 10 between the two；It is described
The upper end in negative electrode storehouse 23 connects with the liquid metal discharge pipe 8；
The negative electrode storehouse 23 and anode storehouse 24 are respectively by the cathode mechanism and the negative pole of anode mechanism and external power supply
Connected with positive pole.
Further, the cathode mechanism includes cathode collector bar 7 and graphite cathode plate 14；The cathode collector bar 7 with it is described
Upper lid 6 is tightly connected, and lower end is connected after passing through the upper lid 6 with the graphite cathode plate 14；The graphite cathode plate 14 is located at
In the negative electrode storehouse 23；
The anode mechanism includes anode rod 9 and graphite anode plate 15；The anode rod 9 is sealed with the upper lid 6
Connection, lower end is connected after passing through the upper lid 6 with the graphite anode plate 15；The graphite anode plate 15 is located at the anode storehouse
In 24；
The surface of the cathode collector bar 7 and anode rod 9 is coated with ceramic insulating layer 25；
Distinguish the negative pole and positive pole of external power supply in the upper end of the cathode collector bar 7 and anode rod 9.
Further, the material of the cathode collector bar 7 and anode rod 9 is nickel；The thickness of the ceramic insulating layer 25 is
10~30 microns.
Further, described being tightly connected is realized using polytetrafluoro insulated enclosure mechanism；
The polytetrafluoro insulated enclosure mechanism includes polytetrafluoro insulated enclosure set 18, arch fastening nut 19, the and of O-ring 20
Stainless steel male-pipe 21；
The stainless steel male-pipe 21 is fixed on the upper lid 6, and extrudes the polytetrafluoro by fastening nut 19
The mode of insulated enclosure set 18 and O-ring 20, is tightly connected with connector；
The connector includes cathode collector bar 7, liquid metal discharge pipe 8, anode rod 9 and anodic gas collecting pipe 22.
Further, the number in the negative electrode storehouse 23 is 2；2 negative electrode storehouses 23 are symmetrically distributed in the two of the anode storehouse 24
Side.
Further, it is additionally provided with inert gas outlet valve 4 on the upper lid 6；The inert gas outlet valve 4 is used to control
Inert gas processed is filled with the flow of the reactor 17.
Further, the material of the reactor 17 and upper lid 6 is 304 stainless steels；The Gas Stirring conduit 1, crucible
16 and fused salt conduit 2 material be nickel；The material in the electrode storehouse 11 is quartz.
To reach the two of above-mentioned purpose, the present invention adopts the following technical scheme that realization：
A kind of purification method of fused salt, the purification method is realized using purifier described above, specifically included：
Step one, in confined conditions, the vacuum valve for opening inert gas/vacuum tube 3 is vacuumized, until reactor 17
Interior absolute pressure≤100Pa, maintains 20~40 minutes；
Step 2, the vacuum valve for closing inert gas/vacuum tube 3, open the gas valve of inert gas/vacuum tube 3
Inert gas is filled with, gas washing is carried out；
After step 3, gas washing, continue to be filled with inert gas, until being 300~800Pa of malleation in reactor 17, heating rises
After warm to 750~800 DEG C, fused salt is imported in crucible 16 along fused salt conduit 2；
Step 4, by the negative electrode storehouse 23 and anode storehouse 24 in electrode storehouse 11 respectively by cathode collector bar 7 and anode rod 9 with it is outer
Positive pole and the negative pole connection of power supply are connect, 5~10A direct currents are passed through, is electrolysed 4~5 hours, liquid metal is arranged by liquid metal
Outlet pipe 8 is discharged, so that the fused salt being obtained after purification；
Step 5, under condition of negative pressure, during the fused salt after purification sucked into electrolytic cell by fused salt conduit 2.
Further, in gas scrubbing, when the pressure in reactor 17 is malleation 10kPa, inert gas outlet is adjusted
Valve 4, controls gas flow, and malleation is between 300~800Pa in maintenance reaction device 17.
Further, step 4 also includes Gas Stirring step, specially：
In electrolytic process, often it is powered 50~70 minutes, inert gas is passed into by reaction by stirring of inert gas conduit 1
The bottom of device 17, is stirred by bubble, and duration of ventilation is 5~15 minutes.
Beneficial effects of the present invention：
1st, the present invention uses electrolysis, effectively removes slaine, oxide form impurity in fused salt, can effectively improve
The purity of electrolytic titanium.
2nd, fused salt of the present invention purification purity is high, with can be continuously produced feature.
Brief description of the drawings
Accompanying drawing is only used for showing the purpose of specific embodiment, and is not considered as limitation of the present invention, in whole accompanying drawing
In, identical reference symbol represents identical part.
Fig. 1 is fused salt purifier structural representation of the invention；
Fig. 2 is electrode chamber structure schematic diagram of the invention；
Fig. 3 is cathode mechanism structural representation of the invention；
Fig. 4 is anode mechanism structural representation of the invention；
Fig. 5 is polytetrafluoro insulated enclosure structural scheme of mechanism of the invention.
In figure：1- Gas Stirrings conduit, 2- fused salts conduit, 3- inert gases/vacuum tube, 4- inert gas outlets valve, 5-
Lid on arch fastener, 6-, 7- cathode collector bars, 8- liquid metals discharge pipe, 9- anode rods, 10- quartz rods, 11- electrodes storehouse,
12- anode gas bubbles (Cl2), 13- molten salt electrolytes, 14- graphite cathodes plate, 15- graphite anodes plate, 16- crucibles, 17- reactors,
18- polytetrafluoro insulated enclosures set, 19- fastening nuts, 20-O types circle, 21- stainless steels male-pipe, 22- anodic gas collecting pipe,
23- negative electrodes storehouse, 24- anodes storehouse, 25- ceramic insulation coating.
Specific embodiment
The preferred embodiments of the present invention are specifically described below in conjunction with the accompanying drawings, wherein, accompanying drawing constitutes the application part, and
It is used to explain principle of the invention together with embodiments of the present invention.
This gives a kind of purifier of fused salt, its structural reference Fig. 1, the purifier includes electrode storehouse
11st, the reactor 17 with upper lid 6, crucible 16 and Gas Stirring conduit 1.
Wherein, crucible 16 is placed in reactor 17, and reactor 17 is sealed using arch fastener 5 with upper lid 6 and fixed.Upper lid
6 are connected with fused salt conduit 2, inert gas/vacuum tube 3 and inert gas outlet valve 4.The lower end of fused salt conduit 2 passes through upper lid 6 simultaneously
Extend to the lower end of crucible 16；The lower end of inert gas/vacuum tube 3 and inert gas outlet valve 4 both passes through lid 6 and reactor
17 connections.Liquid metal discharge pipe 8, cathode mechanism and anode mechanism (unmarked in figure) are sealedly connected with upper lid 6.Gas is stirred
The lower end of conduit 1 is mixed through upper lid 6 and the bottom of crucible 16 is extended to, lower end carries nozzle.
The material in the electrode storehouse 11 of the present embodiment is preferably quartz, its structural reference Fig. 2, including is collected including anodic gas
Pipe 22, negative electrode storehouse 23 and anode storehouse 24.Anodic gas collecting pipe 22 is tightly connected with upper lid 6, lower end through after upper lid 6 with anode
Storehouse 24 connects.The upper end in negative electrode storehouse 23 connects with liquid metal discharge pipe 8.Negative electrode storehouse 23 and anode storehouse 24 are placed in crucible 16
Molten salt electrolyte 13 in, be fixedly connected by quartz rod 10 between the two.The number in the negative electrode storehouse 23 of the present embodiment is 2.2
Negative electrode storehouse 23 is symmetrically distributed in the both sides in anode storehouse 24.Negative electrode storehouse 23 and anode storehouse 24 pass through cathode mechanism and anode mechanism respectively
It is connected with the negative pole and positive pole of external power supply.
Structural reference Fig. 3 of the cathode mechanism of the present embodiment, including cathode collector bar 7 and graphite cathode plate 14.Cathode collector bar 7
It is tightly connected with upper lid 6, lower end is connected after passing through upper lid 6 with graphite cathode plate 14.Graphite cathode plate 14 is located at negative electrode storehouse 23
It is interior.
Structural reference Fig. 4 of the anode mechanism of the present embodiment, including anode rod 9 and graphite anode plate 15.Anode rod 9
It is tightly connected with upper lid 6, lower end is connected through upper lid 6 with graphite anode plate 15.Graphite anode plate 15 is located in anode storehouse 24.
The cathode collector bar 7 of the present embodiment and the upper end of anode rod 9 are connected with the negative pole and positive pole of external power supply respectively, its
Surface is coated with ceramic insulating layer 25, and its thickness is 10~30 microns.
The present embodiment is realized being tightly connected using polytetrafluoro insulated enclosure mechanism (not shown).Polytetrafluoro insulation is close
Sealing mechanism structural reference Fig. 5, including polytetrafluoro insulated enclosure set 18, arch fastening nut 19, O-ring 20 and stainless steel external screw thread
Pipe 21.Stainless steel male-pipe 21 is fixed on the upper lid 6, and extrudes the polytetrafluoro insulated enclosure by fastening nut 19
The mode of set 18 and O-ring 20, is tightly connected with connector.Connector in the present embodiment includes cathode collector bar 7, liquid metal
Discharge pipe 8, anode rod 9 and anodic gas collecting pipe 22.
The reactor 17 of the present embodiment and the material of upper lid 6 are 304 stainless steels.Cathode collector bar 7, anode rod 9, crucible 16
It is nickel with the material of fused salt conduit 2.The material in electrode storehouse 11 is quartz.The fused salt of the present embodiment is halide fused salt, preferably
Molten chloride and fluoride molten salt.
The present embodiment can effectively remove slaine, oxide form impurity in fused salt, so as to effectively improve electricity
Solve the purity of titanium；Fused salt purification purity is high obtained in the present embodiment, with can be continuously produced feature.
Another embodiment gives a kind of purification method of fused salt, and the purification method uses purifier reality described above
Existing, specifically include：
Step one, in confined conditions, the vacuum valve for opening inert gas/vacuum tube 3 is vacuumized, until reactor 17
Interior absolute pressure≤100Pa, maintains 20~40 minutes.
Step 2, the vacuum valve for closing inert gas/vacuum tube 3, open the gas valve of inert gas/vacuum tube 3
Inert gas is filled with, gas washing is carried out.
The number of times of the gas washing in the present embodiment is generally 2~4 times, preferably 3 times.
In order to ensure, while faint malleation can also be maintained, can to prevent outside air from entering full of argon gas in reactor 17.
In gas scrubbing, when in reactor 17 for malleation 10kPa, by adjusting inert gas outlet valve 4, inert gas is controlled
(such as argon gas) flow, malleation is between 300~800Pa in maintenance reaction device 17.
After step 3, gas washing, continue to be filled with inert gas, until the pressure in reactor 17 maintain malleation 300~
800Pa, after being heated to 750~800 DEG C, earthenware is imported by fused salt (such as NaCl, KCl or NaCl-KCl) along fused salt conduit 2
In crucible 16.
Step 4, by the negative electrode storehouse 23 and anode storehouse 24 in electrode storehouse 11 respectively by cathode collector bar 7 and anode rod 9 with it is outer
Positive pole and the negative pole connection of power supply are connect, 5~10A direct currents are passed through, is electrolysed 4~5 hours, liquid metal is arranged by liquid metal
Outlet pipe 8 is discharged, so that the fused salt being obtained after purification.
During often energization 50~70 minutes (preferably 60 minutes) of the present embodiment, argon is passed through by stirring of inert gas conduit 1
Gas agitating 5~15 minutes (preferably 10 minutes), can so ensure that molten salt electrolyte is well mixed, and promote impurity element diffusion.
Gas Stirring conduit 1 is tightly connected with upper lid 6, and its lower end passes through upper lid 6, and extends to the bottom of crucible 16.Gas Stirring conduit 1
End portion carry nozzle, the material of Gas Stirring conduit 1 is preferably nickel.
The fused salt of the present embodiment is generally halide fused salt.Its cleaning principle is：In electrolytic process, alkali metal cation
And foreign metal cation is reduced to metal in negative electrode, alkali metal density is less than molten chloride and with relatively low fusing point,
It is in a liquid state under electrolysis temperature, floats on electrolyte top.Other refractory metal cations obtain electronics and are reduced in negative electrode
Metal, is attached to cathode surface or comes off in negative electrode storehouse.Cl-Electronics is lost in anode, Cl is oxidized to2。Cl2Floating
During be fully contacted with fused salt, the metal impurities oxide in fused salt, hydroxide and Cl2Reaction generation metal chloride
And O2, the metal chloride for being generated migrated to negative electrode, is reduced to metal, so as to realize that fused salt is purified.
Cathode reaction：M2++2e-=M (M represents metallic impurity elements)；
In negative electrode, Na+、K+Metal liquid (based on Liquid Sodium) is reduced to, cathode chamber top, Fe is swum in2+、Cu2+、
Ni2+、Cr3+And Mn4+It is reduced to metal simultaneously and is attached to cathode surface or comes off in quartz cathode orlop Deng metal impurities ion
Portion.
Anode electrochemical reacts：
2Cl-=Cl2+2e-
Chemical reaction：2MO+2Cl2=2MCl2+O2↑ (M represents metallic impurity elements)
4AOH+2Cl2=2H2O↑+4ACl+O2↑ (A represents alkali metal or alkaline-earth metal)
In anode, Cl-Electronics is lost, Cl is oxidized to2。Cl2It is fully contacted with fused salt during floating, in fused salt
Metal impurities oxide, hydroxide and Cl2Reaction generation metal chloride and O2, the metal chloride for being generated migrate to
Negative electrode, is reduced to metal, so as to realize that fused salt is purified.
Step 5, under condition of negative pressure, the fused salt after purification is sucked in electrolytic cell or derived by fused salt conduit 2.
After the completion of electrolytic cleaning, during the halide fused salt after purification sucked into electrolytic cell by fused salt conduit 2 using negative pressure
Or derive.In order to prevent outside air from entering, during salt discharge, enough inert gases are passed through always (such as in reactor 17
Argon gas).
Embodiment 1：
1st, in confined conditions, the vacuum valve for opening inert gas/vacuum tube 3 is vacuumized, until in reactor 17
Absolute pressure is 50Pa, and the vacuum valve of inert gas/vacuum tube 3 is closed after maintaining 30 minutes, opens inert gas/vacuum tube
3 gas valve is filled with argon gas, is repeated 2 times, and completes gas washing.
2nd, continue to be filled with argon gas, until the pressure in reactor 17 maintains malleation 300Pa, after being heated to 800 DEG C,
NaCl fused salts are imported in crucible 16 along fused salt conduit 2.
3rd, the negative electrode storehouse 23 and anode storehouse 24 in electrode storehouse 11 are passed through into cathode collector bar 7 and anode rod 9 and external electricity respectively
Positive pole and the negative pole connection in source, are passed through 5A direct currents, are electrolysed 4 hours,
Often it is powered 50 minutes, being passed through argon gas by stirring of inert gas conduit 1 carries out Gas Stirring 5 minutes.
4th, the fused salt after purification is sucked in electrolytic cell or is derived by fused salt conduit 2 using negative pressure.
Through purity analysis, purity reaches 99.99% to molten salt electrolyte after purification, and oxygen content is 60ppm.
Embodiment 2：
The present embodiment is substantially the same manner as Example 1, and difference is：
1st, the absolute pressure in the excessively middle reactor 17 of gas washing is 100Pa, is maintained 40 minutes, is repeated 3 times.
2nd, fused salt is KCl, and normal pressure of the fused salt in reactor 17 is 800Pa, and temperature is 750 DEG C of importings.
3rd, electric current is 10A direct currents, is often powered 70 minutes, Gas Stirring 15 minutes.
Through purity analysis, purity reaches 99.985% to molten salt electrolyte after purification, and oxygen content is 70ppm.
Embodiment 3：
The present embodiment is substantially the same manner as Example 1, and difference is：
1st, the absolute pressure in the excessively middle reactor 17 of gas washing is 30Pa, is maintained 30 minutes, is repeated 5 times.
2nd, fused salt is NaCl-KCl, and normal pressure of the fused salt in reactor 17 is 600Pa, and temperature is 780 DEG C of importings.
3rd, electric current is 7A direct currents, is often powered 60 minutes, Gas Stirring 10 minutes.
Through purity analysis, purity reaches 99.995% to molten salt electrolyte after purification, and oxygen content is 40ppm.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
Should all be included within the scope of the present invention.
Claims (10)
1. a kind of purifier of fused salt, it is characterised in that the purifier electrode storehouse (11), the reaction with upper lid (6)
The Gas Stirring conduit (1) of device (17), crucible (16) and lower end with nozzle；
The crucible (16) is placed in the reactor (17)；
The upper lid (6) is connected with fused salt conduit (2) and inert gas/vacuum tube (3)；Wear the lower end of the fused salt conduit (2)
Cross the upper lid (6) and extend to the lower end of the crucible (16)；The lower end of the inert gas/vacuum tube (3) is described in
Upper lid (6) connects with the reactor (17)；The upper lid (6) be sealedly connected with liquid metal discharge pipe (8), cathode mechanism and
Anode mechanism；
The lower end of the Gas Stirring conduit (1) passes through the upper lid (6) and extends to the lower end of the crucible (16)；
The electrode storehouse (11) includes anodic gas collecting pipe (22), negative electrode storehouse (23) and anode storehouse (24)；The anodic gas
Collecting pipe (22) is tightly connected with the upper lid (6), and lower end connects after passing through the upper lid (6) with the anode storehouse (24)；Institute
State negative electrode storehouse (23) and anode storehouse (24) are placed in the molten salt electrolyte (13) in the crucible (16), between the two by stone
English bar (10) is fixedly connected；The upper end of the negative electrode storehouse (23) connects with the liquid metal discharge pipe (8)；
The negative electrode storehouse (23) and anode storehouse (24) are respectively by the cathode mechanism and the negative pole of anode mechanism and external power supply
Connected with positive pole.
2. purifier according to claim 1, it is characterised in that the cathode mechanism includes cathode collector bar (7) and stone
Black minus plate (14)；The cathode collector bar (7) is tightly connected with the upper lid (6), lower end through after the upper lid (6) with it is described
Graphite cathode plate (14) is connected；The graphite cathode plate (14) is in the negative electrode storehouse (23)；
The anode mechanism includes anode rod (9) and graphite anode plate (15)；The anode rod (9) and the upper lid (6)
It is tightly connected, lower end is connected after passing through the upper lid (6) with the graphite anode plate (15)；The graphite anode plate (15) is located at
In the anode storehouse (24)；
The surface of the cathode collector bar (7) and anode rod (9) is coated with ceramic insulating layer (25)；
Distinguish the negative pole and positive pole of external power supply in the upper end of the cathode collector bar (7) and anode rod (9).
3. purifier according to claim 2, it is characterised in that the material of the cathode collector bar (7) and anode rod (9)
Expect to be nickel；The thickness of the ceramic insulating layer (25) is 10~30 microns.
4. purifier according to claim 1 and 2, it is characterised in that described being tightly connected is insulated using polytetrafluoro
What sealing mechanism was realized；
The polytetrafluoro insulated enclosure mechanism includes polytetrafluoro insulated enclosure set (18), arch fastening nut (19), O-ring (20)
With stainless steel male-pipe (21)；
The stainless steel male-pipe (21) is fixed on the upper lid (6), and extrudes described poly- four by fastening nut (19)
The mode of fluorine insulated enclosure set (18) and O-ring (20), is tightly connected with connector；
The connector includes cathode collector bar (7), liquid metal discharge pipe (8), anode rod (9) and anodic gas collecting pipe
(22)。
5. purifier according to claim 1 and 2, it is characterised in that the number of the negative electrode storehouse (23) is 2；2 the moon
Pole storehouse (23) is symmetrically distributed in the both sides of the anode storehouse (24).
6. purifier according to claim 1 and 2, it is characterised in that be additionally provided with inert gas on the upper lid (6)
Outlet valve (4)；The inert gas outlet valve (4) is for controlling inert gas to be filled with the flow of the reactor (17).
7. purifier according to claim 1, it is characterised in that the material of the reactor (17) and upper lid (6) is
304 stainless steels；The material of the Gas Stirring conduit (1), crucible (16) and fused salt conduit (2) is nickel；The electrode storehouse (11)
Material for quartz.
8. a kind of purification method of fused salt, it is characterised in that the purification method is using any one of claim 1-7
What purifier was realized, specifically include：
Step one, in confined conditions, the vacuum valve for opening inert gas/vacuum tube (3) is vacuumized, until reactor (17)
Interior absolute pressure≤100Pa, maintains 20~40 minutes；
Step 2, the vacuum valve for closing inert gas/vacuum tube (3), open the gas valve of inert gas/vacuum tube (3)
Inert gas is filled with, gas washing is carried out；
After step 3, gas washing, continue to be filled with inert gas, until the pressure in reactor (17) is 300~800Pa of malleation, plus
After heat is warming up to 750~800 DEG C, fused salt is imported in crucible (16) along fused salt conduit (2)；
Step 4, by the negative electrode storehouse (23) and anode storehouse (24) of electrode storehouse (11) respectively pass through cathode collector bar (7) and anode rod
(9) it is connected with the positive pole and negative pole of external power supply, is passed through 5~10A direct currents, be electrolysed 4~5 hours, liquid metal is passed through into liquid
State metal discharge pipe (8) is discharged, so that the fused salt being obtained after purification；
Step 5, under condition of negative pressure, by the fused salt after purification by fused salt conduit (2) suck electrolytic cell.
9. purification method according to claim 8, it is characterised in that in gas scrubbing, the pressure in reactor (17)
During for malleation 10kPa, inert gas outlet valve (4) is adjusted, control gas flow, the malleation in maintenance reaction device (17) is 300
Between~800Pa.
10. purification method according to claim 8 or claim 9, it is characterised in that step 4 also includes Gas Stirring step, tool
Body is：
In electrolytic process, often it is powered 50~70 minutes, inert gas is passed into by reactor by stirring of inert gas conduit 1
(17) bottom, is stirred by bubble, and duration of ventilation is 5~15 minutes.
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| CN201611218940.3A CN106835203B (en) | 2016-12-26 | 2016-12-26 | A kind of purification device and method of fused salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611218940.3A CN106835203B (en) | 2016-12-26 | 2016-12-26 | A kind of purification device and method of fused salt |
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| CN106835203B CN106835203B (en) | 2019-05-31 |
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| CN109440139A (en) * | 2018-11-30 | 2019-03-08 | 中国工程物理研究院材料研究所 | A kind of double cup type ceramic crucibles and preparation method thereof for molten salt electrolysis of metals refining |
| CN110042434A (en) * | 2018-01-15 | 2019-07-23 | 中国科学院上海应用物理研究所 | Reaction unit and its operation method for molten salt system uranium fluorination reaction |
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| CN111172563A (en) * | 2020-02-25 | 2020-05-19 | 中南大学 | Method and device for electrolyzing antimony sulfide-containing material by using molten salt |
| CN111876793A (en) * | 2020-07-16 | 2020-11-03 | 江西理工大学 | Method for purifying dysprosium-copper alloy by liquid cathode in molten salt system |
| CN113603059A (en) * | 2021-07-12 | 2021-11-05 | 中国科学院上海应用物理研究所 | Molten salt, electrochemical purification method of molten salt and electrochemical device |
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| CN110042434A (en) * | 2018-01-15 | 2019-07-23 | 中国科学院上海应用物理研究所 | Reaction unit and its operation method for molten salt system uranium fluorination reaction |
| CN110042434B (en) * | 2018-01-15 | 2024-04-12 | 中国科学院上海应用物理研究所 | Reaction device for uranium fluorination reaction of molten salt system and operation method thereof |
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| CN110079834A (en) * | 2019-06-10 | 2019-08-02 | 永嘉县纳海川科技有限公司 | A kind of fused salt electrolysis apparatus and its application method for rare earth metal preparation |
| CN111172563A (en) * | 2020-02-25 | 2020-05-19 | 中南大学 | Method and device for electrolyzing antimony sulfide-containing material by using molten salt |
| CN111876793A (en) * | 2020-07-16 | 2020-11-03 | 江西理工大学 | Method for purifying dysprosium-copper alloy by liquid cathode in molten salt system |
| CN113603059A (en) * | 2021-07-12 | 2021-11-05 | 中国科学院上海应用物理研究所 | Molten salt, electrochemical purification method of molten salt and electrochemical device |
| CN113603059B (en) * | 2021-07-12 | 2022-11-29 | 中国科学院上海应用物理研究所 | Molten salt, electrochemical purification method of molten salt and electrochemical device |
| CN115762834A (en) * | 2022-12-01 | 2023-03-07 | 中国原子能科学研究院 | Molten salt purification device and molten salt purification method |
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