CN107419297B - A kind of fused-salt bath producing rare earth metal and alloy - Google Patents
A kind of fused-salt bath producing rare earth metal and alloy Download PDFInfo
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- CN107419297B CN107419297B CN201710687074.0A CN201710687074A CN107419297B CN 107419297 B CN107419297 B CN 107419297B CN 201710687074 A CN201710687074 A CN 201710687074A CN 107419297 B CN107419297 B CN 107419297B
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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
- C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts
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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
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
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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
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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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
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
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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
- C25C7/06—Operating or servicing
Abstract
Rare earth metal synthesis device technical field of the present invention, specifically disclose a kind of fused-salt bath for producing rare earth metal and alloy, including electrolytic cell ontology, electrolytic cell ontology ecto-entad is disposed with shell, insulating layer and solution tank, closing cap is covered with above electrolytic cell ontology, closing cap bottom is provided with first anode plate, cathode plate and second plate plate, cathode plate is slidably connected at closing cap bottom, exhaust outlet there are two being opened up on closing cap, two exhaust ports are provided with air extractor, the first chlorine density tester is additionally provided on closing cap, second chlorine density tester, the driving device of controller and driving cathode plate sliding.It is the production rare earth metal of raw material and the preparation process of alloy device of the invention is mainly intended for anhydrous rare-earth chlorination, in electrolytic process, the position between electrode is adjustable, and the gas for being electrolysed generation can be discharged in time, improves electrolytic efficiency.
Description
Technical field
The invention belongs to rare earth metal synthesis device technical fields, and in particular to a kind of to produce the molten of rare earth metal and alloy
Salt electrolytic cell.
Background technique
For common problem present in China's Rare earth metal metallurgy technology, equipment, managed with melten salt electriochemistry, high-temperature fusant
Based on, fused-salt bath made of the principle and technical research of the subjects such as integrated use computer, chemistry, material and molten
Salt electrolysis method is that domestic and international common production mixing and single rare earth metal are rare earth metal production equipment and method at present, makes
Electrolyte system includes two kinds of rare earth-iron-boron electrolyte (RECl-KCl) and rare earth oxide electrolyte (REO-REF3)
Common system.
In the prior art, Chinese patent CN 202157124U discloses a kind of electrolytic tank for electrolyzing fused salt, including bracket,
The devices such as groove body, sealing cover, cathode, anode, the diaphragm on bracket are placed in, which is easy to connect and be easy between having electrode
The advantages of replacing electrode, but the distance between electrode is non-adjustable, with the continuous accumulation of metal and electrode surface bubble, if
The distance between electrode is too small, non-adjustable, is easy to cause bubble not to be discharged in time, will affect electrolytic efficiency.
Summary of the invention
A kind of fused-salt bath producing rare earth metal and alloy provided by the invention, the distance between electrode is adjustable, solution
The distance between prior art electrode of having determined is too small, non-adjustable, is easy to cause bubble not to be discharged in time, influences electrolytic efficiency
Problem.
The object of the present invention is to provide a kind of fused-salt bath for producing rare earth metal and alloy, including electrolytic cell ontology,
The electrolytic cell ontology ecto-entad is disposed with shell, insulating layer and solution tank, is covered with above the electrolytic cell ontology
Closing cap, the closing cap bottom are successively spaced from left to right and are arranged in parallel with first anode plate, cathode plate and second plate
Plate, and the cathode plate is slidably connected at the closing cap bottom, and can be in the first anode plate and the second plate plate
Between move, opened up on the closing cap there are two exhaust outlet, two exhaust ports are provided with air extractor, the envelope
It closes to cover and is additionally provided with the first chlorine density tester, the second chlorine density tester, controller and drives the cathode plate sliding
Dynamic driving device, the probe of the first chlorine density tester are set across the closing cap and close to the first anode plate
It sets, the probe of the second chlorine density tester is arranged across the closing cap and close to the second plate plate, the controller
It is electrically connected respectively with the first chlorine density tester, the second chlorine density tester, driving device and two air extractors.
Preferably, the shell two sides are respectively equipped with inlet and liquid outlet, and the outer wall around the solution tank is equipped with
The pipeline to interweave in length and breadth is connected between adjacent pipeline, and all pipelines are discharged by the same liquid outlet, and by same
One inlet is intake, and is filled with thermal insulation material in the gap and the insulating layer between adjacent pipeline.
Preferably, the bottom of the closing cap is provided with the sliding rail vertical with the first anode plate, the cathode plate
Upper end is arranged with protective case, and the protective case is slidably connected with the sliding rail, and the driving device is connect with the protective case, uses
In the driving cathode plate sliding.
Preferably, the driving device is stepper motor, and one end of the stepper motor is connect with the protective case, another
End is electrically connected with the controller.
Preferably, the shell is iron-clad.
Preferably, the first anode plate, cathode plate and second plate plate are shapes and sizes comb plate, comb joint all the same,
And the position of comb teeth is opposite one by one.
Preferably, the air extractor is exhaust fan.
Preferably, the hull outside, be provided with refrigerating plant at the inlet, control is provided on the refrigerating plant
Warm device.
Compared with prior art, a kind of fused-salt bath for producing rare earth metal and alloy that this practical invention provides, tool
Have it is following the utility model has the advantages that
1, being mainly used for anhydrous rare-earth chlorination is the production rare earth metal of raw material and the preparation process of alloy, electrolytic process
In, the position between electrode is adjustable, and the gas for being electrolysed generation can be discharged in time, improves electrolytic efficiency；Exhaust fan takes chlorine away
While gas, air pressure is reduced in solution tank, is also further promoted chlorine to overflow from electrolyte and is shed.
2, by the way that the pipeline to interweave in length and breadth is arranged, thermal insulating material is filled in the gap and insulating layer between adjacent pipeline
Material, when electrolysis, thermal insulation material plays the role of insulation, at the end of electrolysis, is passed through coolant liquid by pipeline, accelerates molten
The cooling of substance in liquid bath is convenient for operating in next step.
3, the setting of refrigerating plant and temperature regulating device is kept away so that can be passed through high temperature coolant or cooling gas at the beginning
It is excessive to exempt from solution tank internal-external temperature difference, opens refrigerating plant, gradually decreases coolant liquid or cooling gas temperature, so that it is cold to reach cooling
But the effect of solution tank.
4, first anode plate, cathode plate and second plate plate are shapes and sizes comb plate, comb joint all the same, and comb teeth
Position is opposite one by one, increases the contact area between each electrode and electrolyte, improves electrolytic efficiency, and is conducive to gas row
Out.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the fused-salt bath of present invention production rare earth metal and alloy；
Fig. 2 is the connection signal of cathode plate and closing cap in the fused-salt bath of present invention production rare earth metal and alloy
Figure；
Fig. 3 is the connection schematic diagram of pipeline and solution tank in the fused-salt bath of present invention production rare earth metal and alloy；
Fig. 4 is the structural schematic diagram of first anode plate in the fused-salt bath of present invention production rare earth metal and alloy.
Description of symbols: 1. shells, 11. inlets, 12. liquid outlets, 2. insulating layers, 21. pipelines, 3. solution tanks, 4.
Closing cap, 41. first anode plates, 42. cathode plates, 421. protective cases, 43. second plate plates, 44. exhaust outlets, 45. pumping dresses
It sets, 5. first chlorine density testers, 51. second chlorine density testers, 6. controller, 7. driving device, 71. sliding rails.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings, but should not be construed as limit of the invention
System.The test method of actual conditions is not specified in the following example, operates usually according to normal condition.Unless otherwise defined, originally
All technical and scientific terms used in invention are identical as the normally understood meaning of those skilled in the art of the present technique.
The present invention provides a kind of fused-salt bath for producing rare earth metal and alloy, specific as shown in Figs 1-4, including electrolysis
Slot ontology, electrolytic cell ontology ecto-entad are disposed with shell 1, insulating layer 2 and solution tank 3, and solution tank 3 is by fireproof high-temperature resistant
Steel are made, such as No. 314 steel, and 1 two sides of shell are respectively equipped with inlet 11 and liquid outlet 12, and the outer wall around solution tank 3 is spread
It equipped with the pipeline 21 to interweave in length and breadth, is connected between adjacent pipeline 21, all pipelines 21 are gone out by the same liquid outlet 12
Water, and intake by the same inlet 11, thermal insulating material is filled in the gap and insulating layer 2 between adjacent pipeline 21
Material.Thermal insulation material is the thermal insulation materials such as refractory brick, ceramic alumina fiber.
It is covered with closing cap 4 above electrolytic cell ontology, 4 bottom of closing cap is successively spaced from left to right and is arranged in parallel with the
One anode plate 41, cathode plate 42 and second plate plate 43, first anode plate 41 and second plate plate 43 are mounted on 4 bottom of closing cap
Connector sleeve, connector sleeve and 4 bottom spiral shell of closing cap are enclosed with outside the upper end of portion, first anode plate 41 and second plate plate 43
It connecing, cathode plate 42 is slidably connected at 4 bottom of closing cap, and can move between first anode plate 41 and second plate plate 43, with
Change cathode plate 42 and the distance between first anode plate 41 and second plate plate 43, opens up that there are two exhaust outlets on closing cap 4
44, one of exhaust outlet 44 is located at 41 surface center of first anode plate, another exhaust outlet 44 is located at second plate plate 43
Surface center is provided with air extractor 45 at two exhaust outlets 44, the first chlorine density measurement is additionally provided on closing cap 4
5 (FIX800-Cl of instrument2Online chlorine gas detector, Wan An enlightening company), 51 (FIX800-Cl of the second chlorine density tester2
Online chlorine gas detector, Wan An enlightening company), the driving device 7 slided of controller 6 and driving cathode plate 42, and the
The probe of one chlorine density tester 5 is arranged across closing cap 4 and close to first anode plate 41, the second chlorine density tester 51
Probe be arranged across closing cap 4 and close to second plate plate 43, probe and first anode plate 41 or second plate plate 43 it
Between distance be 2-10mm, controller respectively with the first chlorine density tester 5, the second chlorine density tester 51, driving fill
Set 7 and two electrical connections of air extractors 45.
It should be noted that the bottom of closing cap 4 is provided with the sliding rail 71 vertical with first anode plate 41, cathode plate 42
Upper end is arranged with protective case 421, and protective case 421 is slidably connected with sliding rail 71, and driving device 7 is connect with protective case 421, for driving
Dynamic cathode plate 42 slides.
Driving device 7 is stepper motor, and one end of stepper motor is connect with protective case 421, for driving cathode plate 42 sliding
Dynamic, the other end is electrically connected with controller 6.Stepper motor uses the stepper motor of displacement of the lines.
Air extractor 45 is exhaust fan.The refrigerating plants such as compressor are provided at external, the close inlet 11 of shell 1.
It is raw material that the fused-salt bath of production rare earth metal and alloy of the invention, which is mainly used for anhydrous rare-earth chlorination,
The preparation process of rare earth metal and alloy is produced, places appropriate electrolyte, first anode plate according to actual needs in solution tank 3
41, cathode plate 42 and second plate plate 43 immerse in electrolyte, the electricity of first anode plate 41, cathode plate 42 and second plate plate 43
Pole interface is all set in 4 top of closing cap.It drives cathode plate 42 close to first anode plate 41 by stepper motor first, exists in this way
Under electric field action, since the move distance of ion is short, the chlorine that first anode plate 41 generates is more, when adjacent with first anode plate 41
When the first close chlorine density tester 5 detects that chlorine reaches a certain concentration, controller is transmitted a signal to, at this moment controller
Controlling stepper motor drives cathode plate 42 mobile to second plate plate 43, and the chlorine generated on such second plate plate 43 gradually increases
More, at the same time, the air extractor 45 that controller controls close first anode plate 41 takes what first anode plate 41 nearby generated away
Chlorine guarantees there is good contact area between first anode plate 41 and electrolyte；When neighbouring with second plate plate 43
When dichloro air tightness tester 51 detects that chlorine reaches a certain concentration, controller is transmitted a signal to, at this moment controller controls
Stepper motor drives cathode plate 42 mobile to first anode plate 41, and the chlorine generated on such first anode plate 41 gradually increases,
At the same time, controller controls the chlorine for taking the generation nearby of second plate plate 43 away close to the air extractor 45 of second plate plate 43
Gas guarantees there is good contact area between second plate plate 43 and electrolyte.Looping back and forth like this terminates up to being electrolysed, electricity
In solution preocess, the position between electrode is adjustable, and the gas for being electrolysed generation can be discharged in time, improves electrolytic efficiency.
While exhaust fan takes chlorine away, air pressure is reduced in solution tank 3, is also further promoted chlorine to overflow from electrolyte and is dissipated
Out.
In addition, be equipped with the pipeline 21 to interweave in length and breadth around the outer wall of solution tank 3, the gap between adjacent pipeline 21 with
And thermal insulation material is filled in insulating layer 2.When electrolysis, thermal insulation material plays the role of insulation, at the end of electrolysis, leads to
Piping 21 is passed through coolant liquid, accelerates the cooling of substance in solution tank 3, is convenient for operating in next step, steel can be used in pipeline 21
The preparation of the heat proof materials such as pipe, ceramic tube.Since pipeline 21 is bonded with solution tank 3, gap is very small, gap≤2mm, central filler
Thermal insulation material, avoid pipeline 21 from directly contacting with solution tank 3, on the one hand can obstruct partial heat, it is on the other hand again unlikely
In blocking cooling effect.
The refrigerating plants such as compressor are provided at external, the close inlet 11 of shell 1, temperature control dress is provided on refrigerating plant
Set, temperature regulating device includes the first singlechip of temperature sensor, 51 serial model No.s, first singlechip respectively with temperature sensor and
Refrigerating plant electrical connection, for controlling the opening and closing of refrigerating plant, being passed through high temperature coolant at the beginning, (water, water steam
Vapour) or cooling gas (inert gases such as vapor, nitrogen, helium), it avoids 3 internal-external temperature difference of solution tank excessive, opens refrigeration
Device gradually decreases coolant liquid or cooling gas temperature, to achieve the effect that cooling down solution tank 3.
It should be noted that second singlechip of the controller 6 using 51 serial model No.s, shell 1 is iron-clad, these materials
Material easily obtains, and at low cost.
It should be noted that the driving devices such as stepper motor, electric wire, controller, exhaust fan etc. are with heat-insulated, heat-resisting, resistance to
The materials such as ceramic alumina fiber, refractory brick, the asbestos of high temperature package, prevents the abrasion of these components.
It should be noted that first anode plate 41, cathode plate 42 and second plate plate 43 are that shapes and sizes are all the same
Comb plate, comb joint, and the position of comb teeth is opposite one by one.And first anode plate 41 and second plate plate 43 are graphite anode plate, cathode plate
42 be molybdenum cathode plate.The contact area between each electrode and electrolyte is increased, electrolytic efficiency is improved, and is conducive to gas row
Out.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. a kind of fused-salt bath for producing rare earth metal and alloy, which is characterized in that including electrolytic cell ontology, the electrolytic cell
Ontology ecto-entad is disposed with shell (1), insulating layer (2) and solution tank (3), is covered with envelope above the electrolytic cell ontology
It closes lid (4), closing cap (4) bottom is successively spaced from left to right and is arranged in parallel with first anode plate (41), cathode plate
(42) and second plate plate (43), and the cathode plate (42) is slidably connected at the closing cap (4) bottom, and can be described
It moves, opens up on the closing cap (4) there are two exhaust outlet (44) between one anode plate (41) and the second plate plate (43),
It is provided with air extractor (45) at two exhaust outlets (44), is additionally provided with the first chlorine density on the closing cap (4)
The driving device of tester (5), the second chlorine density tester (51), controller (6) and driving cathode plate (42) sliding
(7), the bottom of the closing cap (4) is provided with the sliding rail (71) vertical with first anode plate (41), the cathode plate
(42) upper end is arranged with protective case (421), and the protective case (421) is slidably connected with the sliding rail (71), the driving dress
It sets (7) to connect with the protective case (421), for driving the cathode plate (42) to slide；The first chlorine density tester
(5) probe is arranged across the closing cap (4) and close to the first anode plate (41), the second chlorine density tester (51)
Probe be arranged across the closing cap (4) and close to the second plate plate (43), the controller is respectively with described first
Chlorine density tester (5), the second chlorine density tester (51), driving device (7) and two air extractor (45) electrical connections.
2. the fused-salt bath of production rare earth metal according to claim 1 and alloy, which is characterized in that the shell
(1) two sides are respectively equipped with inlet (11) and liquid outlet (12), and the outer wall around the solution tank (3) is equipped with to interweave in length and breadth
Pipeline (21), adjacent pipeline are connected between (21), and all pipelines (21) are discharged by the same liquid outlet (12), and
It is intake by the same inlet (11), filled with guarantor in the gap and the insulating layer (2) between adjacent pipeline (21)
Adiabator.
3. the fused-salt bath of production rare earth metal according to claim 1 and alloy, which is characterized in that the driving dress
Setting (7) is stepper motor, and one end of the stepper motor is connect with the protective case (421), the other end and the controller (6)
Electrical connection.
4. the fused-salt bath of production rare earth metal according to claim 1 and alloy, which is characterized in that the shell
It (1) is iron-clad.
5. the fused-salt bath of production rare earth metal according to claim 1 and alloy, which is characterized in that first sun
Pole plate (41), cathode plate (42) and second plate plate (43) are shapes and sizes comb plate, comb joint all the same, and the position of comb teeth
It is opposite one by one.
6. the fused-salt bath of production rare earth metal according to claim 1 and alloy, which is characterized in that the pumping dress
Setting (45) is exhaust fan.
7. the fused-salt bath of production rare earth metal according to claim 1 and alloy, which is characterized in that the shell
(1) it is provided with refrigerating plant at external, close inlet (11), is provided with temperature regulating device on the refrigerating plant.
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| CN201710687074.0A CN107419297B (en) | 2017-08-11 | 2017-08-11 | A kind of fused-salt bath producing rare earth metal and alloy |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710687074.0A CN107419297B (en) | 2017-08-11 | 2017-08-11 | A kind of fused-salt bath producing rare earth metal and alloy |
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| CN107419297B true CN107419297B (en) | 2019-01-08 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2298263Y (en) * | 1997-03-12 | 1998-11-25 | 石富 | Electric tank |
| CN202465911U (en) * | 2012-03-14 | 2012-10-03 | 江西南方稀土高技术股份有限公司 | 25KA fluorosilicate rare earth fused salt electrolytic bath |
| CN103502511A (en) * | 2011-09-28 | 2014-01-08 | 吉坤日矿日石金属株式会社 | Process for producing high -purity lanthanum, high-purity lanthanum, sputtering target comprising high-purity lanthanum, and metal gate film comprising high-purity lanthanum as main component |
-
2017
- 2017-08-11 CN CN201710687074.0A patent/CN107419297B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2298263Y (en) * | 1997-03-12 | 1998-11-25 | 石富 | Electric tank |
| CN103502511A (en) * | 2011-09-28 | 2014-01-08 | 吉坤日矿日石金属株式会社 | Process for producing high -purity lanthanum, high-purity lanthanum, sputtering target comprising high-purity lanthanum, and metal gate film comprising high-purity lanthanum as main component |
| CN202465911U (en) * | 2012-03-14 | 2012-10-03 | 江西南方稀土高技术股份有限公司 | 25KA fluorosilicate rare earth fused salt electrolytic bath |
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| CN107419297A (en) | 2017-12-01 |
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