CN115449853A - Up-inserted special-shaped electrode and method for preparing rare earth metal by molten salt electrolysis of up-inserted special-shaped electrode - Google Patents
Up-inserted special-shaped electrode and method for preparing rare earth metal by molten salt electrolysis of up-inserted special-shaped electrode Download PDFInfo
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- CN115449853A CN115449853A CN202210919532.XA CN202210919532A CN115449853A CN 115449853 A CN115449853 A CN 115449853A CN 202210919532 A CN202210919532 A CN 202210919532A CN 115449853 A CN115449853 A CN 115449853A
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- 150000003839 salts Chemical class 0.000 title claims abstract description 38
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 30
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 17
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 11
- 206010066054 Dysmorphism Diseases 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000003575 carbonaceous material Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- 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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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The utility model provides an on insert formula dysmorphism electrode and fused salt electrolysis preparation rare earth metal's method, belongs to rare earth fused salt electrolysis field, goes up formula of inserting dysmorphism electrode, including going up formula of inserting negative pole and the formula of inserting positive pole, one or two kinds in going up formula of inserting negative pole and the formula of inserting positive pole set to the formula of inserting dysmorphism electrode for the polar distance between the two satisfies: (1) the polar distance of the molten salt liquid surface is larger than the polar distance inside the molten salt; and (2) the distance between the polar distances is 5-80 cm. During electrolysis, the cathode is inserted into the center of the electrolytic cell from the upper part of the electrolytic cell, the anode is inserted into the periphery of the electrolytic cell from the upper part of the electrolytic cell around the cathode, and through the matching of the shapes of the cathode and the anode, the polar distance of the fused salt surface is large, the polar distance inside the fused salt is small, so that the current distribution inside the fused salt is increased, the surface current of the fused salt is weakened, the chemical reaction at the three-phase interface is weakened, and the service life and the electrolytic current efficiency of the anode can be improved.
Description
Technical Field
The invention belongs to the field of rare earth molten salt electrolysis, and particularly relates to an upward-inserted special-shaped electrode and a method for preparing rare earth metal by molten salt electrolysis.
Background
Rare earth metals are widely used. Part of rare earth metals, especially light rare earth metals, are produced by a molten salt electrolysis method. The existing rare earth electrolytic cell is an upward-inserted cathode electrolytic cell, namely, a cathode is inserted into the middle of the electrolytic cell from the upper part of the electrolytic cell, and an anode is inserted into the periphery of the electrolytic cell from the upper part of the electrolytic cell. The existing cathode is a cylindrical cathode, and the existing anode is a cuboid anode or an arc anode. The current efficiency of the upper-inserted cathode electrolytic cell with the structure is low and is generally between 60 and 75 percent. In addition, the anode scrap rate is high, the anode is positioned at a gas-liquid-solid three-phase interface in the area of the surface of the fused salt, and the anode in the area is quickly consumed under the combined action of electrochemical reaction, chemical reaction and mechanical washing. In order to avoid the anode from breaking off and falling off, the anode needs to be replaced when other areas of the anode are not seriously consumed, so that the anode scrap rate is increased.
The patent CN202626314U, CN 1033970350A, CN209162215U invent a structure in which the anode is thick at the upper part (part of the anode at the three-phase interface) and thin at the lower part, that is, the polar distance is small at the molten salt liquid level and the polar distance inside the molten salt is large, but reducing the polar distance near the liquid level will reduce the current efficiency. Patent CN207685375U discloses a cathode with a liquid collecting channel and a liquid conveying channel, which can improve the current efficiency to a certain extent, but the cathode structure is complex and the cost is high. Patent CN208685078U discloses an anode structure capable of prolonging the service life of a trough graphite crucible, but cannot improve the current efficiency and the service life of the anode.
Disclosure of Invention
Aiming at the defects, the invention provides an upward-inserted special-shaped electrode and a method for preparing rare earth metal by molten salt electrolysis. The polar distance (the distance between the cathode and the anode) is an important parameter in the rare earth electrolysis process, and directly influences the current efficiency and the energy consumption. According to the invention, the variable-pole-distance electrolysis is formed by changing the shapes of the cathode and the anode, so that the pole distance at the surface of the fused salt is large, the pole distance in the fused salt is small, the current distribution in the fused salt is further increased, the surface current of the fused salt is weakened, the chemical reaction at a three-phase interface is weakened, and the variable-pole-distance electrolysis is different from the conventional equal-pole-distance electrolysis process, and the service life of the anode and the electrolysis current efficiency can be obviously improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention discloses an upward-inserting type special-shaped electrode, which comprises an upward-inserting type cathode and an upward-inserting type anode, wherein one or two of the upward-inserting type cathode and the upward-inserting type anode are arranged into the upward-inserting type special-shaped electrode, so that the polar distance between the upward-inserting type cathode and the upward-inserting type anode meets the following requirements: (1) the polar distance of the molten salt liquid surface is greater than the polar distance inside the molten salt; and (2) the distance between the poles is 5-80 cm.
More preferably: when the upper inserting type cathode is a cylindrical cathode, the upper inserting type anode adopts a special-shaped anode; when the upper inserting type anode is a cuboid anode or an arc anode, the upper inserting type cathode adopts a special-shaped cathode.
When the special-shaped anode or the special-shaped cathode is adopted, the electrode polar distance in the electrolytic cell is satisfied with the distance between the electrode and the surface of the molten salt and the distance between the electrode and the inside of the molten salt.
The cross section shape of the special-shaped anode along the horizontal direction plane comprises but is not limited to one of a quadrangle and a circular ring, and the cross section shape along the vertical direction comprises but is not limited to one of a trapezoid, a triangle, an L shape and a step shape with a narrow top and a wide bottom, and the trapezoid and the L shape are preferred.
The sectional shape of the special-shaped cathode along the horizontal direction surface comprises but is not limited to one of a circle, a triangle, a quadrangle and a polygon, and the sectional shape along the vertical direction comprises but is not limited to one of a trapezoid, a soil character shape, a convex character shape and a step shape with a narrow upper part and a wide lower part.
Wherein, the material selected by the upper inserted cathode comprises but is not limited to one of tungsten, molybdenum and carbon material; materials selected for the upper-inserted anode include, but are not limited to, carbon materials.
The polar distance between the upper-inserted cathode and the upper-inserted anode is between 5cm and 80cm.
The utility model provides a method of fused salt electrolysis preparation rare earth metal, adopts above-mentioned formula of inserting dysmorphism electrode on, goes up the formula of inserting negative pole and inserts the electrolysis trough center by electrolysis trough upper portion, goes up the formula of inserting positive pole and inserts around the electrolysis trough by electrolysis trough upper portion around the formula of inserting negative pole, carries out fused salt electrolysis preparation rare earth metal, and electrolysis trough current efficiency is greater than 80%, and when using the formula of inserting dysmorphism positive pole on, with traditional positive pole ratio, the electrode utilization ratio improves more than 10%, and the life of the formula of inserting positive pole that goes up improves more than 10%.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
(1) The current efficiency can be greatly improved, the current efficiency is between 80% and 95%, the average current efficiency is more than 80%, and the energy consumption of products in unit mass is further reduced;
(2) The service life of the anode can be prolonged, and the anode scrap rate is reduced; because the polar distance on the surface of the fused salt is large and the polar distance in the fused salt is small, the consumption of the interface is reduced, and the service life of the whole anode is prolonged.
Drawings
FIG. 1 is a schematic horizontal cross-sectional view of a shaped cathode; the shape of (a) is round, (b) is isosceles triangle, (c) is square, (d) is rhombus, (e) is hexagon;
FIG. 2 is a schematic vertical cross-sectional view of a shaped cathode; the structure comprises (a) a trapezoid, (b) a soil character, (c) a convex character, (d) a combination of the trapezoid and the convex character, and (e) a step shape;
FIG. 3 is a schematic horizontal cross-sectional view of a shaped anode; the (a) is a quadrangle, and the (b) is a circular ring;
FIG. 4 is a schematic vertical cross-sectional view of a shaped anode; the structure comprises (a) a trapezoid, (b) a right-angled triangle, (c) an L-shaped structure, and (d) a step-shaped structure.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
An upper-inserted special-shaped electrode comprises an upper-inserted cathode and an upper-inserted anode, wherein the upper-inserted anode is the upper-inserted special-shaped anode, the cross section of the upper-inserted anode along the horizontal direction is circular (shown in figure 3), the cross section of the upper-inserted anode along the vertical direction is L-shaped (shown in figure 4), and carbon materials are adopted; the adopted cathode is a traditional cylindrical cathode, and the adopted material is a tungsten material; go up the formula of inserting negative pole and insert the electrolysis trough center by electrolysis trough upper portion, go up the formula of inserting dysmorphism positive pole and insert around the electrolysis trough is inserted by electrolysis trough upper portion around last formula negative pole, go up the formula of inserting negative pole and go up the utmost point distance between the formula of inserting dysmorphism positive pole and satisfy: (1) the polar distance of the molten salt liquid surface is larger than the polar distance inside the molten salt; and (2) the distance between the polar distances is 5-15 cm. The method is characterized in that the rare earth metal is prepared by molten salt electrolysis, the electrolysis voltage is 9-10V, the electrolysis current is 5800-6000A, the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is 80%, compared with the traditional anode, the electrode utilization rate is improved by 10%, and the service life of the upper-inserted anode is improved by 10%.
Example 2
Same as example 1
The difference lies in that the adopted anode is a ring-shaped anode (see figure 3) with a section along the horizontal direction, the adopted anode is a trapezoidal anode (see figure 4) with a section along the vertical direction, the polar distance is 10-30cm, the electrolytic current is 10000A, the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is 85%, compared with the traditional anode, the electrode utilization rate is improved by 10%, and the service life of the upper-inserting type anode is improved by more than 10%.
Example 3
Same as example 1
The difference lies in that the adopted anode is a traditional rectangular anode, the cathode is a round anode along the horizontal direction (see figure 1), the section of the cathode along the vertical direction is a trapezoid anode (see figure 2), the cathode is made of carbon materials, the polar distance is 20-40cm, the electrolytic current is 15000A, and the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is 90%.
Example 4
Same as example 1
The difference lies in that the adopted anode is a traditional rectangular anode, the cathode is a quadrilateral, specifically a square (see figure 1) with a cross section along the horizontal direction, the cross section along the vertical direction is a convex shape (see figure 2), the polar distance is 30-80cm, the electrolytic current is more than 20000A, and the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is more than 85%.
Example 5
Same as example 1
The difference lies in that the adopted anode is a quadrilateral anode (see figure 3) with a cross section along the horizontal direction, a trapezoidal anode (see figure 4) with a cross section along the vertical direction, a carbon material is adopted, the polar distance is 10-30cm, the electrolytic current is 10000A, the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is 87%, compared with the traditional anode, the electrode utilization rate is improved by 10%, and the service life of the upper-inserting anode is prolonged by more than 10%.
Example 6
Same as example 1
The difference lies in that the adopted anode is quadrangular in cross section along the horizontal direction (see figure 3), L-shaped in cross section along the vertical direction (see figure 4), carbon material is adopted, the polar distance is 10-30cm, the electrolytic current is 10000A, the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is 84%, compared with the traditional anode, the electrode utilization rate is improved by 10%, and the service life of the upper-inserting anode is improved by more than 10%.
Example 7
Same as example 1
The difference lies in that the adopted anode is a traditional rectangular anode, the cathode is a polygon with a cross section along the horizontal direction, specifically a hexagon (see figure 1), the cross section along the vertical direction is in a shape of Chinese character 'tu' (see figure 2), the polar distance is 30-80cm, the electrolytic current is more than 20000A, and the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is more than 82%.
Example 8
Same as example 1
The difference lies in that the adopted anode is a traditional rectangular anode, the cathode is a polygon along the cross section of the horizontal direction, specifically a hexagon (see figure 1), the cross section of the vertical direction is a step shape (see figure 2), the polar distance is 20-40cm, the electrolytic current is larger than 15000A, and the current efficiency of the electrolytic cell adopting the special-shaped electrode structure is larger than 92%.
Comparative example 1
The adopted upper-inserted cathode is a cylindrical cathode, the adopted upper-inserted anode is a cuboid anode, and the current density is 60-75%.
Comparative example 2
An upward-inserted type special-shaped anode is the same as that in the embodiment 1, except that the mode of being wide at the upper part and narrow at the lower part is adopted, and the current efficiency is lower than 80 percent and is 70 to 75 percent.
Claims (9)
1. The utility model provides an on insert formula dysmorphism electrode, inserts formula negative pole and last formula positive pole including last, its characterized in that, goes up and inserts the formula negative pole and one or two kinds of settings in the formula positive pole of inserting on and insert formula special-shaped electrode for the polar distance between the two satisfies: (1) the polar distance of the molten salt liquid surface is greater than the polar distance inside the molten salt; and (2) the distance between the poles is 5-80 cm.
2. The upward-inserted special-shaped electrode as claimed in claim 1, wherein when the upward-inserted cathode is a cylindrical cathode, the upward-inserted anode is a special-shaped anode; when the upper inserted anode is a cuboid anode or an arc anode, the upper inserted cathode is a special-shaped cathode;
when the special-shaped anode or the special-shaped cathode is adopted, the distance between the electrode polar distance in the electrolytic cell and the surface of the fused salt is more than the distance between the electrode polar distance in the fused salt.
3. The upward-inserted special-shaped electrode according to claim 2, wherein the cross-sectional shape of the special-shaped anode along the horizontal plane comprises but is not limited to a quadrilateral shape or a circular ring shape, and the cross-sectional shape along the vertical direction comprises but is not limited to a trapezoid, a triangle, an L shape or a step shape with a narrow top and a wide bottom.
4. The upward-inserted special-shaped electrode according to claim 3, wherein the cross-sectional shape of the special-shaped anode along the vertical direction is L-shaped or stepped.
5. The upward-inserted special-shaped electrode according to claim 2, wherein the cross-sectional shape of the special-shaped cathode along the horizontal direction comprises but is not limited to one of a circle, a triangle, a quadrangle and a polygon, and the cross-sectional shape along the vertical direction comprises but is not limited to one of a trapezoid, a square, a convex and a step with a narrow top and a wide bottom.
6. The upward-inserted profiled electrode of claim 2, wherein the material of the upward-inserted cathode includes but is not limited to one of tungsten, molybdenum, and carbon material; materials selected for the upper-inserted anode include, but are not limited to, carbon materials.
7. The upward-inserted profiled electrode as claimed in claim 2, characterized in that the pole pitch of the upward-inserted cathode and the upward-inserted anode is between 5cm and 80cm.
8. A method for preparing rare earth metal by molten salt electrolysis is characterized in that the upward-inserted special-shaped electrode of any one of claims 1 to 7 is adopted, an upward-inserted cathode is inserted into the center of an electrolytic cell from the upper part of the electrolytic cell, an upward-inserted anode surrounds the upward-inserted cathode and is inserted into the periphery of the electrolytic cell from the upper part of the electrolytic cell, the molten salt electrolysis is carried out to prepare the rare earth metal, and the current efficiency of the electrolytic cell is more than 80 percent.
9. The method of claim 8, wherein when the anode is a conventional anode, the electrode utilization is increased by 10% or more, and the service life of the anode is increased by 10% or more.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210919532.XA CN115449853A (en) | 2022-08-02 | 2022-08-02 | Up-inserted special-shaped electrode and method for preparing rare earth metal by molten salt electrolysis of up-inserted special-shaped electrode |
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| CN202210919532.XA CN115449853A (en) | 2022-08-02 | 2022-08-02 | Up-inserted special-shaped electrode and method for preparing rare earth metal by molten salt electrolysis of up-inserted special-shaped electrode |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014051731A (en) * | 2012-09-10 | 2014-03-20 | Nagoya Univ | Recovery method and recovery system of rare earth metal |
| CN105441988A (en) * | 2015-11-19 | 2016-03-30 | 中国科学院青海盐湖研究所 | Furnace starting method for preparing simple substance metal or alloy in molten salt electrolysis mode |
| CN105624736A (en) * | 2016-03-25 | 2016-06-01 | 中南大学 | Rare earth molten salt electrolytic cell with novel electrode structure |
| JP2017179488A (en) * | 2016-03-30 | 2017-10-05 | 日立金属株式会社 | Molten salt electrolysis apparatus and molten salt electrolysis method |
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- 2022-08-02 CN CN202210919532.XA patent/CN115449853A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014051731A (en) * | 2012-09-10 | 2014-03-20 | Nagoya Univ | Recovery method and recovery system of rare earth metal |
| CN105441988A (en) * | 2015-11-19 | 2016-03-30 | 中国科学院青海盐湖研究所 | Furnace starting method for preparing simple substance metal or alloy in molten salt electrolysis mode |
| CN105624736A (en) * | 2016-03-25 | 2016-06-01 | 中南大学 | Rare earth molten salt electrolytic cell with novel electrode structure |
| JP2017179488A (en) * | 2016-03-30 | 2017-10-05 | 日立金属株式会社 | Molten salt electrolysis apparatus and molten salt electrolysis method |
Non-Patent Citations (1)
| Title |
|---|
| 厉衡隆: "铝熔炼生产技术手册", 31 July 2011, 北京：冶金工业出版社, pages: 303 * |
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