CN108004568B - Rare earth electrolytic cell lining structure and rare earth electrolytic cell - Google Patents
Rare earth electrolytic cell lining structure and rare earth electrolytic cell Download PDFInfo
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- CN108004568B CN108004568B CN201711474369.6A CN201711474369A CN108004568B CN 108004568 B CN108004568 B CN 108004568B CN 201711474369 A CN201711474369 A CN 201711474369A CN 108004568 B CN108004568 B CN 108004568B
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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
Abstract
The invention relates to a rare earth electrolytic cell lining structure and an electrolytic cell, comprising a bottom lining and a side lining, wherein the bottom lining comprises a ceramic fiber layer, a bottom refractory layer, an impermeable layer and a graphite layer which are sequentially stacked from bottom to top; the side lining is arranged around the bottom lining, the side lining extends upwards to the position above the top surface of the graphite layer, and the bottom lining and the side lining are combined and enclose a cavity for electrolytic reaction. The lining structure of the rare earth electrolytic cell has reasonable material selection and layout, the thermal balance performance of the electrolytic cell is good, and the heat loss can be effectively reduced; the use of the high-thermal-conductivity silicon carbide protective layer enables the furnace side of the electrolytic cell to be formed more easily, so that the side heat-insulating material of the electrolytic cell is protected more effectively; in addition, the cylindrical cathode is adopted, so that the high anode and the low anode of the current density cathode are more obvious, and the electrolytic reaction area is effectively increased.
Description
Technical Field
The invention relates to a fused salt rare earth electrolytic cell lining structure and a rare earth electrolytic cell, and belongs to the technical field of rare earth fused salt electrolysis equipment.
Background
The existing rare earth electrolysis mainly uses rare earth oxide as raw material and fluoride as electrolyte in the molten salt rare earth electrolysis process, the electrolysis bath type of the existing rare earth electrolysis process is an up-inserting cathode-anode structure, the cylindrical surfaces of the cathode and the anode are placed in the electrolyte in parallel, and a tungsten crucible is placed below the cathode and the anode for receiving metal. This kind of current tombarthite electrolysis trough is mostly open type design, its heat insulating ability is relatively poor, a large amount of heats scatter and disappear to the air through radiation and convection, thereby make ambient temperature rise, workman's operational environment has worsened, also make the thermal balance of electrolysis trough unstable, the mode that has to pass through high cell voltage maintains thermal balance, the voltage of electrolysis trough is too high simultaneously, when the oxide is not enough, tombarthite fluoride decomposes seriously, produce the fluorine-containing harmful gas and directly discharge from cell body upper portion, the environment is polluted, the health that gives the workman has brought very big hidden danger simultaneously. In addition, the polar distance of the existing rare earth metal electrolytic cell can not be adjusted, the polar distance is larger and larger along with the rare earth electrolysis, the cell voltage is generally 10-12V, a large amount of electric energy is wasted, the production efficiency is low, the process parameter fluctuation is large, the cell type current intensity is 3000-7000A, and the development of large-scale and energy-saving of the rare earth electrolytic cell is seriously hindered. Therefore, the development of a large energy-saving and environment-friendly rare earth molten salt electrolytic cell is the key to realizing the rare earth electrolysis industry and the technical development thereof.
The Chinese invention patent CN103614747A discloses a large-scale combined rare earth molten salt electrolytic bath system, which realizes compact bath body structure and reasonable wiring structure, but the anode and the cathode are the up-inserted anode and cathode, the polar distance can not be changed, the rare earth electrolytic bath voltage is not reduced, and the design of the anode and cathode structure is not beneficial to the operation of the electrolytic process and the large-scale of the electrolytic rare earth.
Chinese patent CN105441987A discloses a molten salt electrolytic cell for producing rare earth metals and alloys with liquid cathode, the structure is that the cathode and the anode are inserted into the electrolyte vertically in parallel, the liquid metal of the electrolytic cell is used as the cathode, although the invention is beneficial to the large-scale of the electrolytic cell, the liquid metal is used as the cathode, the metal is easy to be secondarily oxidized, and the liquid metal is always in the reaction zone, so that the bottom of the electrolytic cell is easy to be corroded, and at the same time, the great difficulty is brought to the start-up operation of the electrolytic cell. In addition, the liquid metal acts as a cathode, increasing the area of the cathode, decreasing the current density of the cathode, and resulting in a decrease in current efficiency.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a rare earth electrolytic cell lining structure and a rare earth electrolytic cell so as to optimize the rare earth electrolytic cell lining structure.
The technical scheme of the invention is as follows: a lining structure of a rare earth electrolytic cell comprises a bottom lining and a side lining, wherein the bottom lining comprises a ceramic fiber layer, a bottom refractory brick layer, an impermeable layer and a graphite layer which are sequentially stacked from bottom to top; the side lining is arranged around the bottom lining, the side lining extends upwards to the position above the top surface of the graphite layer, and the bottom lining and the side lining are combined and enclose a cavity for electrolytic reaction.
Preferably, the side liner is disposed on the top surface of the barrier layer.
The lateral lining comprises an anti-seepage pouring layer, a lateral refractory brick layer and a lateral shell which are sequentially distributed from inside to outside. Preferably, the side refractory brick layers are mainly built of refractory bricks. Preferably, the side casing is mainly made of a steel plate.
Furthermore, the thickness of the side shell is 5-20mm, the thickness of the side refractory brick layer is 50-300mm, and the thickness of the impermeable casting material is 50-300 mm.
Furthermore, the thickness of the ceramic fiber layer is 10-100mm, the thickness of the bottom refractory brick layer is 50-300mm, the thickness of the impermeable layer is 50-300mm, and the thickness of the graphite layer is 100-500 mm.
The top surface and the inner side surface of the side lining are covered with protective layers. Preferably, the thickness of the protective layer is 50-300 mm.
The cross section of the protective layer is Z-shaped and is mainly made of silicon carbide materials. The silicon carbide ceramic material has good high temperature resistance and corrosion resistance, simultaneously has very good oxidation resistance, has certain electrical insulation, is relatively cheap, has good heat conduction performance, can protect the side lining, and simultaneously forms a local low-temperature area on the side to promote the formation of the electrolytic bath furnace side, thereby more effectively protecting the side lining.
Preferably, the barrier layer consists essentially of a dry barrier material. The use of the dry type impermeable material is beneficial to prolonging the service life of the electrolytic cell and reducing the consumption of electrolyte. On one hand, when the electrolyte leaks to be in contact with the dry impermeable material, the aluminosilicate in the dry impermeable material can react with the electrolyte to generate a glassy hard impermeable layer, so that the electrolyte is prevented from continuously leaking to corrode the lower heat-insulating material; on the other hand, the dry type impermeable material has certain compressibility, can relieve the thermal expansion of surrounding structures, can better meet the rare earth electrolysis production conditions (the temperature use range of the electrolytic cell is 950-.
The bottom refractory brick layer is mainly formed by laying refractory bricks.
And a collecting tank for collecting rare earth is arranged at the top of the graphite layer. Preferably, the cross-section of the collecting trough is circular or square.
And a flow guide layer is laid on the top surface of the graphite layer and inclines towards the direction of the collecting tank. Preferably, the inclination is 2-10 °.
The setting on graphite layer surface water conservancy diversion layer, the metal that is convenient for appear flows in the collecting vat firstly, and secondly the effectual corruption that prevents the graphite layer has improved the purity of product simultaneously, is favorable to prolonging the electrolysis trough life-span.
Furthermore, the flow guide layer is mainly composed of tungsten or molybdenum, so that the flow guide layer is high temperature resistant and has good compatibility with rare earth molten metal.
The rare earth electrolytic cell comprises a cell body, wherein the lining structure of the rare earth electrolytic cell is arranged in the cell body.
The electrolytic bath is characterized by further comprising an anode and a cathode, wherein the anode is suspended above the cavity and extends into the electrolyte in the cavity, the bottom surface of the anode is an upwards-concave arc surface, the cathode is arranged at the central axis of the arc surface, the part of the cathode corresponding to the arc surface is a cylindrical surface, the central axis of the cylindrical surface is coincided with the central axis of the arc surface, and the distance between the bottom surface of the cathode and the inner bottom surface of the bath body is larger than 0.
Further, the cathode is cylindrical.
The distance between the cathode and the top surface of the lining structure of the rare earth electrolytic cell is 10-150mm, and preferably 20-50 mm.
Further, the cathode is made of tungsten. So as to adapt to the environment with high electrolysis temperature and strong corrosivity of electrolyte in the rare earth electrolysis process.
In the present invention, it is preferable that the cathodic current density is 1 to 10A/cm2Anode current density of 0.4-2A/cm2。
Further, the anode is mainly made of a carbon material.
Furthermore, one end of the cathode is fixed in the side lining, and the other end of the cathode penetrates through the side lining and extends out of the tank body. The use of silicon carbide material can meet the insulation requirement.
The lining structure of the rare earth electrolytic cell uses the silicon carbide ceramic material with excellent oxidation resistance and corrosion resistance, solves the problem of serious oxidation corrosion of the side part caused by using carbon blocks as the side part protective material in the conventional rare earth electrolytic cell, has good heat-conducting property of silicon carbide, can ensure that the temperature of the side part of the electrolytic cell is relatively low, is beneficial to forming a ledge, thus forming double protection for the electrolytic cell and prolonging the service life of the electrolytic cell. The lining of the electrolytic cell is reasonable in heat preservation design, is beneficial to the stability of the heat balance of the electrolytic cell, effectively reduces the heat loss of the electrolytic cell caused by radiation and convection, and saves electric energy.
The invention uses the mode of transversely inserting the cathode at the lower part of the cell in the field of subversion of rare earth electrolysis, so that the electrolytic heating area is changed from the traditional middle-upper part to the bottom of the electrolytic cell, and the fluctuation of electrolyte and the energy consumption of electrolysis are greatly reduced.
The anode and the cathode of the rare earth electrolytic cell are vertically arranged, so that the requirements of low anode current density and high cathode current density required in the rare earth electrolysis process are met, and high current efficiency is obtained; the cathode with a cylindrical structure is adopted, a certain space is reserved at the lower part of the cathode, and the cathode is matched with the anode with a circular structure at the upper part of the cathode, so that the metal can be separated out at the cathode. In addition, the polar distance between the cathode and the anode of the rare earth electrolytic cell can be adjusted according to the electrolysis process conditions of different stages, so that the voltage and the temperature of the electrolytic cell can be better controlled.
The rare earth electrolytic cell can be used for the fusion electrolysis extraction of rare earth, and comprises one metal or two or more mixed metals of lanthanum, cerium, praseodymium, neodymium and the like.
Compared with the prior art, the invention has the following beneficial effects:
1. the lining structure of the rare earth electrolytic cell has reasonable material selection and layout, the thermal balance performance of the electrolytic cell is good, and the heat loss can be effectively reduced.
2. The rare earth electrolytic cell side high-thermal-conductivity Z-shaped silicon carbide protective layer is used, so that the ledge of the electrolytic cell is easier to form, and the side lining is protected by two layers, so that the side heat-insulating material of the electrolytic cell is more effectively protected.
3. The cathode of the rare earth electrolytic cell is arranged below, the polar distance between the cathode and the anode can be adjusted according to the electrolytic process, the utilization rate of the anode can be improved, and the cell voltage can be reduced.
4. The rare earth electrolytic cell is provided with the flow guide layer on the graphite layer, so that liquid metal can flow into the collector more easily, the corrosion of the graphite layer is avoided, the service life of the electrolytic cell can be prolonged, and the purity of rare earth metal products is improved.
5. The anode of the rare earth electrolytic cell adopts a round surface shape and a cathode cylindrical shape, so that the high anode and the low anode of the current density cathode are more obvious, and the electrolytic reaction area is effectively increased.
Drawings
FIG. 1 is a front view of a rare earth electrolyzer structure;
FIG. 2 is a side view of a rare earth electrolytic cell structure;
FIG. 3 is a front view of the rare earth electrolyzer liner and cathode and anode structures;
FIG. 4 is a side view of the rare earth electrolyzer liner and cathode and anode structures;
in the figure: 1-guide rod, 2-anode steel claw, 3-nut, 4-anode, 5-side shell, 6-cathode, 7-protective layer, 8-side refractory brick layer, 9-impermeable casting layer, 10-diversion layer, 11-graphite layer, 12-impermeable layer, 13-bottom refractory brick layer, 14-ceramic fiber layer, 15-collecting tank, 16-electrolyte, 17-anticorrosion jacket, 18-transmission guide rod, 19-bus, 20-protective sleeve, 21-lifting motor, 22-lifting rod, 23-truss beam, 24-clamp, 25-hook, 26-blanking machine, 27-horizontal cover plate, 28-smoke tube, 29-gas collecting hood, 30-tank shell, 31-end sealing hood, 32-corner sealing hood, 33-side seal cover.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. For convenience of description, the words "upper", "lower", "left" and "right" in the following description are used only to indicate the correspondence between the upper, lower, left and right directions of the drawings themselves, and do not limit the structure.
As shown in fig. 1 to 4, a rare earth electrolytic cell comprises a cell upper structure, a cell shell 30, a bottom lining, a side lining, a cathode structure and an anode structure, wherein the cell upper structure comprises an anode lifting structure, a blanking machine 26, a truss beam 23, a sealing system and the like, and the anode lifting structure comprises a lifting motor 21, a transmission guide rod 18, a lifting rod 22, a protective sleeve 20, a bus bar 19, a clamp 24 and a hook 25; the sealing system comprises an end sealing cover 31, a side sealing cover 33, a corner sealing cover 32, a horizontal cover plate 27, a smoke pipe 28 and a gas collecting cover 29, wherein the end sealing cover 31, the side sealing cover 33, the corner sealing cover 32, the horizontal cover plate 27 and the gas collecting cover 29 are combined to form an integral cover, so that the heat preservation capacity of the electrolytic cell is improved; the bottom lining comprises a ceramic fiber layer 14, a bottom refractory brick layer 13, an impermeable layer 12, a graphite layer 11 and a diversion layer 10 which are sequentially distributed from bottom to top, a collecting tank 15 is arranged on the graphite layer 11, and the side lining comprises a side shell 5, a side refractory brick layer 8, a protective layer 7 and an impermeable pouring layer 9 from outside to inside; the cathode structure is mainly a cathode 6; the anode structure comprises an anode 4, an anode steel claw 2 and a guide rod 1.
Wherein the current of the rare earth electrolytic cell is 20 kA; the anode current density is 0.75A; the cell voltage was 4.7V.
In the anode structure, two anode carbon blocks are connected below an anode steel claw 2 to form an anode 4, and a proper distance is reserved between the two anode carbon blocks 4 according to a rare earth electrolysis process. Preferably, the number of the anode carbon blocks is 14 in the transverse arrangement, and the number of the anode carbon blocks is 2 in the longitudinal arrangement.
The anode structure is connected to the bus bar, and the anode lifting mechanism drives the bus bar 19 to drive the anode to move up and down, so as to adjust the polar distance.
The cathode 6 is in a cylindrical shape, the length of the cathode is determined according to the size of the rare earth electrolytic cell, and an anti-corrosion jacket 17 is arranged at the outlet of the cathode 6. Preferably, the cathode 6 has a diameter of 70mm and is mainly made of metallic tungsten.
The lower surface of the anode 4 is semicircular, and the circle center of the anode is at the same point as that of the cathode 6. Preferably, the semi-circle diameter is 300 mm.
The collecting groove 15 is arranged at the upper part of the graphite layer 11 and used for receiving rare earth metal, and the flow guide layer 10 has a certain inclination so as to facilitate the metal to flow into the tungsten crucible 15. Preferably, the inclination of the flow guiding layer 10 is 3 °.
The thickness of the bottom material structure ceramic fiber layer 14 is 50mm, the thickness of the bottom fire-resistant layer 13 is 195mm, the thickness of the impermeable layer 12 is 185mm, and the thickness of the graphite layer 11 is 395 mm.
The thickness of the lateral shell 5 is 10mm, the thickness of the lateral refractory brick 8 is 130mm, the thickness of the impermeable casting material 9 is 118mm, and the thickness of the silicon carbide protective layer 7 with the Z-shaped section is 200 mm.
In this embodiment, the electrolyte has a liquid level of 380mm, and includes 85% of rare earth fluoride and 15% of lithium fluoride by mass, and the rare earth oxide accounts for 3% of the rare earth fluoride and the lithium fluoride.
Referring to fig. 1-4, firstly, a cell shell is manufactured for an electrolytic cell according to the structure of the rare earth electrolytic cell, then the electrolytic cell is built, the building is started from the bottom, a ceramic fiber layer is laid at the bottommost part, bottom refractory bricks are built on the upper part of the ceramic fiber layer by using carbon paste to form a bottom refractory brick layer, and then dry type impermeable materials are laid on the bottom refractory bricks. Then, a graphite layer and an electrolytic cell side portion are constructed, the graphite layer is formed by stacking graphite bricks using a carbon paste, the electrolytic cell side portion refractory bricks are stacked like bottom portion refractory bricks, and then silicon carbide and a steel plate are formed. After the building of the electrolytic cell is completed, other equipment required by the electrolytic cell is installed, including an anode lifter, blanking equipment and a sealing cover, then the electrolytic cell is roasted, the electrolyte of the electrolytic cell is heated into a molten state by using a plurality of arc striking machines, and current flows from a guide rod to a steel claw, to an anode carbon block, to the electrolyte and to a cathode, and then flows out of an aluminum bus to form a current loop. The metal is separated out on the cathode, then flows into the tungsten crucible through a flow guiding layer with a slope, and the rare earth metal is taken out in a siphoning mode after the rare earth metal electrolysis is carried out for a period of time, so that a rare earth metal product is obtained.
The above examples are illustrative and should be understood that they are only for the purpose of illustrating the invention more clearly and are not intended to limit the scope of the invention, and the above examples are only an embodiment, and the rare earth electrolyzer of the invention can be designed to have a large-scale electrolyzer with current intensity of 60-120kA according to the requirements of different production capacities.
Claims (5)
1. A rare earth electrolytic cell comprises a cell body and is characterized in that a rare earth electrolytic cell lining structure is arranged in the cell body and comprises a bottom lining and a side lining, wherein the bottom lining comprises a ceramic fiber layer (14), a bottom refractory brick layer (13), an impermeable layer (12) and a graphite layer (11) which are sequentially stacked from bottom to top, the ceramic fiber layer is 50mm in thickness, the bottom refractory brick layer is 195mm in thickness, the impermeable layer is 185mm in thickness, the graphite layer is 395mm in thickness, the side lining comprises an impermeable pouring layer (9), a side refractory brick layer (8) and a side shell (5) which are sequentially distributed from inside to outside, the side shell is 10mm in thickness, the side refractory brick layer is 130mm in thickness, and the impermeable pouring layer is 118mm in thickness; the side lining is arranged around the bottom lining, the side lining extends upwards to the position above the graphite layer (11), and the bottom lining and the side lining are combined and enclose a cavity for electrolytic reaction;
the top surface and the inner side surface of the side lining are covered with protective layers (7), the cross section of each protective layer (7) is Z-shaped and is made of silicon carbide materials; the protective layer extends to the top surface of the graphite layer (11) towards the cavity; the thickness of the protective layer is 200 mm;
the electrolytic bath is characterized by further comprising an anode (4) and a cathode (6), wherein the anode (4) is suspended above the cavity and extends into the electrolyte in the cavity, the bottom surface of the anode (4) is an arc surface which is concave upwards, the cathode (6) is arranged at the central axis of the arc surface, the part of the cathode corresponding to the arc surface is a cylindrical surface, the central axis of the cylindrical surface is overlapped with the central axis of the arc surface, and the distance between the bottom surface of the cathode and the inner bottom surface of the bath body is greater than 0; one end of the cathode is fixed in the side lining, and the other end of the cathode penetrates through the side lining and extends out of the tank body; the rare earth electrolytic cell is a 20 kA-grade electrolytic cell.
2. Rare earth electrolysis cell according to claim 1, characterized in that said barrier layer (12) consists essentially of a dry barrier material.
3. Rare earth electrolysis cell according to claim 1, wherein the bottom refractory brick layer (13) is mainly laid out of refractory bricks.
4. Rare earth electrolysis cell according to claim 1, characterized in that the top of the graphite layer (11) is provided with a collection trough (15) for collecting rare earth.
5. Rare earth cell according to claim 4, characterized in that the top surface of the graphite layer (11) is provided with a flow guiding layer (10), said flow guiding layer (10) being inclined in the direction of the collecting trough (15).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711474369.6A CN108004568B (en) | 2017-12-29 | 2017-12-29 | Rare earth electrolytic cell lining structure and rare earth electrolytic cell |
| PCT/CN2018/122243 WO2019128826A1 (en) | 2017-12-29 | 2018-12-20 | Rare earth metal molten salt electrolytic cell |
| ZA2020/04577A ZA202004577B (en) | 2017-12-29 | 2020-07-23 | Rare earth metal molten salt electrolytic cell |
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| WO2019128826A1 (en) * | 2017-12-29 | 2019-07-04 | 中南大学 | Rare earth metal molten salt electrolytic cell |
| CN110528028B (en) * | 2019-09-02 | 2023-10-24 | 益阳鸿源稀土有限责任公司 | Rare earth electrolytic cell bus lifting system and bus lifting method |
| CN110408961B (en) * | 2019-09-05 | 2021-04-23 | 中南大学 | Arc striking starting method of rare earth electrolytic cell |
| CN113737225A (en) * | 2021-09-13 | 2021-12-03 | 沈阳达澳金属科技开发有限公司 | Lining structure and rare earth metal fused salt electrolytic cell adopting same |
| CN114835497B (en) * | 2022-06-13 | 2022-11-08 | 赣州晨光稀土新材料有限公司 | Ceramic material for rare earth molten salt electrolytic cell and preparation method and application thereof |
| CN115074781B (en) * | 2022-06-21 | 2024-03-15 | 东北大学 | Bottom cathode rare earth electrolytic tank |
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| CN101451253A (en) * | 2007-11-28 | 2009-06-10 | 北京有色金属研究总院 | Corrosion resistant and antioxidation insulation seal device for fused salt electrolysis |
| CN101984143B (en) * | 2010-12-04 | 2012-04-25 | 郑州大学 | External heated aluminum electrolytic cell |
| AU2015315380B2 (en) * | 2014-09-10 | 2020-04-16 | Alcoa Usa Corp. | Systems and methods of protecting electrolysis cell sidewalls |
| CN204779870U (en) * | 2015-07-08 | 2015-11-18 | 赣州三友稀土新材料有限公司 | Leak -tight rare earth metal electrolytic cell assembly |
| CN106400053A (en) * | 2016-06-22 | 2017-02-15 | 贵阳铝镁设计研究院有限公司 | Integrally-formed aluminum electrolytic cell based on cathode inner liner and integral forming method thereof |
| CN106283122B (en) * | 2016-10-29 | 2019-03-15 | 虔东稀土集团股份有限公司 | Electrolytic furnace |
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| Si3N4结合SiC材料在稀土电解槽中的应用及效果;陈德宏等;《稀土》;20120615;第33卷(第3期);第12-15页 * |
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