CN207596976U - A kind of rare earth oxide fused-salt bath - Google Patents
A kind of rare earth oxide fused-salt bath Download PDFInfo
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- CN207596976U CN207596976U CN201721708309.1U CN201721708309U CN207596976U CN 207596976 U CN207596976 U CN 207596976U CN 201721708309 U CN201721708309 U CN 201721708309U CN 207596976 U CN207596976 U CN 207596976U
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Abstract
The utility model is related to a kind of rare earth oxide fused-salt bath, including furnace shell, insulating layer, protective layer, graphite cuvette, graphite anode, crucible, cathode；The graphite anode and cathode insert in the graphite cuvette, and the graphite anode is set around the cathode, and the crucible is located in the graphite cuvette and the lower section of cathode described in face；The Integral hollow graphite column sleeve of a both ends open is removably inserted between graphite cuvette and graphite anode, the inside of the Integral hollow graphite column sleeve forms tank house, the electrochemical reaction in electrolytic process is made to act on the inner wall of the graphite anode and the Integral hollow graphite column sleeve, the consumption of graphite cuvette is avoided, reduction prepares the cost of rare earth metal.
Description
Technical field
The utility model is related to Rare Earth Electrolysis apparatus field more particularly to a kind of rare earth oxide fused-salt baths.
Background technology
Using pyrometallurgy technology, which is to pass through reduction under the high temperature conditions for the preparation of rare earth metal and alloy
Rare earth ion realizes the purification process of rare earth metal.Pyrometallurgy technology mainly includes fused salt electrolysis process and metallothermic processes,
Wherein fused salt electrolysis process due to have many advantages, such as at low cost, ingredient be uniformly easy to control, it is high-quality, it is easy realization continuous production,
Become the main production of the industrial rare earth metal of current large-scale and its alloy.Fused salt electrolysis process prepares rare earth
Metal can be divided into two kinds of chloride system and fluoride system, in molten chloride, the solubility of metal according to molten salt system
It is very big, its yield and current efficiency is caused to reduce, and power consumption is caused to increase, while the high volatile of fused salt can cause to be electrolysed
Process generates a large amount of chlorine, causes operational difficulty.Therefore, Chlorides molten salts have gradually been fluorinated object and have been taken
Generation.
Fluoride smelt salt oxide electrolysis technique is for raw material, with molten condition with rare earth oxide (RE2O3)
REF-LiF systems are electrolyte, and using graphite as graphite anode, tungsten bar is cathode, and rare earth metal is prepared by DC electrolysis.Electricity
The structure of slot is solved as shown in Figure 1, according to groove body size and size of current, electrolytic cell can be divided into 3000A, 8000A and 10000-
The large scale electrolytic cell of 28000A.It needs to add REO into fused electrolyte in electrolytic process, the net reaction of electrolytic process
For：RE2O3+ C=2RE+3/2CO2.The substance of entire reaction process consumption is rare earth oxide and graphite anode carbon, reaction product
One of be gas.In electrolytic process, graphite anode 6 is spliced by 4 graphite tiles, therefore anti-in electrochemistry, chemistry
It answers, under the action of fused salt erosion and mechanical force, the stitching portion gap of adjacent two pieces of graphite anodes graphite tile can expose graphite cuvette 5
Cell wall, cause the consumption (as shown in Figure 2) of graphite cuvette 5.Since the slot structure of graphite enlargement manufacture specific shape is very tired
Difficulty, and the bigger manufacturing price of specification is more expensive, therefore the prior art can cause graphite cuvette 5 to be burnt and scrap quickly, make electrolysis
The cost for preparing rare earth metal is excessively high.
As shown in Figure 1, wherein the loss of graphite cuvette 5 include electrochemical reaction loss, chemical reaction loss, fused salt corrosion and
Mechanical force is lost, and specific loss mechanisms are as follows：
(1), graphite cuvette 5 is lost caused by electrochemical reaction：
In electrolytic process, since the gap between several graphite tiles of graphite anode 6 can cause the cell wall conduct of graphite cuvette 5
Graphite anode is consumed, and reaction equation is as follows：
O2--2e-=1/2O2………………(1)
1/2O2+ C=CO ... ... ... (2)
2O2-+C-4e-=CO2………………(3)
2O2—4e-=O2………………(4)
Above-mentioned 4 reactions may occur simultaneously, in electrolysis temperature less than 857 DEG C or under high current density, graphite anode master
It is CO to want product2, but at a temperature of higher (900 DEG C), CO and CO will be generated2Mixed gas.
(2), graphite cuvette 5 caused by chemically reacting consumes：
The disposable gas of the reaction generation of graphite anode 6 is escaped, scorching hot gas above melt by fused electrolyte from interface
With the effect of graphite cuvette 5 following react will occur for body：
CO2+ C=2CO ... ... ... (5)
O2+ C=CO2………………(6)
(3), the corrosional graphite cuvette 5 of fused salt consumes：
Fused salt is corroded there are mainly two types of the modes of graphite cuvette 5, for the first time, during electrolytic furnace use, fused salt and graphite cuvette 5
Prolonged contact can lead to the roughening of 5 material crystal grain of graphite cuvette；Secondly, in electrolytic process, since graphite anode effect is led
The CF of causenType or COFnType intermediate compound can also occur on 5 surface of graphite cuvette, in turn result in graphite cuvette 5 groove body be consumed and
It destroys.
In addition, during the graphite tile of graphite anode 6 and sampling is replaced, due to graphite caused by mechanical external force
5 groove body of slot damages the consumption that can also aggravate graphite cuvette 5.
Also occur the way of some protection electrolytic cell cell walls, such as the patent of invention of CN104451835 in the prior art
Application is coated with three-layer protection layer in four walls of the groove body and bottom, is graphite linings, titanium dioxide successively outward from groove body
Layer and resin protective layer.But when the protective layer being applied to electrofluorination rare earth molten salt preparing in the electrolytic cell of rare earth metal, slot
The resin protective layer of internal wall can destroy the homogeneity of electric field in electrolytic process, and energy consumption is caused to increase.In addition, the total thickness of the coating
Only 3mm or so is spent, for the non-light rare earth metal such as electrolytic preparation metallic cerium, due to the oxidisability of the cerium ion of 4+, corruption
Corrosion is very strong, the consumption that will aggravate graphite significantly during electrolysis, which also may be only available for certain light dilute
The preparation of earth metal, therefore the electrolytic cell of the technology its application field is limited to, application range is relatively narrow.In addition, also have
The prior art proposes the technological concept of double-layer graphite slot, i.e., is piled up again with graphite brick in the inboard of outer layer graphite cuvette in being formed
Layer graphite, however the packing structure can cause electric field line to directly act on graphite crucible, and then lead to stone due to the presence in gap
The increase of black anode effect not only wastes the increase that cost also results in energy consumption；Secondly, double-layer graphite slot has little significance,
Loss described in aforementioned (one)-(three) item can't occur for the bottom wall of graphite cuvette 5, thus double-layer graphite slot can only be added to stone significantly
Material cost (bulk entirety graphite is expensive), manufacturing cost, the manufacture craft difficulty of ink tank.
Utility model content
In conclusion in order to extend the service life of existing Rare Earth Electrolysis equipment, reduce in electrolytic process due to graphite sun
Graphite tank caused by the reasons such as polar effect and the corrosion of fluoride melt is lost, and the utility model proposes a kind of novel rare earths
The structure of oxide and salt melt electrolyzing slot, it is detachable by being inserted between graphite anode and the groove body inner wall of electrolytic cell
A piece Integral hollow graphite column sleeve, realizes the protection to electrolytic cell.
In order to realize above-mentioned technical purpose, the technical solution adopted in the utility model is as follows：
A kind of rare earth oxide fused-salt bath, including furnace shell, insulating layer, protective layer, graphite cuvette, graphite anode, earthenware
Crucible, cathode；The graphite anode and cathode insert in the graphite cuvette, and the graphite anode is set around the cathode, the earthenware
Crucible is located in the graphite cuvette and the lower section of cathode described in face；Wherein one is removably inserted between graphite cuvette and graphite anode
The Integral hollow graphite column sleeve of root both ends open, the inside of the Integral hollow graphite column sleeve form tank house, make electrolysis
Electrochemical reaction in the process acts on the inner wall of the graphite anode and the Integral hollow graphite column sleeve, so as to avoid stone
The consumption of ink tank.
Preferably, the outer wall of the Integral hollow graphite column sleeve is close to the inner wall of the graphite cuvette.
Preferably, the cathode is tungsten cathode or molybdenum cathode, and the crucible is tungsten crucible.
Preferably, the cathode is tungsten cathode or molybdenum cathode, and the crucible is tungsten crucible；The furnace shell is box hat, described
Insulating layer is refractory material filler material；It being set on the outside of the graphite cuvette there are one iron-clad, the graphite cuvette is contained in the iron-clad, and
Gap between the graphite cuvette and the iron-clad is tamped with graphite powder, and the iron-clad and the graphite powder tamped form institute
State protective layer.
Preferably, the graphite used in the graphite cuvette be oil immersion high power graphite, bulk density >=1.6g/cm3, resistivity
≤ 9 μ Ω * m, ash content≤0.3%, the coefficient of expansion≤2.4 (10-6) DEG C.
Preferably, a cover board is further included, the cover plate lid is closed at the top of furnace shell, insulating layer, protective layer, graphite cuvette,
Perforation is additionally provided in cover plate, the perforation is passed through for cathode and the conductive sheet being electrically connected with graphite anode, and the cover board is
Structure with internal cavities is passed through circulating cooling medium in the cavity, to reduce leading for graphite cuvette top and graphite anode
The temperature of electric piece；It is set above the cover board there are one gas sampling cover, the gas sampling cover is a loudspeaker that Open Side Down
Shape is equipped with gas outlet, gas outlet connection exhaust treatment system at the top of gas sampling cover.Electrolysis production institute can so be prevented
Environment is spilt over outside the exhaust gas of generation, improves working environment.
Preferably, the aerial cross sectional of the electrolyte bath be ellipse, round or rectangle, the Integral hollow stone
Black column sleeve is set as the shape to match with the aerial cross sectional of the electrolytic cell, is elliptical ring, annulus or rectangle frame.
Preferably, the bottom end of the Integral hollow graphite column sleeve is less than the lower end of the graphite anode and the cathode；
The medial surface of slot bottom or the graphite cuvette that the bottom end of the Integral hollow graphite column sleeve is shelved on the graphite cuvette is equipped with
One shoulder, the bottom end of the Integral hollow graphite column sleeve are held on the shoulder.
Further, the Integral hollow graphite column sleeve is to use graphite powder and bonding agent one extrusion forming either
It is molded using bulk graphite integral cutting.Wherein described Integral hollow graphite column sleeve is detachable, and each of which monoblock type is empty
The service life of stem set does not need to be too long, therefore the graphite material that quality lower price can be used cheap makes the entirety
Formula hollow plumbago column sleeve.
Its diameter of powerful electrolytic cell reaches 750cm, and the diameter of Integral hollow graphite column sleeve also has 630, and thickness reaches
To 50~70cm, weight is also bigger.Integral hollow graphite column sleeve inner wall smooth, no impetus are not easy to lifting peace very much
If dress without impetus, easily in replacement process is mounted and dismounted, forms the graphite cuvette of itself and outside machinery system damage
Wound.For example, when installing an electrolytic cell, need successively to install from outside to inside, and after graphite cuvette is installed successively, by one
Root Integral hollow graphite column set is inserted into, and installation can not be directly lifted on traditional electrolyte slot, makes the improvement cost pole of electrolytic cell
It is high.And simultaneously with the loss that electrolytic process generates, if need to change a new Integral hollow graphite column sleeve, it can only take
Overall pulling down method abolishes method；Dismounting method is by graphite anode, cathode, furnace shell, insulating layer, protective layer, graphite cuvette, crucible etc. one
One complex process removing, replace, re-assemblying, takes time and effort, and repair and replacement cost are high.The method of abolishing is by old monoblock type
Hollow plumbago column sleeve is broken into chunky shape, then moves to outside graphite cuvette.In the above process, the groove body of graphite cuvette can inevitably be made
Into serious mechanical damage.
For this purpose, the Integral hollow graphite column is arranged with the portion of putting forth effort for installation lifting, the portion of putting forth effort is set on described
The upper end of the medial surface of Integral hollow graphite column sleeve, middle part or lower end, the portion of putting forth effort is relative to the Integral hollow
At least one protruding portion or at least one recessed portion of graphite column sleeve medial surface.But, since protruding portion can influence stone very much
The discharge of the putting and arrange of black anode and cathode, feeding operation, furnace operation and corrosive exhaust gases, therefore, at one preferably
Embodiment in, it is described put forth effort portion be relative to the Integral hollow graphite column sleeve medial surface at least one recess
Portion；It is furthermore preferred that the recessed portion be set on the Integral hollow graphite column sleeve medial surface field homogeneity is influenced it is minimum,
It is that minimum lower end is influenced by electrochemical reaction loss.
Preferably, the recessed portion can be set as the concrete structures such as open-work, counterbore or notch, set on the Integral hollow stone
The lower end of black column sleeve medial surface.On the one hand it can mitigate the weight of Integral hollow graphite column sleeve, reduce lifting installation and removal
Difficulty, on the other hand, machinery lifting installation equipment can be by the way that its gripper be extend into the open-work, counterbore or notch
Place, is then lifted by crane in the vertical direction, the Integral hollow graphite column sleeve is installed in the graphite cuvette or from graphite cuvette
Interior removal.Preferably, the bottom end end face of the Integral hollow graphite column sleeve is equipped at least one convex block, the Integral hollow
Graphite column sleeve is shelved on the slot bottom of the graphite cuvette by the convex block, and the side of the convex block is notch, and the notch is formed
It is described to put forth effort portion.
Preferably, the Integral hollow graphite column sleeve lower end inside face formed a stage portion, the stage portion by
The internal diameter of the Integral hollow graphite column sleeve is expanding suddenly from top to bottom and is formed；The stage portion puts forth effort portion described in forming.
The advantageous effects of the utility model:
The utility model proposes the Integral hollow graphite that a both ends open is inserted between graphite cuvette and graphite anode
Column sleeve forms tank house in the inside of the Integral hollow graphite column sleeve, acts on the electrochemical reaction in electrolytic process
The inner wall of the graphite anode and the Integral hollow graphite column sleeve so as to avoid the consumption of graphite cuvette, reduces electrolysis system
The cost of standby rare earth metal.Occur fused salt leakage and the Integral hollow graphite column sleeve in process of production when being burnt thinning,
Outer layer graphite cuvette is not damaged, it is only necessary to the hollow column sleeve more renewed, without being made again to graphite cuvette.Cooperation should simultaneously
" putting forth effort portion " structure set by Integral hollow graphite column sleeve can be accelerated to repair speed, reduce maintenance cost.Integral hollow stone
Black column sleeve can protect graphite cuvette groove body not by electrochemical reaction, chemical reaction, fused salt corrosion and mechanical force etc. to the greatest extent
The consumption of factor.Further, since Integral hollow graphite column sleeve thickness is much larger than the coating described in background technology, (thickness is only
3mm), therefore the utility model electrolytic cell is suitable for the non-light rare earth metals such as electrolytic preparation metallic cerium, expands electrolytic cell and fits
Range.It is found through actual use, between 8-12 months, the price of graphite cuvette is the service life of traditional electrolyte slot
Between 8000-10000 members；And the price of an Integral hollow graphite column sleeve is only between 3000-4000 members, uses the longevity
Life can be 8-10 months.Even if in the case where being changed without the Integral hollow graphite column sleeve, to the consumption of outer layer graphite cuvette only
Come from the corrosion of fluoride molten salt, the service life of entire electrolytic cell can extend to 3 years as long as.
Description of the drawings
Fig. 1 is the vertical section structure diagram of prior art electrolytic cell.
Fig. 2 is the cross section structure schematic diagram of prior art electrolytic cell.
Fig. 3 is the vertical section structure diagram of the electrolytic cell of the utility model preferred embodiment.
Fig. 4 is the cross section structure schematic diagram of the electrolytic cell of the utility model preferred embodiment.
Fig. 5 A- Fig. 5 C are the structure diagram of Integral hollow graphite column sleeve in the utility model.
【Reference sign】
The prior art：
1：Cathode；2:Charge door；3：Conductive sheet；4：Insulator；5：Graphite cuvette；6：Graphite anode；7：Crucible；8：Graphite cuvette
Pedestal；9：Insulating layer；10：Box hat；
The utility model：
21：Cathode；22：Crucible；23：Graphite anode；231：The conductive sheet of graphite anode；24、24A、24B、24C：It is whole
Formula hollow plumbago column sleeve；241A、241B、241C：Upper end；242A、242B、242C：Lower end；243A、243B、243C：Put forth effort portion；
25：Graphite cuvette；251：Shoulder；26：Protective layer；261：Graphite powder filler material；262：Iron-clad；27：Insulating layer；28：Furnace shell.
Specific embodiment
It is below in conjunction with the accompanying drawings, right by specific embodiment in order to understand in order to preferably explain the utility model
The utility model is described in detail.
It is a kind of rare earth oxide fused-salt bath of the utility model preferred embodiment with reference to shown in Fig. 3 and Fig. 4,
Including furnace shell 28, insulating layer 27, protective layer 26, graphite cuvette 25, graphite anode 23, crucible 22, cathode 21, graphite anode 23 and the moon
Pole 21 inserts in graphite cuvette 25, and graphite anode 23 is set around cathode 21, and crucible 22 is placed in graphite cuvette 25, and face cathode 21
Lower section but be not attached to, for accommodate electrolyte and for accept electrolysis out metal.In graphite cuvette 25 and graphite anode 23
Between be removably inserted into the Integral hollow graphite column sleeve 24 of a both ends open, inside forms tank house, makes to be electrolysed
In journey, the electrochemical reaction between anode and cathode acts on the inner wall of graphite anode 23 and the Integral hollow graphite column sleeve 24,
The consumption of graphite cuvette is avoided whereby, reduces the cost of electrolytic preparation rare earth metal.Wherein, as shown in Figures 3 and 4, to protect as possible
" tank house " enough spaces are demonstrate,proved, outer wall and the inner wall of graphite cuvette 25 of the Integral hollow graphite column sleeve 24 are in be close to.Usually
The section of the graphite cuvette 25 of below 5000A is rounded, and the graphite cuvette 25 of more than 5000A is square.Mainly consider low battery
Graphite cuvette 25, if manufacture squarely, edge temperature have inadequate or non-uniform temperature.As shown in figure 4, this implementation
The 25 inner space section of graphite cuvette of example is ellipse, round or rectangle, at this time Integral hollow graphite column sleeve 24 be set as with
The shape that the aerial cross sectional of graphite cuvette 25 matches, as elliptical ring, annulus or rectangle frame.To ensure electric field in electrolytic process
Homogeneity further reduces energy consumption, for this purpose, the lower end of the Integral hollow graphite column sleeve 24 while graphite cuvette 25 are protected
242 are less than the lower end of graphite anode 23 and cathode 21.Preferably, 25 medial surface of graphite cuvette is set there are one shoulder 251, the monoblock type
The lower end 242 of hollow plumbago column sleeve 24 is held on the shoulder 251, and crucible 22 is sunk in the deep gouge that shoulder 251 is surrounded.At other
In embodiment, the lower end 242 of the Integral hollow graphite column sleeve 24 directly rests on the slot bottom of the graphite cuvette 25.The monoblock type is empty
Cardiolith ink column sleeve 24 can be used graphite powder and is either molded with bonding agent one extrusion forming using bulk graphite integral cutting.By
In the utility model, 24 removable and replaceable of Integral hollow graphite column sleeve, so each Integral hollow column sleeve 24 make
Do not need to be too long with the service life, therefore the graphite material that can be used quality lower price relatively inexpensive makes the Integral hollow graphite column
24。
With reference to shown in Fig. 3, for a kind of rare earth oxide fused-salt bath of the utility model preferred embodiment, installation kit
Include following steps：(1) certain thickness thermal insulation material is laid in 28 bottom of the furnace shell of steel, forms insulating layer 27；(2) by graphite
Slot 25 is put into the iron-clad 262 of drum-shaped, and the gap graphite powder filler material 261 around graphite cuvette 25 is filled secret room, iron-clad
262 and graphite powder filler material 261 form a protective layer 26；(3) tungsten crucible 22 is put into graphite cuvette 25, uses rare-earth oxidation
Object or furnace burdening are by gap filling；(4) the cover board (not shown) at top and the conductive sheet 231 of graphite anode 23 are placed；Lid
Plate lid is closed is additionally provided with perforation on furnace shell 28, insulating layer 27, protective layer 26, the top of graphite cuvette 25, cover plate, for cathode and
The conductive sheet 231 being electrically connected with graphite anode 23 passes through.Preferably, cover board is the structure (double-layer structure) with internal cavities,
Circulating cooling medium is inside passed through, the temperature of the conductive sheet 231 of 25 top of graphite cuvette and graphite anode is advantageously reduced, reduces its oxygen
Change speed and consumption.Further set a gas sampling cover again above cover board, Open Side Down for one for the gas sampling cover
Tubaeform, at the top of gas sampling cover, setting can connect the opening of exhaust treatment system.Institute in electrolytic process can so be prevented
Environment is spilt over outside the exhaust gas of generation, improves working environment.(5) an Integral hollow graphite column sleeve 24 and graphite anode 23 are pacified
It is inserted in graphite cuvette 25, cathode 21 is inserted at the perforation from cover board in graphite cuvette 25.
In the present embodiment, by taking 8000A rare earth oxide electrolytic furnaces as an example, design parameter such as following table:
To illustrate the technique effect of the utility model, now using electrolysis system for above-mentioned 8000A rare earth oxides electrolytic furnace
The concrete application of standby heavy rare earth metal illustrates：
Application examples 1：Electrolytic metal cerium：
(1) baker：It will be cleaned out in graphite cuvette 25, graphite anode 23 be installed, electrolysis material is put into crucible 22, electricity
Solve matter by 31kg LiF and 100kg CeF4Composition；Graphite with certain sectional area is placed on cathode 21 and graphite anode
Between 23, and after being in close contact with anode and cathode, at anode and cathode both ends, loading direct current makes heating graphite and melts electrolysis material.When
After the electrolysis material of thawing is contacted with anode and cathode, the graphite is taken out, logical direct current simultaneously increases voltage to keep higher heating work(
Rate makes electrolysis material be rapidly heated to normal electrolysis temperature；
(2) it is electrolysed：When the temperature in graphite cuvette 25 reaches 760 DEG C, electric current is adjusted to 7000A, voltage 12V,
CeO2Charging rate for 5g/min, continue to increase temperature, the temperature during electrolysis is maintained at 900 DEG C or so；
(3) go out metal：It is electrolysed after 4h, stops charging, continue to be electrolysed 10-15min, Faradaic current is reduced, by cathode 21
After being pushed into graphite anode 23 nearby, start to scoop out metal with titanium spoon；
(4) graphite anode 23, Integral hollow graphite column sleeve 24 are replaced and supplements electrolyte：In electrolytic process, graphite
Anode 23 is constantly consumed, and when graphite anode 23 will run out of, takes out remaining graphite anode 23 at this time and with new stone
Black anode substitution；Due to by chemical reaction and mechanical external force be lost, Integral hollow graphite column sleeve 24 work one section when
Between after also need to be replaced；In addition, the CeF of supplement 30kg is also needed to daily4With the electrolysis material of the LiF of 10kg；
(5) analytical control, polishing packaging：After rare earth metal cools down, rare earth metal is detached with electrolyte, sampling analysis
After sample qualification, rare earth metal is polished clean, packaging.
Application examples 2：Consumable catholyte produces Nd-Fe rare earth alloys：
(1) electrolyte forms：Electrolyte is by NdF3- LiF binary fluoride system and NdF3-LiF-BaF2Ternary fluoride
System is formed, wherein NdF3Mass fraction be 72%, LiF mass fraction be 21%, BaF2Mass fraction be 7%；Baker
Process is similar to application examples 1.
(2) it is electrolysed：The electrolyte of 100kg is added in graphite cuvette 25, the heater of 2-3KW is put into graphite cuvette 25 and is added
Heat slowly heats up, and after electrolyte dissolves, takes out heater, leads to direct current；When temperature rises to 900 DEG C, adjustment electric current to 5-
8A/cm2Between, and Nd is added in the speed of 3.3g/min2O3, continue to increase temperature, temperature maintained to carry out electricity at 1000 DEG C or so
Solution；
(3) graphite anode 23, Integral hollow graphite column sleeve 24 and supplement electrolysis material are replaced：With the mistake of electrolytic metal cerium
Journey is similar, after the electrolysis for carrying out a period of time, needs to carry out the replacement of graphite anode 23 and Integral hollow graphite column sleeve 24；
In addition, the Nd of supplement 20kg is also needed to daily3F, the BaF of the LiF and 3kg of 10kg2；
(4) analytical control, polishing packaging：After rare earth metal cools down, rare earth metal is detached with electrolyte, sampling analysis
After sample qualification, rare earth metal is polished clean, packaging.
Such as the above application examples 1 and application examples 2, as the graphite in electrolytic process and electrolyte are constantly consumed, need and
When " replace graphite anode 23, Integral hollow graphite column sleeve 24 and supplement electrolysis material ", however powerful graphite cuvette 25 its
Diameter reaches 750cm, and more than Integral hollow graphite column sleeve diameter 600cm, thickness reaches 50~70cm, and weight is also bigger,
Surface is smooth, and very inconvenient lifting installation easily in replacement process is mounted and dismounted, is formed the graphite cuvette of itself and outside
Machinery system damage, it is difficult to extremely complicated, the time-consuming expense of the process for directly lifting and being transformed, replace and re-assembly on traditional electrolyte slot
It is power, of high cost.
Put forth effort portion for installation lifting for this purpose, being set in the Integral hollow graphite column sleeve 24, which can be set on
The upper end 241 of outer wall and inner wall, preferably inner wall, middle part or lower end 242, concrete form can be at least one recessed on medial surface
Concave portion or protruding portion.But, since protruding portion can influence that the putting and arrange of graphite anode 23 and cathode 21, feed behaviour very much
The discharge of work, furnace operation and corrosive exhaust gases, therefore, more preferably, portion of putting forth effort is relative to the Integral hollow graphite
At least one recessed portion of the medial surface of column sleeve 24, and it is uniform to electric field to be arranged on Integral hollow graphite 24 medial surfaces of column sleeve
Property influence lower end 242 minimum, that minimum is influenced by electrochemical reaction loss.The recessed portion can be set as open-work, counterbore or notch
Wait concrete structures.The form for being set as recessed portion is better than protruding portion, on the one hand can mitigate Integral hollow graphite column sleeve
Weight reduces the difficulty of lifting installation and removal, and on the other hand, mechanical lifting appliance can be by the way that its gripper be conveniently realized
Put forth effort.Fig. 5 A to Fig. 5 C are several concrete forms of the utility model embodiment Integral hollow graphite column sleeve 24:
Such as Fig. 5 A, at least one convex block A, Integral hollow are equipped in Integral hollow graphite column sleeve 24A lower end surfaces
Graphite column sleeve 24A is shelved on the slot bottom of graphite cuvette 25 or shoulder 251 by convex block A, and the side of convex block A is notch, this is lacked
Mouth, which is formed, puts forth effort portion 243A.When installing or removing Integral hollow graphite column sleeve 24A, only need with " T-shaped or L-shaped or
Similar suspension hook declines from Integral hollow graphite column sleeve 24A centers, then snaps into and puts forth effort portion 243A, realizes convenient lifting
Installation is removed.
As shown in Figure 5 B, at least one open-work or counterbore are equipped in Integral hollow graphite column sleeve 24B lower end surfaces, it should
Open-work or counterbore composition put forth effort portion 243B.As shown in Figure 5 C, one is formed in the lower end inside face of Integral hollow graphite column sleeve 24C
A stage portion, the stage portion form this and put forth effort portion 243C.
Claims (10)
1. a kind of rare earth oxide fused-salt bath, including furnace shell, insulating layer, protective layer, graphite cuvette, graphite anode, crucible,
Cathode；The graphite anode and cathode insert in the graphite cuvette, and the graphite anode is set around the cathode, the crucible position
In the graphite cuvette and cathode described in face lower section；It is characterized in that：Between graphite cuvette and graphite anode removably
The Integral hollow graphite column sleeve of a both ends open is inserted into, the inside of the Integral hollow graphite column sleeve forms tank house,
The electrochemical reaction in electrolytic process is made to act on the inner wall of the graphite anode and the Integral hollow graphite column sleeve.
A kind of 2. rare earth oxide fused-salt bath according to claim 1, which is characterized in that the Integral hollow stone
The outer wall of black column sleeve is close to the inner wall of the graphite cuvette.
3. a kind of rare earth oxide fused-salt bath according to claim 1, which is characterized in that the cathode is tungsten cathode
Or molybdenum cathode, the crucible are tungsten crucible；The furnace shell is box hat, and the insulating layer is refractory material filler material；The graphite
It is set on the outside of slot there are one iron-clad, the graphite cuvette is contained in the iron-clad, and the gap between the graphite cuvette and the iron-clad
It is tamped with graphite powder, the iron-clad and the graphite powder tamped form the protective layer.
4. a kind of rare earth oxide fused-salt bath according to claim 1, which is characterized in that a cover board is further included,
The cover plate lid conjunction is additionally provided with perforation at the top of furnace shell, insulating layer, protective layer, graphite cuvette, in cover plate, and the perforation is for cloudy
Pole and the conductive sheet being electrically connected with graphite anode pass through, and the cover board is the structure with internal cavities, is led in the cavity
Enter circulating cooling medium, to reduce the temperature of the conductive sheet on graphite cuvette top and graphite anode；The top of the cover board is equipped with one
A gas sampling cover, that Open Side Down is tubaeform for one for the gas sampling cover, and outlet is equipped at the top of gas sampling cover
Mouthful, gas outlet connection exhaust treatment system.
5. a kind of rare earth oxide fused-salt bath according to claim 1, which is characterized in that the electrolyte bath
Aerial cross sectional is ellipse, round or rectangle, and the section of the Integral hollow graphite column sleeve is elliptical ring, annulus or rectangular
Frame.
A kind of 6. rare earth oxide fused-salt bath according to claim 1, which is characterized in that the Integral hollow stone
The bottom end of black column sleeve is less than the lower end of the graphite anode and the cathode；It shelves the bottom end of the Integral hollow graphite column sleeve
Shoulder there are one being set in the slot bottom of the graphite cuvette or the medial surface of the graphite cuvette, the Integral hollow graphite column sleeve
Bottom end be held on the shoulder.
A kind of 7. rare earth oxide fused-salt bath according to claim 1, which is characterized in that the Integral hollow stone
Black column sleeve is either to be molded using graphite powder with bonding agent one extrusion forming using bulk graphite integral cutting.
8. according to a kind of rare earth oxide fused-salt bath of claim 1-7 any one of them, which is characterized in that the entirety
Formula hollow plumbago column sleeve is equipped with the portion of putting forth effort for installation lifting, and the portion of putting forth effort is set on the interior of the Integral hollow graphite column sleeve
The upper end of side, middle part or lower end；The portion of putting forth effort is relative at least the one of the Integral hollow graphite column sleeve medial surface
A protruding portion or at least one recessed portion.
9. a kind of rare earth oxide fused-salt bath according to claim 8, which is characterized in that the recessed portion can be set as
Open-work, counterbore, notch, set on the lower end of the Integral hollow graphite column sleeve medial surface.
A kind of 10. rare earth oxide fused-salt bath according to claim 8, which is characterized in that the Integral hollow
The lower end inside face of graphite column sleeve forms a stage portion, the stage portion by the Integral hollow graphite column sleeve internal diameter from
Up to lower expanding and formed suddenly；The stage portion puts forth effort portion described in forming.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779912A (en) * | 2017-12-11 | 2018-03-09 | 凉山稀土产业技术研究院 | A kind of rare earth oxide fused-salt bath |
| CN110578155A (en) * | 2019-09-29 | 2019-12-17 | 苏州拓又达新能源科技有限公司 | automatic production line for rare earth smelting and production method thereof |
| CN114752967A (en) * | 2022-02-25 | 2022-07-15 | 包头市玺骏稀土有限责任公司 | Cluster type rare earth metal fused salt electrolysis device |
| CN110578155B (en) * | 2019-09-29 | 2024-04-26 | 苏州拓又达新能源科技有限公司 | Automatic production line for rare earth smelting and production method thereof |
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2017
- 2017-12-11 CN CN201721708309.1U patent/CN207596976U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779912A (en) * | 2017-12-11 | 2018-03-09 | 凉山稀土产业技术研究院 | A kind of rare earth oxide fused-salt bath |
| CN107779912B (en) * | 2017-12-11 | 2024-02-02 | 凉山稀土产业技术研究院 | Rare earth oxide molten salt electrolytic tank |
| CN110578155A (en) * | 2019-09-29 | 2019-12-17 | 苏州拓又达新能源科技有限公司 | automatic production line for rare earth smelting and production method thereof |
| CN110578155B (en) * | 2019-09-29 | 2024-04-26 | 苏州拓又达新能源科技有限公司 | Automatic production line for rare earth smelting and production method thereof |
| CN114752967A (en) * | 2022-02-25 | 2022-07-15 | 包头市玺骏稀土有限责任公司 | Cluster type rare earth metal fused salt electrolysis device |
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