CN104611732B - Air cooling cathode, molten salt electrolyzer and electrolysis method - Google Patents
Air cooling cathode, molten salt electrolyzer and electrolysis method Download PDFInfo
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Abstract
The invention discloses an air cooling cathode, a molten salt electrolyzer and an electrolysis method. The air cooling cathode comprises a cathode connecting rod and a cathode plate arranged at the lower end of the cathode connecting rod, wherein a gas channel is arranged in the cathode connecting rod and an opening, which penetrates through the upper end of the cathode connecting rod, of the gas channel is a gas inlet; a cooling channel is formed in the cathode plate and an opening, which penetrates through the upper end of the cathode plate, of the cooling channel is a gas outlet; the gas channel is communicated with the cooling channel. The molten salt electrolyzer is electrolyzing equipment with the air cooling cathode as an electrolysis cathode. The electrolysis method is a method applying the molten salt electrolyzer. The air cooling cathode is beneficial to studying the precipitation process of a metal in the cathode, and thus the optimal electrolysis parameters are conveniently found, and the electrolysis efficiency is improved. According to the air cooling cathode, the molten salt electrolyzer and the electrolysis method disclosed by the invention, in the process of manufacturing the cathode, only the gas channel is needed to be added, so that the air cooling cathode is simple in structure and good in cooling effect, does not need large design investment and has strong application and popularization prospect.
Description
Technical field
The invention belongs to field of metallurgy, and in particular to a kind of gas-cooled cathode, fused salt electrolysis apparatus and electrolytic method.
Background technology
Fused salt electrolysis process is the important method of non-ferrous metal metallurgy, particularly with the system of the higher metal of active or fusing point
It is standby, for example：Magnesium, aluminum, titanium, zinc, zirconium etc..The principle of molten-salt electrolysis is to pass through ion gain and loss on electrode in the presence of unidirectional current
Electrolysate is electronically generated, metallic product is generally obtained on negative electrode.In electrolytic process, precipitation of the metallic product on negative electrode
With collect, have a strong impact on the efficiency of electrolysis.Therefore research metallic product is electric for improving in negative electrode precipitation and the shape characteristic for collecting
Solution efficiency is significant.
At present, for the precipitation process of liquid product, such as liquid magnesium has been studied electrolysis under different situations and has separated out Product characteristics
Report, such as public publications of in August, 2006《Magnesium eletrolysis process technology》In page 225 to page 231 and page 461 extremely
Page 469 discloses a kind of employing quartz ampoule to contain the research that electrolyte observes liquid magnesium in negative electrode precipitation process, by
It is that liquid product is observed in which, electrode position and mode of heating make its observing effect not good, and works as presence in electrolyte
When coloured ion or impurity, electrolyte light transmission is deteriorated, or even does not observe the morphology change that magnesium is separated out and collected completely.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of gas-cooled cathode that can be cooled down rapidly liquid product, its
Beneficial to research metal negative electrode precipitation process.
In order to solve above-mentioned technical problem, the invention provides a kind of gas-cooled cathode, including cathode connecting bar and the moon is arranged on
The minus plate of pole connecting rod lower end；The inside of the cathode connecting bar is provided with gas passage, and gas passage passes cathode connecting bar upper end
It is open as gas access；The inside of the minus plate is provided with cooling duct, and it is gas that cooling duct passes the opening of minus plate upper end
Body is exported；The gas passage is connected with cooling duct.
It is further that the gas passage is connected with the bottom of cooling duct.
Be further, the cooling duct be with its with gas passage connectivity part as labyrinth entrance, and with gas outlet
For the labyrinth passage of labyrinth outlet.
It is further that the labyrinth passage is " returning " font labyrinth channel.
It is further that the cooling duct is that multiple serpentine passages are joined end to end the serpentine channel of composition each other.
It is further that the wall thickness everywhere of the minus plate is equal.
Present invention also offers a kind of fused salt electrolysis apparatus that can observe liquid product precipitation process, including reacting furnace,
Anode and electrolyte；Also include cold air supply device and above-mentioned any one gas-cooled cathode；The gas-cooled cathode is connected by negative electrode
Bar is arranged on reacting furnace；Minus plate part is submerged in electrolyte, and gas outlet is located at the outside of electrolyte；The cold air is supplied
Device is answered to be connected with gas access.
It is further that the fused salt electrolysis apparatus also include water electrolytic gas conduit, exhaust duct and heater；The electricity
Solution gas conduit is arranged on reacting furnace, and setting is submerged in the electrolyte in lower end；The anode is arranged on water electrolytic gas conduit
Inside, setting is submerged in the electrolyte and without departing from the lower end of water electrolytic gas conduit in the lower end of anode；The water electrolytic gas are led
Pipe is provided with water electrolytic gas outlet, and the water electrolytic gas outlet is positioned at the outside of reacting furnace；The exhaust duct is arranged on reaction
On stove, and the inside of reacting furnace is made to connect with outside air；The heater is arranged on reacting furnace to be used for heating electrolyte.
Present invention also offers a kind of electrolytic method that can observe liquid product precipitation process, which applies above-mentioned any one
Plant fused salt electrolysis apparatus to be electrolysed, comprise the following steps：
Step one, heating electrolyte and by its temperature control in X ± 10 DEG C；
Step 2, when the temperature of electrolyte is (X+5) DEG C～(X+10) DEG C, anode and gas-cooled cathode are powered carries out electricity
Solution；
Step 3, electrolysis 0.5 hour～1 hour after, from cold air supply device to the gas passage of gas-cooled cathode in be passed through
Noble gases, by noble gases by the temperature control of electrolyte in (X-10) DEG C～(X-5) DEG C；
Power-off after step 4, continuation are electrolysed 0.5 hour～1 hour stops electrolysis, obtains solid metallic product；
Wherein, melting temperatures of the X for metallic product；The depth that minus plate submerges in electrolyte is less than minus plate height
3/4ths.
It is further, the depth that the minus plate submerges in electrolyte for minus plate height 2/3rds；It is described lazy
Property gas be argon；The flow of the noble gases exported from cold air supply device is 10m3/ h～20m3/h。
The invention has the beneficial effects as follows：By being passed through cooling noble gases in gas passage, noble gases flow through cold
But passage makes minus plate lower the temperature, and the liquid product quick solidification produced in can making electrolytic process is separated out and obtains solid metallic product
Thing；So as to the shape characteristic that can be collected by the process of observation metallic product precipitation and metallic product, to determine different condition shape
Precipitation and the morphology change collected of the metal in negative electrode under condition, finds out optimal electrolytic parameter, improves electrolytic efficiency.Gas leads to
Road is connected with the bottom of cooling duct, is made connectivity part farthest apart from gas outlet, is fully caught a cold beneficial to minus plate.Cooling duct
For labyrinth passage or serpentine channel so that the time of staying of the cooling gas in minus plate is longer, so that heat exchange
More fully, cooling effect is more preferably.The equal electrolyte that is more conducive to of the wall thickness everywhere of minus plate carries out heat exchange with cooling with gas,
Good cooling results.Water electrolytic gas conduit can avoid cooling gas from affecting the purity of water electrolytic gas in being mixed into water electrolytic gas；Tail
Discharge of the airway beneficial to cooling gas.By using the research of the invention, current efficiency can be improved.The invention by
Gas passage, simple structure is added to put into without the need for big design in negative electrode manufacturing process, good cooling results, with stronger
Application prospect.
Description of the drawings
Fig. 1 is the side structure schematic view of gas-cooled cathode；
Fig. 2 is a kind of structural representation of embodiment that minus plate line A-A along Fig. 1 is cut open；
Fig. 3 is the structural representation of the another embodiment that minus plate line A-A along Fig. 1 is cut open；
Fig. 4 is the structural representation of fused salt electrolysis apparatus；
It is labeled as in figure：Cathode connecting bar 1, gas passage 11, gas access 12, minus plate 2, cooling duct 21, gas go out
Mouth 22, reacting furnace 3, anode 4, electrolyte 5, the outlet 61, exhaust duct 7 of water electrolytic gas conduit 6, water electrolytic gas and heater 8.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.
As shown in figure 1, gas-cooled cathode, including cathode connecting bar 1 and the minus plate 2 for being arranged on 1 lower end of cathode connecting bar；Minus plate
2 lower ends that can be arranged on cathode connecting bar 1 by connected modes such as screw, bolt or welding, minus plate 2 can also be fabricated to
Integral structure of the cathode connecting bar 1 for an entirety；The gas-cooled cathode is carried out using existing molten-salt electrolysis negative electrode making material
Make；The inside of the cathode connecting bar 1 is provided with gas passage 11, and it is gas that gas passage 11 passes the opening of 1 upper end of cathode connecting bar
Body entrance 12；Cooling gas enters the gas-cooled cathode from gas access 12, and is transmitted by gas passage 11；Cooling gas
Generally from the noble gases of room temperature；The inside of the minus plate 2 is provided with cooling duct 21, and cooling duct 21 passes minus plate 2
The opening of upper end is gas outlet 22；The embodiment of cooling duct 21 can have various, for example：The passage of maze-type structure,
The sinuous passage of formula structure, the passage of straight-through structure directly will arrange a cavity as cooling duct inside minus plate 2
21；It is in order to avoid when minus plate 2 submerges in electrolyte 5, electrolyte 5 enters gas that gas outlet 22 is located at the upper end of minus plate 2
Outlet 22, it is possible to improve the depth that minus plate 2 submerges in electrolyte 5；The gas passage 11 is connected with cooling duct 21；Cause
It is the reaction of high-temperature electrochemistry for Molten, in electrolytic process, electrolyte 5 is and the gas-cooled cathode in the condition of high temperature
2 part of minus plate invade electrolyte 5 in be electrolysed, minus plate used 2 generally also be in the condition of high temperature；By gas passage 11
The cooling for transmitting carries out heat exchange with gas into cooling duct 21 and minus plate 2 makes minus plate 2 lower the temperature, and then reduces
The temperature of electrolyte 5, so that the liquid metal product quick solidification produced in electrolytic process is separated out obtains solid metallic product.
Solid metallic product is beneficial to laboratory observation, the shape characteristic collected by the process and metallic product of observing metallic product precipitation,
Can determine that metal, in precipitation and the morphology change collected of negative electrode, finds out optimal electrolytic parameter under different condition situation,
Improve electrolytic efficiency.
In order that minus plate 2 is fully caught a cold, the gas passage 11 is connected with the bottom of cooling duct 21, is so cooled down
Passage 21 is farthest apart from gas outlet 22 with 11 connectivity part of gas passage, improves the rate of heat exchange of cooling gas.
In order that heat exchange is more abundant, cooling effect more preferably, as shown in Fig. 2 the cooling duct 21 is with itself and gas
11 connectivity part of passage is labyrinth entrance, and the labyrinth passage exported as labyrinth with gas outlet 22；So arrange and cause cooling
Longer with the time of staying of the gas in minus plate 2, rate of heat exchange is higher.Specifically, the labyrinth passage is " returning " font
Labyrinth channel；" returning " font labyrinth channel is mutually formed comprising connection by multiple " time " font passages.The labyrinth passage
Can also be by multiple hexagonal groups into cellular labyrinth channel, the labyrinth channel that is made up of multiple polygons etc..
In order to reach more preferable heat exchange effect, we can be as shown in Figure 3 multiple so that cooling duct 21 is set to
The serpentine passage serpentine channel that first place is connected to form each other；Certainly, cooling duct 22 can also be set to other shapes by us
Serpentine channel, for example：Multiple end to end " M " shapes, " N " shape or Z-shaped passage, multiple " M " shapes, " N " shape or Z-shaped are led to
The passage of the end to end combination in any in road.
There is bigger contact area in view of cooling gas and minus plate 2, so that cooling gas takes away more heat
Amount, the wall thickness everywhere of the minus plate 2 are equal, for example：Minus plate 2 is designed to into a housing, its internal chamber is used as cold
But passage 21.
As shown in figure 4, fused salt electrolysis apparatus, including reacting furnace 3, anode 4, electrolyte 5, cold air supply device and above-mentioned
Any one gas-cooled cathode；Charge door and outlet is usually provided with reacting furnace 3；The gas-cooled cathode passes through cathode connecting bar 1
It is arranged on reacting furnace 3；Anode 4 is general to be made from graphite material；The bar segment and cathode connecting bar 1 of generally anode 4 is fixed
On the bell of reacting furnace 3；2 part of minus plate is submerged in electrolyte 5, and gas outlet 22 is located at the outside of electrolyte 5；Gas
Body outlet 22 can not be submerged in electrolyte 5；The cold air supply device is connected with gas access 12；Cold air supply device passes through
Gas output end is connected with gas access 12 so that gas-cooled cathode is connected with cold air supply device.
Preferably, then as shown in figure 4, the fused salt electrolysis apparatus also include water electrolytic gas conduit 6, exhaust duct 7 and heating
Device 8；The water electrolytic gas conduit 6 is arranged on reacting furnace 3, and lower end is submerged and is arranged in electrolyte 5；The anode 4 sets
Put in the inside of water electrolytic gas conduit 6, the lower end of anode 4 is submerged in being arranged on electrolyte 5 and without departing from water electrolytic gas conduit 6
Lower end；During electrolysis, anode 4 generally has water electrolytic gas to produce, for example：Electrolysis MgCl2Chlorine can be produced in anode；Water electrolytic gas are led
The water electrolytic gas that the electrolysis of anode 4 is produced can be collected and be conveyed to pipe 6, it is ensured that the purity of water electrolytic gas, it is to avoid water electrolytic gas are cold
But other gaseous contaminations in gas or reacting furnace 3 are used；The water electrolytic gas conduit 6 is provided with water electrolytic gas outlet 61, the electricity
Solution gas outlet 61 is located at the outside of reacting furnace 3；Water electrolytic gas outlet 61 is generally connected with water electrolytic gas collection device, electrolytic gas
The water electrolytic gas collected are delivered to water electrolytic gas outlet 61 and are collected by water electrolytic gas collection device again by body canal 6；The tail
Airway 7 is arranged on reacting furnace 3, and the inside of reacting furnace 3 is connected with outside air；Exhaust duct 7 be mainly used in by from
The cooling that gas outlet 22 flows out is discharged with gas, it is to avoid pressure increase in reacting furnace 3；The heater 8 is arranged on reaction
It is used for heating electrolyte 5 on stove 3；Adding apparatus 8 can select thermocouple.The fused salt electrolysis apparatus are generally used for liquid product analysis
Go out the experimentation of process.
Using the electrolytic method are electrolysed by above-mentioned any one fused salt electrolysis apparatus, comprise the following steps：
Step one, heating electrolyte 5 and by its temperature control in X ± 10 DEG C；
Step 2, when the temperature of electrolyte 5 is (X+5) DEG C～(X+10) DEG C, anode 4 and gas-cooled cathode are powered to be carried out
Electrolysis；
Step 3, electrolysis 0.5 hour～1 hour after, from cold air supply device to the gas passage 11 of gas-cooled cathode in lead to
Enter noble gases, by noble gases by the temperature control of electrolyte 5 in (X-10) DEG C～(X-5) DEG C；
Power-off after step 4, continuation are electrolysed 0.5 hour～1 hour stops electrolysis, obtains solid metallic product；
Wherein, melting temperatures of the X for metallic product；The depth that minus plate 2 submerges in electrolyte 5 is high less than minus plate 2
3/4ths of degree.Electrolyte 5 is made to lower the temperature by being passed through noble gases, so that electrolysis obtains solid metallic product, Jin Erneng
Liquid product precipitation process is enough observed, optimal electrolytic parameter is found out, electrolytic efficiency is improved.
Preferably, the depth that the minus plate 2 submerges in electrolyte 5 for 2 height of minus plate 2/3rds；The inertia
Gas is argon；The flow of the noble gases exported from cold air supply device is 10m3/ h～20m3/h。
Embodiment (observation liquid magnesium collects process)
Electrolysis procedure is carried out by above-mentioned fused salt electrolysis apparatus：
Step one, heating electrolyte 5 and by its temperature control at 650 ± 10 DEG C；
Step 2, electrolyte 5 temperature be 655 DEG C～660 DEG C when, anode 4 and gas-cooled cathode are electrolysed；
Step 3, electrolysis 0.5 hour after, from cold air supply device to the gas passage 11 of gas-cooled cathode in be passed through room temperature argon
Gas, by argon by the temperature control of electrolyte 5 at 645 DEG C～650 DEG C；
Power-off after step 4, continuation are electrolysed 0.5 hour stops electrolysis, obtains solid metallic product；
Wherein, the depth that minus plate 2 submerges in electrolyte 5 for 2 height of minus plate 2/3rds；From cold air supply device
The flow of middle output argon is 20m3/h；Electrolyte 5 is existing electrolytic magnesium electrolyte.
Commercial production can be instructed by the use of the present invention：To in electrolytic process separate out magnesium observation understand, the remittance of magnesium
Collection state is degenerated afterwards as the increase of electric current density first improves, and will strictly control the electric current density of anode and cathode in process of production；
The negative electrode magnesium for having rust collects uneven, the aggregation of bulk magnesium locally occurs, and is mingled with electrolyte, and the clean negative electrode in surface
Magnesium granules are evenly distributed, and it is good compared with have rust to collect situation.When steel negative electrode is assembled, must ensure that electrode surface is clean；
In design level, magnesium collects state preferably, works as MgCl2Concentration is reduced to when designing offline, and the state of collecting of magnesium seriously becomes
It is bad.The MgCl of electrolysis bath will be strictly controlled aborning2Concentration, it is impossible to the MgCl less than 8%2Concentration design load.
Claims (8)
1. electrolytic method, it is characterised in that：It is electrolysed using following fused salt electrolysis apparatus；
The fused salt electrolysis apparatus, including reacting furnace (3), anode (4), electrolyte (5), cold air supply device and gas-cooled cathode；
The gas-cooled cathode, including cathode connecting bar (1) and is arranged on the minus plate (2) of cathode connecting bar (1) lower end；The negative electrode connects
The inside of bar (1) is provided with gas passage (11), and it is gas access that gas passage (11) passes the opening of cathode connecting bar (1) upper end
(12)；The inside of minus plate (2) is provided with cooling duct (21), and cooling duct (21) pass the opening of minus plate (2) upper end
For gas outlet (22)；Gas passage (11) are connected with cooling duct (21)；
The gas-cooled cathode is arranged on reacting furnace (3) by cathode connecting bar (1)；Minus plate (2) partly submerges electrolyte (5)
In, and gas outlet (22) is located at the outside of electrolyte (5)；The cold air supply device is connected with gas access (12)；
The electrolytic method comprises the following steps：
Step one, heating electrolyte (5) and by its temperature control in X ± 10 DEG C；
Step 2, when the temperature of electrolyte (5) is (X+5) DEG C～(X+10) DEG C, anode (4) and gas-cooled cathode energization are carried out
Electrolysis；
Step 3, electrolysis 0.5 hour～1 hour after, from cold air supply device to the gas passage (11) of gas-cooled cathode in be passed through
Noble gases, by noble gases by the temperature control of electrolyte (5) in (X-10) DEG C～(X-5) DEG C；
Step 4, continue electrolysis 0.5 hour～1 hour after power-off, stop electrolysis, obtain solid metallic product；
Wherein, melting temperatures of the X for metallic product；The depth that minus plate (2) submerges in electrolyte (5) is less than minus plate (2)
3/4ths of height.
2. electrolytic method as claimed in claim 1, it is characterised in that：Gas passage (11) and cooling duct (21) are most
Lower end connects.
3. electrolytic method as claimed in claim 1, it is characterised in that：Cooling duct (21) are with itself and gas passage
(11) connectivity part is labyrinth entrance, and the labyrinth passage exported as labyrinth with gas outlet (22).
4. electrolytic method as claimed in claim 3, it is characterised in that：The labyrinth passage is " returning " font labyrinth channel.
5. electrolytic method as claimed in claim 1, it is characterised in that：Described cooling duct (21) be multiple serpentine passages that
The serpentine channel of this composition that joins end to end.
6. electrolytic method as claimed in claim 1, it is characterised in that：The wall thickness everywhere of minus plate (2) is equal.
7. the electrolytic method as described in claim 1,2,3,4,5 or 6, it is characterised in that：The fused salt electrolysis apparatus also include
Water electrolytic gas conduit (6), exhaust duct (7) and heater (8)；Water electrolytic gas conduit (6) are arranged on reacting furnace (3)
On, and lower end submerges and is arranged in electrolyte (5)；Anode (4) are arranged on the inside of water electrolytic gas conduit (6), anode (4)
Lower end submerge be arranged on electrolyte (5) in and without departing from the lower end of water electrolytic gas conduit (6)；Water electrolytic gas conduit (6)
Water electrolytic gas outlet (61) are provided with, water electrolytic gas outlet (61) are located at the outside of reacting furnace (3)；The exhaust duct
(7) it is arranged on reacting furnace (3), and the inside of reacting furnace (3) is connected with outside air；Heater (8) are arranged on
It is used for heating electrolyte (5) on reacting furnace (3).
8. electrolytic method as claimed in claim 1, it is characterised in that：The depth that minus plate (2) are submerged in electrolyte (5)
For 2/3rds of minus plate (2) height；The noble gases are argon；The noble gases exported from cold air supply device
Flow is 10m3/ h～20m3/h。
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| US5200054A (en) * | 1992-07-22 | 1993-04-06 | The United States Of America As Represented By The United States Department Of Energy | Ice electrode electrolytic cell |
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| CN202201991U (en) * | 2011-06-15 | 2012-04-25 | 金川集团有限公司 | Cathode plate with cooling system |
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| US3226310A (en) * | 1960-12-19 | 1965-12-28 | Ciba Ltd | Electrolytic fusion cells and method of operating the same |
| CN101248217A (en) * | 2005-08-30 | 2008-08-20 | 株式会社大阪钛技术 | Method for electrolysis of molten salt, electrolytic cell, and process for producing ti using said method |
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