CN204898102U - Device of pyrogenic attack fused salt electrolysis cathode deposition - Google Patents
Device of pyrogenic attack fused salt electrolysis cathode deposition Download PDFInfo
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- CN204898102U CN204898102U CN201520620557.5U CN201520620557U CN204898102U CN 204898102 U CN204898102 U CN 204898102U CN 201520620557 U CN201520620557 U CN 201520620557U CN 204898102 U CN204898102 U CN 204898102U
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- crucible
- filter tank
- vacuum filter
- fused salt
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Abstract
The utility model relates to a device of pyrogenic attack fused salt electrolysis cathode deposition belongs to the metallurgical field of electrochemistry. The device includes resistance furnace, thermocouple, upper cover, heat preservation, sealing washer, connecting bolt, vacuum filters jar, water cooling jacket, the argon -filled tube of managing to find time, support, goes up crucible and lower crucible, the vacuum filters jar is placed in the resistance furnace, and the support is placed in the vacuum filters jar, goes up the crucible and places on the support with lower crucible, and the thermocouple is located vacuum filters jar upper portion surface department, and the upper portion of vacuum filters jar is equipped with the port and is connected with the argon -filled tube of managing to find time, and the upper end of vacuum filters jar is equipped with the cold water cover, and the upper cover passes through connecting bolt and sealing washer and vacuum filters jar sealing connection, and the heat preservation is located the upper cover lower part. This treatment of plants process operation is simple, safety, has avoided resource and the energy waste of adopting wet processing to bring, and going on of continuous production process has been guaranteed to the electrolyte of recovery, has reduced manufacturing cost, has reduced the oxygen content in the metal, has had better using value.
Description
Technical field
The utility model relates to a kind of device of pyrogenic attack fused salt electrolysis cathode deposit, this device is mainly for the treatment of the cathode deposit of reduction of fused salts and refining refractory metal, remove the molten salt electrolyte be mingled with in cathode deposit, obtain cathodic deposition metal and the ionogen of separation is returned electrowinning process recycling, belong to technical field of electrochemical metallurgy.
Background technology
Fused salt electrolysis and fused-salt electrolytic refining method are the important method of preparation and rare refractory metal of purifying, and are particularly useful for making metal titanium, zirconium, hafnium etc.High pure metal titanium is mainly used in the high-tech areas such as large-scale integrated circuit, aerospace, medical alloys.Metal zirconium, hafnium are used as the optimal structured material of nuclear reactor respectively due to himself nuclear properties and are controlled material, the compound of high pure metal zirconium hafnium is used to Coating Materials and unicircuit hafnium, along with traditional energy is to the pollution of environment, the demand of increase to zirconium hafnium material as the nuclear power demand of clean energy also increases day by day.
The production method of current industrial titanium, zirconium, hafnium mainly adopts magnesium reduction process, but fused-salt electrolytic refining method has, and flow process is short, the simple feature of operation of equipment, there is certain application, particularly fused-salt electrolytic refining method can be recovered in the scrap of a large amount of zirconium and the hafnium produced in material processing, and can synthesis high pure metal zirconium, hafnium, there is good application prospect.
Reduction of fused salts and electrorefining prepare metal titanium, zirconium, hafnium electrolyte system mainly contain fluoro-chloride system and chloride system two kinds.When adopting chloride system to carry out electrolysis, the metal chloride (TiCl obtained after can directly chlorination being purified
4, ZrCl
4, HfCl
4) as raw material, and with fluorochemical (K in fluoro-chloride system
2tiF
6, K
2zrF
6and K
2hfF
6) be raw material.No matter which kind of ionogen to carry out electrolysis with or electrorefining prepares metal, always have part molten salt electrolyte in its electrolysis cathode product to be mingled with, being about 20-30% with electrolysis of fluorides matter for its ionogen of raw material is mingled with, is that its ionogen of raw material is mingled with and is about 10-20% with chloride electrolyte.When adopting continuous fused salt electrolysis, along with the continuous taking-up of cathode product, the ionogen in electrolyzer takes needs constantly interpolation out of owing to being mingled with.
And electrolyte dissolution is generally separated to the wet processing in the aqueous solution by washing by the molten salt electrolyte be mingled with in cathode deposit.Adopt wet processing process cathode deposit Problems existing as follows: due to the certain disproportionation reaction existed between metal M (M=Ti, Zr, Hf) and M ion, to result in cathode deposit and there is " black powder " (sub-compound of metal M)." black powder " is water insoluble in water washing process, is not separated by washing with metal M, must could be obtained the metal M of higher degree by pickling process.
For metal hafnium, due to hafnium be through the separation of zirconium and hafnium of high cost after obtain, must the hafnium element be included in cathode deposit to be reclaimed (the hafnium element contained except hafnium powder in cathode deposit accounts for the 12wt% of settling gross weight).Water lotion and pickle solution are added ammoniacal liquor and obtain hafnium hydroxide precipitation, obtain hafnia through calcining, hafnia enters silicon fluoro acid potassium sintering process again and is converted into the K that can add
2hfF
6molten salt electrolyte, or hafnia carries out chlorination and obtains HfCl
4.Adopting wet processing process cathode deposit being separated the waste obtaining and all cause resource and the energy in hafnium powder and recovery hafnium element, adding operation and production cost, being not suitable for continuous prodution.
Therefore, provide a kind of cost low, the device of the pyrogenic attack fused salt electrolysis cathode deposit that can be continuously produced just becomes the technical barrier that technical field is badly in need of solution.
Utility model content
It is low that the purpose of this utility model is to provide a kind of cost, the device of the pyrogenic attack fused salt electrolysis cathode deposit that can be continuously produced.
Above-mentioned purpose of the present utility model reaches by the following technical programs:
A device for pyrogenic attack fused salt electrolysis cathode deposit, this device comprises: resistance furnace, thermopair, upper cover, thermal insulation layer, sealing-ring, joint bolt, vacuum filter tank, water jacket, argon-filled tube of finding time, support, upper crucible and lower crucible; Described vacuum filter tank is positioned in described resistance furnace, described stentplacement is in described vacuum filter tank, described upper crucible and lower crucible are positioned on described support, described thermopair is positioned at vacuum filter tank outer surface of upper place, the top of described vacuum filter tank is provided with port and is connected with described argon-filled tube of finding time, the upper end of described vacuum filter tank is provided with cold water jacket, described upper cover is tightly connected by joint bolt and sealing-ring and described vacuum filter tank, and described thermal insulation layer is positioned at described upper cover bottom.
Described resistance furnace is crucible type resistance furnace; The thermometric end of described thermopair is close to the position of crucible in vacuum filter tank outer surface of upper, correspondence.
Described upper crucible is porous ceramics crucible, has certain porosity, for holding cathode deposit; The porosity ranges of ceramic crucible can be 70 ~ 90%, and the ionogen under molten state can through ceramic crucible.
The material of described lower crucible is stainless steel, nickel or pyrolytic graphite, filters molten salt electrolyte for access.
Described thermopair is the thermopair of accurate temperature controlling.
Major advantage of the present utility model:
The utility model is for employing wet processing process fused salt electrolysis cathode deposit Problems existing, the cathode deposit adopting thermal process process fused salt electrolysis to obtain is proposed, fully mix after cathode deposit fragmentation with a certain proportion of molten salt electrolyte, then be encased in the porous ceramics crucible of certain porosity, and put into vacuum filter tank, insulation at a certain temperature makes molten salt electrolyte fusing drippage be separated with metal M, after cooling, the molten salt electrolyte of collection is turned back to continuous electrolysis operation to use, obtain metal simultaneously.This device adopts vacuum fusion to filter the molten salt electrolyte that is mixed in cathode deposit and metal separation, ionogen is returned electrowinning process, reduces processing cost, achieve the serialization of explained hereafter.
The utility model device can be continuous fused salt electrolysis and rare refractory metal reduction production cost is prepared in refining, the ionogen reclaimed ensure that the carrying out of continuous seepage operation, avoid resource and energy dissipation that wet processing cathode deposit causes, be of great practical significance.
Accompanying drawing explanation
Fig. 1 is the structural representation of the device of the utility model pyrogenic attack fused salt electrolysis cathode deposit.
Main Reference Numerals illustrates:
1 crucible electrical resistance furnace 2 epimere temperature-control heat couple
3 vacuum filter tank upper cover 4 thermal insulation layers
5 sealing-ring 6 joint bolts
7 vacuum filter tank 8 water jackets
9 find time argon-filled tube 10 support
Crucible 12 times crucibles on 11
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is further elaborated.
As shown in Figure 1, be the structural representation of the device of the utility model pyrogenic attack fused salt electrolysis cathode deposit, this device comprises crucible electrical resistance furnace 1, epimere temperature-control heat couple 2, vacuum filter tank upper cover 3, thermal insulation layer 4, sealing-ring 5, joint bolt 6, vacuum filter tank 7, water jacket 8, argon-filled tube 9 of finding time, support 10, upper crucible 11 and lower crucible 12 etc., vacuum filter tank 7 is arranged in crucible electrical resistance furnace 1, support 10, upper crucible 11 and lower crucible 12 are positioned among vacuum filter tank 7, upper crucible 11 and lower crucible 12 are positioned on support 10, the thermometric end of epimere temperature-control heat couple 2 is close to the position of crucible 11 in vacuum filter tank 7 outer surface of upper correspondence, the top of vacuum filter tank 7 is provided with port and is connected with argon-filled tube 9 of finding time, the upper end of vacuum filter tank 7 is provided with cold water jacket 8, vacuum filter tank upper cover 3 is fastened and connected with vacuum filter tank 7 by joint bolt 6 and sealing-ring 5, thermal insulation layer 4 is positioned at the bottom of vacuum filter tank upper cover 3.
Upper crucible 11 is the porous ceramics crucibles with certain porosity, for holding cathode deposit.The porosity ranges of upper crucible 11 is 70 ~ 90%, and the ionogen under molten state can through ceramic crucible.The material of lower crucible 12 is stainless steel, nickel or pyrolytic graphite etc., filters molten salt electrolyte for access.Epimere temperature-control heat couple 2 is the thermopair of accurate temperature controlling.
Crucible electrical resistance furnace 1, comprises the epimere temperature-control heat couple 2 of accurate temperature controlling for controlling the temperature of upper crucible 11.Upper crucible 11, for the ionogen holding broken fused salt electrolysis cathode deposit product He add, makes molten salt electrolyte melt by temperature control, drips from the upper crucible 11 with certain porosity, is mixed in the metal separation of ionogen in cathode deposit and deposition.Lower crucible 12, for receiving the molten salt electrolyte product of drippage from upper crucible 11, takes out after cooling and turns back to electrowinning process use.
Adopt the utility model device, mix after the fragmentation of fused salt electrolysis cathode deposit with a certain amount of sodium-chlor, Repone K, Sodium Fluoride, load in the upper crucible 11 of certain porosity, upper crucible 11 is put into vacuum filter tank 7, be first evacuated down to 10
-3pa, is warmed up to 750 DEG C gradually, and insulation, is then filled with a certain amount of argon gas to vacuum filter tank 7.Adding of fluorochemical inhibits disproportionation reaction, and original molten salt electrolyte containing low-valent metal compound (" black powder ") be mingled with drips under gravity, and cooling turns back in electrowinning process after collecting and uses.After cooling, metal is taken out, achieve being separated between electrolytic production and the molten salt electrolyte be mingled with.
First, the cathode deposit that electrolysis and electrorefining hafnium obtain is broken into certain granules degree and mixes with the NaCl-KCl-NaF ionogen of certain mol proportion, then load in the upper crucible 11 of certain porosity.
Then, the support 10 in vacuum filter tank 7 is put into successively lower crucible 12 and upper crucible 11, in upper crucible 11, load the NaCl-KCl-NaF ionogen of cathode deposit and the certain mol proportion mixed.
After treating tinning, cover vacuum filter tank upper cover 3, by sealing-ring 5, vacuum filter tank 7 seals by thermal insulation layer 4 and joint bolt 6.Vacuumize, then by argon-filled tube 9 applying argon gas of finding time to pressure-fired, on computer heating control, the temperature of crucible 11 is about 250 DEG C under an argon atmosphere, under argon gas stream takes offence atmosphere, carry out insulation dehydration 2 hours by cold water jacket 8, and then vacuumize, be filled with argon gas and keep pressure-fired.
By temperature control, the temperature of upper crucible 11 is controlled at 700-750 DEG C, make the molten salt electrolyte fusing be mingled with in cathode deposit, by the hole drippage in upper crucible 11, realize the effect with the metal separation in settling, lower crucible 12 is for receiving the ionogen of drippage from upper crucible 11.The ionogen collected after cooling turns back to electrowinning process and uses, and obtains the metal hafnium after being separated in upper crucible 11.
This device treating processes is simple to operate, safety, avoid the waste of resource and the energy adopting wet processing to bring, the ionogen reclaimed ensure that the carrying out of continuous seepage operation, reduces production cost, reduces the oxygen level in metal, has good using value.
Claims (6)
1. a device for pyrogenic attack fused salt electrolysis cathode deposit, is characterized in that: this device comprises resistance furnace, thermopair, upper cover, thermal insulation layer, sealing-ring, joint bolt, vacuum filter tank, water jacket, argon-filled tube of finding time, support, upper crucible and lower crucible; Described vacuum filter tank is positioned in described resistance furnace, described stentplacement is in described vacuum filter tank, described upper crucible and lower crucible are positioned on described support, described thermopair is positioned at vacuum filter tank outer surface of upper place, the top of described vacuum filter tank is provided with port and is connected with described argon-filled tube of finding time, the upper end of described vacuum filter tank is provided with cold water jacket, described upper cover is tightly connected by joint bolt and sealing-ring and described vacuum filter tank, and described thermal insulation layer is positioned at described upper cover bottom.
2. the device of pyrogenic attack fused salt electrolysis cathode deposit according to claim 1, is characterized in that: described resistance furnace is crucible type resistance furnace.
3. the device of pyrogenic attack fused salt electrolysis cathode deposit according to claim 1, is characterized in that: the thermometric end of described thermopair is close to the position of crucible in vacuum filter tank outer surface of upper, correspondence.
4. the device of pyrogenic attack fused salt electrolysis cathode deposit according to claim 1, is characterized in that: described upper crucible is porous ceramics crucible.
5. the device of pyrogenic attack fused salt electrolysis cathode deposit according to claim 4, is characterized in that: the porosity of described upper crucible is 70 ~ 90%.
6. the device of pyrogenic attack fused salt electrolysis cathode deposit according to claim 1, is characterized in that: the material of described lower crucible is stainless steel, nickel or pyrolytic graphite.
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|---|---|---|---|
| CN201520620557.5U CN204898102U (en) | 2015-08-17 | 2015-08-17 | Device of pyrogenic attack fused salt electrolysis cathode deposition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520620557.5U CN204898102U (en) | 2015-08-17 | 2015-08-17 | Device of pyrogenic attack fused salt electrolysis cathode deposition |
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| CN204898102U true CN204898102U (en) | 2015-12-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702437B (en) * | 2015-08-17 | 2018-08-28 | 北京有色金属研究总院 | A kind of device of pyrogenic attack molten-salt electrolysis cathode deposition |
-
2015
- 2015-08-17 CN CN201520620557.5U patent/CN204898102U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702437B (en) * | 2015-08-17 | 2018-08-28 | 北京有色金属研究总院 | A kind of device of pyrogenic attack molten-salt electrolysis cathode deposition |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190815 Address after: 101407 Beijing city Huairou District Yanqi Economic Development Zone Branch Hing Street No. 11 Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088 Beijing city Xicheng District Xinjiekou Avenue No. 2 Patentee before: General Research Institute for Nonferrous Metals |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210331 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Youyan resources and Environment Technology Research Institute (Beijing) Co.,Ltd. Address before: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: YOUYAN ENGINEERING TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |
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| TR01 | Transfer of patent right |