CN106978612A - A kind of metallurgical method of metallic compound - Google Patents
A kind of metallurgical method of metallic compound Download PDFInfo
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- CN106978612A CN106978612A CN201710155751.4A CN201710155751A CN106978612A CN 106978612 A CN106978612 A CN 106978612A CN 201710155751 A CN201710155751 A CN 201710155751A CN 106978612 A CN106978612 A CN 106978612A
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- metallic compound
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/04—Electrolytic production, recovery or refining of metals by electrolysis of melts of magnesium
-
- 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
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
-
- 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
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- Chemical Kinetics & Catalysis (AREA)
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- Electrolytic Production Of Metals (AREA)
Abstract
A kind of metallurgical method of metallic compound.Step is to regard metal compound powders or compressing metallic compound test piece and afflux bluk recombination as negative electrode, anode is used as using graphite, in inert atmosphere or air atmosphere, in the alkali halide of melting, alkaline-earth halide or the two mixture, decomposition voltage is 1.4 ~ 3.2V, it is electrolysed 1 ~ 4 hour under the operating temperature higher than the fusing point of correspondence metallic product, cathodic reduction is corresponding molten metal or molten alloy.The present invention provides a kind of electrolytic process reaction rate, the electrolytic metallurgy of reduction product impurity of effectively being lifted and gives birth to metalliferous method.
Description
Technical field
The present invention relates to a kind of metallurgical method of metallic compound, more particularly to a kind of electrolytic metallurgy gives birth to metalliferous side
Method.
Background technology
With green regenerative energy sources（Such as solar energy, wind energy, geothermal energy and nuclear energy）The lasting rising researched and developed Deng electric energy, clearly
Clean efficient electrochemistry New Metallurgical Technique will play an increasingly important role.Modern Aluminium Industry production use Hall-angstrom
Shandong cryolite-alumina molten salt electrolysis, i.e., the fluoride salt based on ice crystal is as flux, and aluminum oxide is molten matter composition multiphase
Electrolyte system, liquid aluminium is obtained after electrolysis in negative electrode.The current production technology of rare earth metal is equally that rare earth oxide is molten
Solution deposits the rare earth metal melted in corresponding molten salt electrolyte, after electrolysis in negative electrode.Both the above electrolytic process is all
It is that, by the process of liquid phase presoma to liquid product, it is limited in the solubility of molten salt system that its production is limited by oxide.Meanwhile,
Especially for the electrolysis of rare earth metal, there is the problem of shuttling electric discharge in rare-earth cation, cause electrolytic efficiency low in fused salt
Under.Molten-salt electrolysis solid-oxide and the electrolysis of superhigh temperature molten oxide are that closely wide concerned, environment is friendly in the world during the last ten years
Good electrochemistry New Metallurgical Technique.The core that molten-salt electrolysis solid-oxide prepares metal/semiconductor/alloy is with solid oxide
Thing is negative electrode and is electrolysed at less than the temperature of melting point metal and the voltage of fused salt decomposition.Directly solid compounds predecessor is existed
Electrochemical cathode is converted into solid product, has the advantages that flow is short, not long dendrite, but this electrochemical conversion process be related to it is multiple
Gu it is miscellaneous it is solid/, reaction and the Transport And Transformation step of solid/liquid interfaces and solid liquid phase.Solid-state electrochemistry process reaction speed is partially slow, and
And diffusion coefficient is slow in solids for the oxygen in solid-oxide.Therefore, it is electrolysed under high decomposition voltage for a long time, negative electrode
In product still can the ppm high contents of encumbrance thousand oxygen residual.Meanwhile, during product is isolated and purified, metallic particles table
Layer is oxidized again, further increases the oxygen content of product.The molten oxide electricity that the electrolysis of superhigh temperature molten oxide is used
Solution matter has the advantages that steam is forced down under high temperature, high, relatively small to anode material aggressivity to oxide solubility, and in pole
Hold reaction rate under high temperature fast.But, the fusing point of oxide is universal very high, also causes this method need to be in thermal extremes situation
Lower to carry out, the continuous industrialization production for this method proposes great challenge.
The content of the invention
It is anti-that the purpose of the present invention is that the deficiency existed for above-mentioned prior art there is provided one kind can effectively lift electrolytic process
Answer speed, reduce the metalliferous method of electrolytic metallurgy life of product impurity.
The purpose of the present invention is achieved through the following technical solutions：By metal compound powders or compressing gold
Belong to compound test piece with afflux bluk recombination as negative electrode, using graphite as anode, in inert atmosphere or air atmosphere, molten
In alkali halide, alkaline-earth halide or the two mixture for melting, decomposition voltage is 1.4 ~ 3.2V, higher than correspondence
It is electrolysed 1 ~ 4 hour under the operating temperature of the fusing point of metallic product, cathodic reduction is corresponding molten metal or molten alloy.
The mixtures that the alkali halide constitutes for the one or several kinds of Li, Na, K, Rb or Cs halide.
The mixtures that the alkaline-earth halide constitutes for the one or several kinds of Mg, Ca, Sr or Ba halide.
The halide is Cl or F one kind or both mixture.
The metallic compound is a kind of or many of Zn, Al, Mg, Sn, In, Ga, Ge, lanthanide oxide or sulfide
Kind.
The test piece is that commercial metals compound powder suppress under 2 ~ 20MPa of pressure, the sintering at 600 ~ 900 DEG C of temperature
Form.
The collector is titanium, stainless steel, molybdenum, tungsten, nickel or graphite of the fusing point higher than the crucible shape of reaction temperature.
The present invention principle be：Research concentrates on solid-phase compound → solid metallic process, its reaction speed and production at present
Quality is limited by solid phase mass transport process.Meanwhile, relative to traditional molten-salt electrolysis technique, the dispensing of compounds precursors is not
Its solubility in molten salt electrolyte is limited by, is also not in the shuttle electric discharge influence of respective metal cation.In the present invention,
Solid compounds → liquid metal process, the i.e. anion that be extracted as of metal is transmitted the diffusion for being changed into solid liquid interface by solid phase,
It is expected to accelerate reaction process to improve cell reaction speed.Because operating temperature is higher than metallic product fusing point, products therefrom melts
It is fine and close ingot after body cooling, only surface needs cleaning, can not only simplify subsequent treatment process, can be with high degree
Avoid subsequent treatment from reoxidizing, so as to reduce the impurity content of product.
Brief description of the drawings
Fig. 1 is the X diffracting spectrums of the metallic zinc of embodiment 1.
Fig. 2 is the stereoscan photograph of the metallic zinc of embodiment 1.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, these descriptions are intended merely to preferably say
The bright present invention, rather than limitation of the present invention.
Embodiment 1
Commercially available ZnS powder is put into after graphite crucible and is wound on long molybdenum filament as negative electrode, using graphite rod as anode, is rubbed with melting
You compare 1:1 NaCl and KCl mixture are electrolyte, in argon gas atmosphere, and temperature is 700 DEG C, and voltage is 2.8V, electrolysis 1
Hour, negative electrode graphite crucible is proposed into fused salt liquid level after the completion of electrolysis and is cooled to after normal temperature takes out product in a cell, warp
Distilled water is cleaned, and obtains metallic zinc ball in 60 DEG C of vacuum dryings.Fig. 1 is XRD spectrum；Fig. 2 is SEM spectrum.S contents in product
Analysis result is 100ppm.
Embodiment 2
By commercially available Al2O3Powder is pressed into diameter 20mm under 6MPa, thickness 3mm test piece, in atmosphere 700 DEG C of sintering 2
Hour, obtain Al2O3Test piece.Test piece is put into stainless steel crucible to be wound on long stainless steel bar as negative electrode with stainless steel wire again,
Using graphite rod as anode, to melt mol ratio 1:1 CaCl2And SrCl2Mixture be electrolyte, in argon gas atmosphere, temperature
For 850 DEG C, voltage is 3.0V, is electrolysed 3 hours, and negative electrode stainless steel crucible is proposed into fused salt liquid level and in electrolysis after the completion of electrolysis
It is cooled in groove after normal temperature and takes out product, metal aluminium ball is obtained through washes of absolute alcohol, and in 60 DEG C of vacuum dryings.The oxygen of product
Content analysis result is 1000ppm.
Embodiment 3
Commercially available MgS powder is put into titanium crucible to be wound on titanium rod as negative electrode with titanium silk again, using graphite rod as anode, to melt
Mol ratio 1:1 MgCl2Mixture with RbCl is electrolyte, in argon gas atmosphere, and temperature is 700 DEG C, and voltage is 2.4V, electricity
Solution 2 hours, proposes fused salt liquid level by cathode titanium crucible after the completion of electrolysis and is cooled to after normal temperature takes out product in a cell, warp
Distilled water is cleaned, and obtains magnesium metal ball in 60 DEG C of vacuum dryings.
Embodiment 4
By commercially available SnO2Powder is put into molybdenum crucible and is wound in again with molybdenum filament as negative electrode on molybdenum bar, using graphite crucible as anode, with
Melt mol ratio 1:1:1 LiCl, NaCl, KCl mixture are electrolyte, in argon gas atmosphere, and temperature is 400 DEG C, voltage
For 2.2V, it is electrolysed 2 hours, negative electrode molybdenum crucible proposes fused salt liquid level and be cooled in a cell after normal temperature after the completion of electrolysis to take
Go out product, cleaned through distilled water, and metal Sn balls are obtained in 60 DEG C of vacuum dryings.
Embodiment 5
By commercially available Yn2O3Powder is put into molybdenum crucible and is wound in again with molybdenum filament as negative electrode on molybdenum bar, using graphite crucible as anode, with
Melt mol ratio 1:2:1 LiCl, NaCl, CsCl mixture are electrolyte, in argon gas atmosphere, and temperature is 450 DEG C, voltage
For 2.0V, it is electrolysed 1.5 hours, negative electrode molybdenum crucible is proposed into fused salt liquid level after the completion of electrolysis and is cooled in a cell after normal temperature
Product is taken out, is cleaned through distilled water, and metal Yn balls are obtained in 60 DEG C of vacuum dryings.
Embodiment 6
By commercially available Ga2O3Powder is put into tungsten crucible and is wound in again with tungsten filament as negative electrode on tungsten bar, using graphite crucible as anode, with
Melt mol ratio 1:2:1 LiCl, NaCl, BaCl2Mixture be electrolyte, in argon gas atmosphere, temperature be 450 DEG C, electricity
Press as 2.0V, be electrolysed 1.5 hours, negative electrode molybdenum crucible is proposed into fused salt liquid level after the completion of electrolysis and normal temperature is cooled in a cell
After take out product, cleaned through distilled water, and in normal-temperature vacuum drying obtain metal Ga balls.
Embodiment 7
By commercially available Ge2O3Powder is put into tungsten crucible and is wound in again with tungsten filament as negative electrode on tungsten bar, using graphite crucible as anode, with
Melt mol ratio 2:1 CaCl2、CaF2Mixture be electrolyte, in argon gas atmosphere, temperature is 1000 DEG C, and voltage is
2.0V, is electrolysed 2 hours, and negative electrode molybdenum crucible is proposed into fused salt liquid level after the completion of electrolysis and taking-up after normal temperature is cooled in a cell
Product, is cleaned through distilled water, and obtains metal Ge balls in 60 DEG C of vacuum dryings.
Embodiment 8
By commercially available La2O3Powder is put into tungsten crucible and is wound in again with tungsten filament as negative electrode on tungsten bar, using graphite crucible as anode, with
Melt mol ratio 3:1 CaCl2、CaF2Mixture be electrolyte, in argon gas atmosphere, temperature be 950 DEG C, voltage is 3.2V,
Electrolysis 4 hours, proposes fused salt liquid level by negative electrode molybdenum crucible after the completion of electrolysis and is cooled to after normal temperature takes out product in a cell,
Cleaned through distilled water, and vacuum drying is spent in 60 DEG C and obtain metal La balls.
Embodiment 9
By commercially available Ce2O3Powder is put into tungsten crucible and is wound in again with tungsten filament as negative electrode on tungsten bar, using graphite crucible as anode, with
Melt mol ratio 2:1 CaCl2、CaF2Mixture be electrolyte, in argon gas atmosphere, temperature be 950 DEG C, voltage is 3.2V,
Electrolysis 4 hours, proposes fused salt liquid level by negative electrode molybdenum crucible after the completion of electrolysis and is cooled to after normal temperature takes out product in a cell,
Cleaned through distilled water, and vacuum drying is spent in 60 DEG C and obtain metal Ce balls.
Embodiment 10
By commercially available MgS, Al2O3Powder is put into tungsten crucible and is wound in again with tungsten filament on tungsten bar as the moon after mixing in proportion
Pole, using graphite crucible as anode, to melt mol ratio 3:1 CaCl2, NaCl mixture be electrolyte, in argon gas atmosphere,
Temperature is 750 DEG C, and voltage is 2.8V, is electrolysed 3 hours, and negative electrode molybdenum crucible is proposed into fused salt liquid level and in electrolytic cell after the completion of electrolysis
In be cooled to after normal temperature and take out product, cleaned through distilled water, and vacuum dryings spent in 60 DEG C and obtain magnesium alloy ball.
Embodiment 11
Tungsten crucible is put into after commercially available ZnS, MgS powder is mixed in proportion to be wound in as negative electrode on tungsten bar with tungsten filament again,
Using graphite crucible as anode, to melt mol ratio 3:1 NaCl, KCl mixture are electrolyte, in argon gas atmosphere, temperature
For 750 DEG C, voltage is 2.6V, is electrolysed 4 hours, and negative electrode molybdenum crucible is proposed into fused salt liquid level and cold in a cell after the completion of electrolysis
But to product is taken out after normal temperature, cleaned through distilled water, and vacuum dryings are spent in 60 DEG C and obtain zinc magnesium alloy ball.
Embodiment 12
By commercially available In2O3、SnO2Powder is put into tungsten crucible and is wound in again with tungsten filament on tungsten bar as the moon after mixing in proportion
Pole, using graphite crucible as anode, to melt mol ratio 1:2:1 LiCl, NaCl, KCl mixture are electrolyte, in argon gas gas
In atmosphere, temperature be 500 DEG C, voltage is 2.2V, be electrolysed 2 hours, after the completion of electrolysis by negative electrode molybdenum crucible propose fused salt liquid level and
It is cooled in electrolytic cell after normal temperature and takes out product, cleaned through distilled water, and vacuum drying is spent in 60 DEG C and obtains indium stannum alloy ball.
Claims (7)
1. a kind of metallurgical method of metallic compound, it is characterized in that step is as follows：By metal compound powders or compressing
Metallic compound test piece and afflux bluk recombination as negative electrode, using graphite as anode, in inert atmosphere or air atmosphere,
In the alkali halide of melting, alkaline-earth halide or the two mixture, decomposition voltage be 1.4 ~ 3.2V, higher than
It is electrolysed 1 ~ 4 hour under the operating temperature of the fusing point of correspondence metallic product, cathodic reduction is that corresponding molten metal or melting are closed
Gold.
2. the metallurgical method of metallic compound according to claim 1, it is characterized in that the alkali halide be Li,
The mixture of one or several kinds of compositions of Na, K, Rb or Cs halide.
3. the metallurgical method of metallic compound according to claim 1, it is characterized in that the alkaline-earth halide be Mg,
The mixture of one or several kinds of compositions of Ca, Sr or Ba halide.
4. the metallurgical method of the metallic compound according to claim 1,2 or 3, it is characterized in that the halide is Cl or F
One kind or both mixture.
5. the metallurgical method of metallic compound according to claim 1, it is characterized in that the metallic compound be Zn, Al,
Mg, Sn, In, Ga, Ge, the one or more of lanthanide oxide or sulfide.
6. the metallurgical method of metallic compound according to claim 1, it is characterized in that the test piece is commercial metals chemical combination
Thing powder is suppressed under 2 ~ 20MPa of pressure, is sintered and is formed at 600 ~ 900 DEG C of temperature.
7. the metallurgical method of metallic compound according to claim 1, is higher than instead it is characterized in that the collector is fusing point
Answer titanium, stainless steel, molybdenum, tungsten, nickel or the graphite of the crucible shape of temperature.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541754A (en) * | 2017-09-08 | 2018-01-05 | 董晓 | A kind of preparation method of thermal crack resistant magnesium alloy |
| CN108118364A (en) * | 2018-01-19 | 2018-06-05 | 广东省稀有金属研究所 | A kind of method that metal and magnesium sulfide are prepared by metal sulfide |
| CN108677218A (en) * | 2018-04-26 | 2018-10-19 | 西安建筑科技大学 | A kind of method that molten-salt electrolysis prepares metallic zinc |
| CN108754544A (en) * | 2018-05-29 | 2018-11-06 | 昆明理工大学 | A method of using melten salt electriochemistry method thick indium is recycled from useless ITO powder |
| CN109732187A (en) * | 2019-01-29 | 2019-05-10 | 东北大学 | A kind of method of melten salt electriochemistry assistant metal welding |
| CN110429356A (en) * | 2019-07-15 | 2019-11-08 | 华中科技大学 | A kind of recovery method and device of liquid metal cell |
| CN111501069A (en) * | 2020-06-02 | 2020-08-07 | 株洲科能新材料有限责任公司 | Molten salt electrolysis purification method of crude gallium |
| CN112391653A (en) * | 2020-11-16 | 2021-02-23 | 中国科学院上海应用物理研究所 | Method for reducing rare earth oxide into rare earth metal simple substance in chloride molten salt system |
| CN112941567A (en) * | 2018-07-10 | 2021-06-11 | 东北大学 | Electrochemical method and apparatus for high temperature molten salt electrolysis in humid atmosphere |
| CN114481228A (en) * | 2022-02-21 | 2022-05-13 | 中国工程物理研究院材料研究所 | Method for preparing uranium-titanium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541754A (en) * | 2017-09-08 | 2018-01-05 | 董晓 | A kind of preparation method of thermal crack resistant magnesium alloy |
| CN108118364A (en) * | 2018-01-19 | 2018-06-05 | 广东省稀有金属研究所 | A kind of method that metal and magnesium sulfide are prepared by metal sulfide |
| CN108677218A (en) * | 2018-04-26 | 2018-10-19 | 西安建筑科技大学 | A kind of method that molten-salt electrolysis prepares metallic zinc |
| CN108754544A (en) * | 2018-05-29 | 2018-11-06 | 昆明理工大学 | A method of using melten salt electriochemistry method thick indium is recycled from useless ITO powder |
| CN112941567A (en) * | 2018-07-10 | 2021-06-11 | 东北大学 | Electrochemical method and apparatus for high temperature molten salt electrolysis in humid atmosphere |
| CN112941567B (en) * | 2018-07-10 | 2024-02-23 | 东北大学 | Electrochemical method and device for high-temperature molten salt electrolysis in humid atmosphere |
| CN109732187B (en) * | 2019-01-29 | 2020-07-21 | 东北大学 | Method for electrochemically assisting metal welding through molten salt |
| CN109732187A (en) * | 2019-01-29 | 2019-05-10 | 东北大学 | A kind of method of melten salt electriochemistry assistant metal welding |
| CN110429356A (en) * | 2019-07-15 | 2019-11-08 | 华中科技大学 | A kind of recovery method and device of liquid metal cell |
| CN111501069A (en) * | 2020-06-02 | 2020-08-07 | 株洲科能新材料有限责任公司 | Molten salt electrolysis purification method of crude gallium |
| CN112391653A (en) * | 2020-11-16 | 2021-02-23 | 中国科学院上海应用物理研究所 | Method for reducing rare earth oxide into rare earth metal simple substance in chloride molten salt system |
| CN112391653B (en) * | 2020-11-16 | 2021-11-05 | 中国科学院上海应用物理研究所 | Method for reducing rare earth oxide into rare earth metal simple substance in chloride molten salt system |
| CN114481228A (en) * | 2022-02-21 | 2022-05-13 | 中国工程物理研究院材料研究所 | Method for preparing uranium-titanium alloy |
| CN114481228B (en) * | 2022-02-21 | 2023-11-24 | 中国工程物理研究院材料研究所 | Method for preparing uranium titanium alloy |
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