CN107630234B - A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis - Google Patents
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis Download PDFInfo
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Abstract
A method of scandium bearing master alloy being prepared using villaumite oxide system molten-salt electrolysis, using scandium oxide as raw material, in NaCl-CaCl2Or KCl-CaCl2In the electrolysis of fused chloride salt matter of composition, CaO or MgO is added, and electrolysis raw material Sc is added2O3Chloride-oxide fused salt mixt electrolyte is formed, using liquid aluminium as cathode, graphite is anode, and direct current electrolysis is passed under the conditions of temperature is 670~780 DEG C, and anodic current density is 0.5~1.5A/cm2, 4~10h of electrolysis time obtains liquid scandium bearing master alloy in bottom of electrolytic tank cathode.The advantages of present invention has simple process, and production cost is low, and product purity is high, is easy to continuous production, is not necessarily to reducing agent；Bottom of electrolytic tank cathode obtains liquid scandium bearing master alloy in electrolytic process simultaneously, and anode releases CO2, no other pernicious gases generate, are effectively reduced and cause seriously to pollute to environment.
Description
Technical field
The present invention relates to scandium bearing master alloy preparation technical field more particularly to a kind of utilization villaumite oxide system fused salts
The method of electrolytic preparation scandium bearing master alloy.
Background technique
Scandium is a kind of rare earth element, is that the strongest alterant of cast aluminium alloy gold grain structure and processing semi-finished product are most effective
Recrystallization inhibitor adds Microamounts of Scandium (0.1wt%~0.4wt%) into aluminium alloy, can promote crystal grain refinement, inhibits to tie again
Crystalline substance significantly improves intensity, toughness, welding and the corrosion resistance of aluminium alloy.Mo-bearing granitoid is because can significantly improve conventional aluminum
The comprehensive performance of alloy is widely used in the fields such as aerospace industry, military industry, civilian industry.However due to the negative electricity of scandium
Property is highest in rare earth metal, and chemical activity is high, and fusing point is up to 1541 DEG C, differs greatly with 660 DEG C of fusing point of aluminium, directly
It is not easy to be uniformly mixed when connecing melted aluminium-scandium alloy, the aluminium scadium compound coarse grains of formation, segregation is serious；In industrial aluminium-scandium alloy
Scandium must be added in the form of scandium bearing master alloy in production process, therefore scandium bearing master alloy is the pass for producing industrial aluminium-scandium alloy
Key raw material.
Scandium bearing master alloy preparation method has to the method for mixing, metallothermic processes and fused salt electrolysis process, wherein fused salt electrolysis process
The advantages that with simple process, production cost is low, is easy to continuous production, is not necessarily to reducing agent, it can be difficult to be used to produce
Fusing point is higher than 1000 DEG C or more of pure metal, when making cathode using liquid metal Al, Mg or Zn, in cathode deposit alloy element
Corresponding alloy can be produced.In fluoride smelt salt, with Sc2O3When for waste Al-Sc intermediate alloy, usually it is fluorinated
Object molten salt electrolyte temperature is higher, to the seriously corroded of equipment and electrode, and Sc2O3Solubility is lower in the electrolyte, is unfavorable for
Electrolytic process steady efficient operation for a long time.At present used by Chlorides molten salts electrolytic preparation scandium bearing master alloy
Electrolyte composition is mainly LiCl/NaCl-KCl-ScCl3, during electrolysis, suitable condition is controlled, Sc is made3+In cathode
On be reduced to metal simple-substance, while carrying out alloying, scandium bearing master alloy can be obtained, since electrolysis raw material uses chlorination
Scandium, the Cl on anode-It is oxidized generation chlorine, because of the not no good utilization ways of the chlorine to generation, easily environment is caused seriously
Pollution, and raw material ScCl3Preparation flow is long, and the device is complicated, high production cost.
Summary of the invention
Technical problem solved by the invention, which is to provide, a kind of prepares aluminium scandium using the molten-salt electrolysis of villaumite oxide system
The method of intermediate alloy, to solve the disadvantage in above-mentioned background technique.
Technical problem solved by the invention is realized using following technical scheme:
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
S1, using scandium oxide as raw material, in NaCl-CaCl2Or KCl-CaCl2In the electrolysis of fused chloride salt matter of composition, it is added
CaO or MgO, and electrolysis raw material Sc is added simultaneously2O3Form chloride-oxide fused salt mixt electrolyte；
S2, the chloride-oxide fused salt mixt electrolyte prepared in step S1) is placed in electrolytic cell, with liquid aluminium
For cathode, graphite is anode, connects DC power supply electrolytic chlorine compound-oxide fused salt mixt electrolyte, in bottom of electrolytic tank yin
Pole obtains liquid scandium bearing master alloy；Anode releases CO2, no other pernicious gases generations.
In the present invention, step S1) in, NaCl:CaCl2Molar ratio is 0.35~0.85:1, KCl:CaCl2Molar ratio is
0.35~3:1.
In the present invention, step S1) in, the additional amount of CaO accounts for the 5 of chloride-oxide fused salt mixt electrolyte total amount
The additional amount of~10%, MgO account for 5~10%, Sc of chloride-oxide fused salt mixt electrolyte total amount2O3Additional amount account for chlorine
Compound-oxide fused salt mixt electrolyte total amount 2~8%.
In the present invention, step S2) in, because electrolyte forms difference, electrolytic cell Inner electrolysis temperature is 670 DEG C~780 DEG C,
Actual temp selects 20 DEG C~80 DEG C on electrolyte primary crystal temperature to be electrolysed according to the liquidus temperature of electrolyte.
In the present invention, step S2) in, anodic current density is 0.5~1.5A/cm in electrolytic cell2, electrolysis time 4~
10h。
The utility model has the advantages that the present invention has simple process, production cost is low, and product purity is high, is easy to continuous production, is not necessarily to
The advantages of with reducing agent；Bottom of electrolytic tank cathode obtains liquid scandium bearing master alloy in electrolytic process simultaneously, and anode releases CO2,
No other pernicious gases generate, and are effectively reduced and cause seriously to pollute to environment.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Embodiment is closed, the present invention is further explained.
Embodiment 1
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in NaCl-CaCl2Electrolysis of fused chloride salt matter (the NaCl:CaCl of composition2Molar ratio is
In 0.35:1), the CaO for accounting for chloride-oxide fused salt mixt electrolyte total amount 5% is added and accounts for chloride-oxide mixing
The Sc of molten salt electrolyte total amount 2%2O3Chloride-oxide fused salt mixt electrolyte is formed, then mixes chloride-oxide
It closes molten salt electrolyte to be placed in electrolytic cell, using liquid aluminium as cathode, graphite is anode, connects DC power supply, electrolysis temperature 720
DEG C, anodic current density 0.5A/cm2, electrolysis time 4h obtains liquid scandium bearing master alloy in bottom of electrolytic tank cathode,
Anode releases CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 0.8%, remaining is aluminium.
Embodiment 2
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in NaCl-CaCl2Electrolysis of fused chloride salt matter (the NaCl:CaCl of composition2Molar ratio is
In 0.4:1), the CaO for accounting for chloride-oxide fused salt mixt electrolyte total amount 8% is added and accounts for chloride-oxide mixing and melts
The Sc of salt electrolyte total amount 6%2O3Chloride-oxide fused salt mixt electrolyte is formed, then mixes chloride-oxide
Molten salt electrolyte is placed in electrolytic cell, and using liquid aluminium as cathode, graphite is anode, connects DC power supply, electrolysis temperature 700
DEG C, anodic current density 0.9A/cm2, electrolysis time 6h obtains liquid scandium bearing master alloy in bottom of electrolytic tank cathode,
Anode releases CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 1.5%, remaining is aluminium.
Embodiment 3
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in NaCl-CaCl2Electrolysis of fused chloride salt matter (the NaCl:CaCl of composition2Molar ratio is
In 0.85:1), the CaO for accounting for chloride-oxide fused salt mixt electrolyte total amount 10% is added and accounts for chloride-oxide mixing
The Sc of molten salt electrolyte total amount 8%2O3Chloride-oxide fused salt mixt electrolyte is formed, then mixes chloride-oxide
It closes molten salt electrolyte to be placed in electrolytic cell, using liquid aluminium as cathode, graphite is anode, connects DC power supply, electrolysis temperature 670
DEG C, anodic current density 1.5A/cm2, electrolysis time 10h obtains liquid scandium bearing master alloy in bottom of electrolytic tank cathode,
Anode releases CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 3.2%, remaining is aluminium.
Embodiment 4
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in NaCl-CaCl2Electrolysis of fused chloride salt matter (the NaCl:CaCl of composition2Molar ratio is
In 0.8:1), the MgO for accounting for chloride-oxide fused salt mixt electrolyte total amount 10% is added and accounts for chloride-oxide mixing
The Sc of molten salt electrolyte total amount 4%2O3Chloride-oxide fused salt mixt electrolyte is formed, then mixes chloride-oxide
It closes molten salt electrolyte to be placed in electrolytic cell, using liquid aluminium as cathode, graphite is anode, connects DC power supply, electrolysis temperature 670
DEG C, anodic current density 1.5A/cm2, electrolysis time 4h obtains liquid scandium bearing master alloy in bottom of electrolytic tank cathode,
Anode releases CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 1.6%, remaining is aluminium.
Embodiment 5
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in KCl-CaCl2Electrolysis of fused chloride salt matter (the KCl:CaCl of composition2Molar ratio is
In 0.35:1), the CaO for accounting for chloride-oxide fused salt mixt electrolyte total amount 5% is added and accounts for chloride-oxide mixing
The Sc of molten salt electrolyte total amount 2%2O3Chloride-oxide fused salt mixt electrolyte is formed, then mixes chloride-oxide
It closes molten salt electrolyte to be placed in electrolytic cell, using liquid aluminium as cathode, graphite is anode, connects DC power supply, electrolysis temperature 690
DEG C, anodic current density 0.5A/cm2, electrolysis time 4h obtains liquid scandium bearing master alloy in bottom of electrolytic tank cathode,
Anode releases CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 1.0%, remaining is aluminium.
Embodiment 6
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in KCl-CaCl2Electrolysis of fused chloride salt matter (the KCl:CaCl of composition2Molar ratio is 3:1)
In, the CaO for accounting for chloride-oxide fused salt mixt electrolyte total amount 10% is added and accounts for chloride-oxide fused salt mixt electricity
Solve the Sc of matter total amount 8%2O3Chloride-oxide fused salt mixt electrolyte is formed, then by chloride-oxide fused salt mixt
Electrolyte is placed in electrolytic cell, and using liquid aluminium as cathode, graphite is anode, connects DC power supply, and electrolysis temperature is 670 DEG C, sun
Electrode current density is 1.5A/cm2, electrolysis time 10h obtains liquid scandium bearing master alloy, anode in bottom of electrolytic tank cathode
Release CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 2.8%, remaining is aluminium.
Embodiment 7
A method of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis, the specific steps are as follows:
Using scandium oxide as raw material, in KCl-CaCl2Electrolysis of fused chloride salt matter (the KCl:CaCl of composition2Molar ratio is 1:1)
In, the CaO for accounting for chloride-oxide fused salt mixt electrolyte total amount 10% is added and accounts for chloride-oxide fused salt mixt electricity
Solve the Sc of matter total amount 8%2O3Chloride-oxide fused salt mixt electrolyte is formed, then by chloride-oxide fused salt mixt
Electrolyte is placed in electrolytic cell, and using liquid aluminium as cathode, graphite is anode, connects DC power supply, and electrolysis temperature is 780 DEG C, sun
Electrode current density is 0.5A/cm2, electrolysis time 10h obtains liquid scandium bearing master alloy, anode in bottom of electrolytic tank cathode
Release CO2, no other pernicious gases generations；Wherein the mass fraction of scandium is 1.5%, remaining is aluminium.
From 1~embodiment of above-described embodiment 7 it is found that preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis
Optimal processing parameter are as follows: NaCl:CaCl2Molar ratio is 0.85:1, and the additional amount of CaO accounts for chloride-oxide fused salt mixt
10%, Sc of electrolyte total amount2O3Additional amount account for the 8% of chloride-oxide fused salt mixt electrolyte total amount, electrolysis temperature
It is 670 DEG C, anodic current density 1.5A/cm2, electrolysis time 10h.
Basic principles and main features and major advantage of the invention have been shown and described above.The technical staff of the industry
It should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (7)
1. a kind of method for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis, which is characterized in that specific step
It is rapid as follows:
S1, using scandium oxide as raw material, in NaCl-CaCl2Or KCl-CaCl2In the electrolysis of fused chloride salt matter of composition, CaO is added
Or MgO, and electrolysis raw material Sc is added simultaneously2O3Form chloride-oxide fused salt mixt electrolyte；
S2, the chloride-oxide fused salt mixt electrolyte prepared in step S1) is placed in electrolytic cell, is yin with liquid aluminium
Pole, graphite are anode, connect DC power supply electrolytic chlorine compound-oxide fused salt mixt electrolyte, obtain in bottom of electrolytic tank cathode
To liquid scandium bearing master alloy；Anode releases CO2, no other pernicious gases generations.
2. a kind of side for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis according to claim 1
Method, which is characterized in that step S1) in, NaCl:CaCl2Molar ratio is 0.35~0.85:1, KCl:CaCl2Molar ratio be 0.35~
3:1.
3. a kind of side for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis according to claim 1
Method, which is characterized in that step S1) in, the additional amount of CaO account for chloride-oxide fused salt mixt electrolyte total amount 5~
10%, Sc2O3Additional amount account for the 2~8% of chloride-oxide fused salt mixt electrolyte total amount.
4. a kind of side for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis according to claim 1
Method, which is characterized in that step S1) in, the additional amount of MgO account for chloride-oxide fused salt mixt electrolyte total amount 5~
10%.
5. a kind of side for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis according to claim 1
Method, which is characterized in that step S2) in, electrolytic cell Inner electrolysis temperature is 670 DEG C~780 DEG C.
6. a kind of side for preparing scandium bearing master alloy using villaumite oxide system molten-salt electrolysis according to claim 1
Method, which is characterized in that step S2) in, anodic current density is 0.5~1.5A/cm in electrolytic cell2, 4~10h of electrolysis time.
7. according to claim 1~3,5~6 described in any item a kind of preparing aluminium scandium using the molten-salt electrolysis of villaumite oxide system
The method of intermediate alloy, which is characterized in that the best work of scandium bearing master alloy is prepared using villaumite oxide system molten-salt electrolysis
Skill parameter are as follows: NaCl:CaCl2Molar ratio is 0.85:1, and it is total that the additional amount of CaO accounts for chloride-oxide fused salt mixt electrolyte
10%, Sc of amount2O3Additional amount account for the 8% of chloride-oxide fused salt mixt electrolyte total amount, electrolysis temperature is 670 DEG C,
Anodic current density is 1.5A/cm2, electrolysis time 10h.
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| CN1514042A (en) * | 2003-08-21 | 2004-07-21 | 中国铝业股份有限公司 | Production method of high purity aluminium scandium alloy |
| CN1664170A (en) * | 2004-12-24 | 2005-09-07 | 北京科技大学 | Method for producing aluminium and aluminium alloy by low temperature electrolysis |
| WO2006079353A1 (en) * | 2005-01-25 | 2006-08-03 | Alcan Technology & Management Ltd. | Method for the production of an aluminum-scandium master alloy |
| CN1936085A (en) * | 2006-09-19 | 2007-03-28 | 东北大学 | Method for preparing aluminium and aluminium alloy by low temperature molten-salt electrolysis |
| EP3081671A1 (en) * | 2014-01-27 | 2016-10-19 | Sumitomo Metal Mining Co., Ltd. | Scandium concentrate production method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1514042A (en) * | 2003-08-21 | 2004-07-21 | 中国铝业股份有限公司 | Production method of high purity aluminium scandium alloy |
| CN1664170A (en) * | 2004-12-24 | 2005-09-07 | 北京科技大学 | Method for producing aluminium and aluminium alloy by low temperature electrolysis |
| WO2006079353A1 (en) * | 2005-01-25 | 2006-08-03 | Alcan Technology & Management Ltd. | Method for the production of an aluminum-scandium master alloy |
| CN1936085A (en) * | 2006-09-19 | 2007-03-28 | 东北大学 | Method for preparing aluminium and aluminium alloy by low temperature molten-salt electrolysis |
| EP3081671A1 (en) * | 2014-01-27 | 2016-10-19 | Sumitomo Metal Mining Co., Ltd. | Scandium concentrate production method |
Non-Patent Citations (2)
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| Electrochemical production of Al–Sc alloy in CaCl2–Sc2O3 molten salt;Masanori Harata et al.,;《Journal of Alloys and Compounds》;20080813;第474卷;124–130 |
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