CN105177632B - It is rare earth modified to prepare copper aluminium rare earth intermediate alloy molten salt electrolysis method and alloy - Google Patents
It is rare earth modified to prepare copper aluminium rare earth intermediate alloy molten salt electrolysis method and alloy Download PDFInfo
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- CN105177632B CN105177632B CN201510458909.6A CN201510458909A CN105177632B CN 105177632 B CN105177632 B CN 105177632B CN 201510458909 A CN201510458909 A CN 201510458909A CN 105177632 B CN105177632 B CN 105177632B
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Abstract
Copper aluminium rare earth intermediate alloy molten salt electrolysis method and alloy are prepared the present invention relates to rare earth modified.The inventive method includes：(1) raw material, (2) preelectrolysis, (3) electrolysis, (4) collection of products step are matched；Alloy of the present invention is with the AlF without the crystallization water3, NaF, LiF be supporting electrolyte, with without absorption water Al2O3、CuO、RE2O3It is active material, ratio requirement：Al2O3、CuO、RE2O3It is 2 4%, wherein Al that mixture accounts for whole electrolyte weight/mass percentage compositions2O3:CuO:RE2O3Mass ratio is 9:2:1；Remaining is AlF3, NaF, LiF salt-mixture, mixing mol ratio be：NaF:AlF3:LiF=7:4:1, wherein RE are the one kind in La, Ce, Pr, Nd element.Up to more than 90%, alloy purity is up to more than 99% for its recovery rate of iron.
Description
Technical field
The present invention relates to molten-salt electrolysis ternary intermediate alloy technology is prepared, it is specifically rare earth modified to prepare copper-aluminium-rare-earth
Between alloy molten salt electrolysis method and alloy.
Background technology
Rare earth element is the preferable modifying agent of copper-aluminium alloy, is easily combined with the hole of metallic grain boundaries, the rare earth gold of generation
There are grain boundaries in category compound, so as to crystal grain thinning, improve alloy high-temp performance and mechanical performance.
At present, preparing copper-main method of aluminium-rare-earth alloy has thermal reduction, miscible method, fused salt electrolysis process.Tradition is mixed
Molten method is mainly characterized by for Cu and rare earth each element adding miscible according to Different Weight percentage, prepares different aluminium systems and closes
Gold, this method equipment is simple, process conditions requirement is low, but its raw material for being used is single metal, high cost, and alloying component
Easy segregation, oxidizable loss, scaling loss, the alloy of preparation need a series of problems, such as remelting and double refining removal of impurities；Thermal reduction is deposited
Complicated in equipment, preparation process expendable waste residue, influence product qualities occurs while the problems such as having an impact to environment.Into
Since 21 century, Cu-Al system alloy production has been prepared towards low energy consumption, technological process be short, high financial profit direction is developed, therefore
The upsurge of new technology and method is started, wherein it is considered as a kind of very promising at present to prepare acieral using molten-salt electrolysis
Method, but be there is also in molten salt electrolysis method system selection unreasonable, electrolysate purity and rare earth element skewness
Even the problems such as, subsequent treatment is carried out more than the product of preparation.
The content of the invention
The purpose of the present invention is directed to the defect that above-mentioned prior art is present, there is provided can effectively simplify production procedure, raising
Copper-Al-RE intermediate alloys purity, what is reduced energy consumption and production costs rare earth modified prepares copper-Al-RE intermediate alloys fused salt
Electrolytic method and alloy.
Technical scheme：One kind is rare earth modified to prepare copper-Al-RE intermediate alloys, with without the crystallization water
AlF3, NaF, LiF be supporting electrolyte, with without absorption water Al2O3、CuO、RE2O3It is active material, ratio requirement：
Al2O3、CuO、RE2O3Mixture accounts for whole electrolyte weight/mass percentage compositions for 2-4%, wherein Al2O3:CuO:RE2O3Mass ratio is
9:2:1；Remaining is AlF3, NaF, LiF salt-mixture, mixing mol ratio be：NaF:AlF3:LiF=7:4:1,
Wherein RE is the one kind in La, Ce, Pr, Nd element.
A kind of rare earth modified molten salt electrolysis method for preparing copper-Al-RE intermediate alloys, comprises the following steps：
(1) raw material are matched
With the AlF without the crystallization water3, NaF, LiF be supporting electrolyte, with without absorption water Al2O3、CuO、RE2O3For
Active material, ratio requirement：Al2O3、CuO、RE2O3Mixture accounts for whole electrolyte weight/mass percentage compositions for 2-4%, wherein
Al2O3:CuO:RE2O3Mass ratio is 9:2:1；Remaining is AlF3, NaF, LiF salt-mixture, mixing mol ratio be：NaF:AlF3:LiF
=7:4:1,
Wherein RE is the one kind in La, Ce, Pr, Nd element；
(2) preelectrolysis
It is moisture and impurity in abundant removing supporting electrolyte, under conditions of 800 DEG C of temperature, 1.3~1.5V of tank voltage,
1.2~1.5h of preelectrolysis；Wherein negative electrode is tungsten metallic crucible, and anode is graphite rod；
(3) it is electrolysed
The active material of pretreatment and electrolyte are sufficiently mixed, 800-850 DEG C of temperature, tank voltage 2.5-2.8V,
Current density 0.7-0.9A/cm2Under the conditions of be electrolysed, electrolysis time 5-6h；Wherein negative electrode is tungsten metallic crucible, and anode is
Graphite rod；
(4) collection of products
Cathode deposition is collected through tungsten crucible, ingot casting, peeling, packaging.
AlF without the crystallization water3, NaF, LiF and without absorption water Al2O3、CuO、RE2O3It is by containing the crystallization water
AlF3, NaF, LiF and containing absorption water Al2O3、CuO、RE2O3Respectively 24h is dehydrated in 400 DEG C of nitrogen of temperature to obtain.
Primary outer control condition and foundation：
1st, electrolysis temperature will make the electrolysis system of set proportioning fully melt and reach appropriate activity, and OK range is
800-850℃。
2nd, tank voltage is higher than the decomposition voltage of active material and less than the decomposition voltage of fused salt support system, OK range
It is 2.5-2.8V.
3rd, electrolysis time will make the recovery rate of metal reach more than 90%, and OK range is 5-6h.
Cost of material of the present invention is low, and technological process is short, equipment is simple, does not have the discharge of solid, liquid, gas discarded object, does not cause
Secondary pollution, can be with relatively low cost directly from Al2O3、CuO、RE2O3(wherein RE=La, Ce, Pr, Nd) electrolytic preparation Cu-
Al-RE (RE is one of La, Ce, Pr, Nd) intermediate alloy；Meanwhile, the recovery rate of metal reaches more than 90%, alloy purity
Up to more than 99%, business efficiency is significantly improved.
Specific embodiment
Embodiment 1：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.3V tank voltages, preelectrolysis 1.5h；Then, will
Mass ratio Al2O3:CuO:Nd2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
2%) electrolytic cell is added, in 800 DEG C of temperature, current density 0.7A/cm2, be electrolysed 6h under the conditions of tank voltage 2.5V, received with tungsten crucible
Collection liquid alloy, ingot casting, peeling obtains Cu-Al-Nd intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 2：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.4V tank voltages, preelectrolysis 1.3h；Then, will
Mass ratio Al2O3:CuO:Nd2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
3%) electrolytic cell is added, in 825 DEG C of temperature, current density 0.8A/cm2, be electrolysed 5.5h under the conditions of tank voltage 2.7V, use tungsten crucible
Liquid alloy is collected, ingot casting, peeling obtains Cu-Al-Nd intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 3：By the mol ratio NaF after 400 DEG C of dehydration 12h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.5V tank voltages, preelectrolysis 1.2h；Then, will
Mass ratio Al2O3:CuO:Nd2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
4%) electrolytic cell is added, in 850 DEG C of temperature, current density 0.9A/cm2, be electrolysed 5h under the conditions of tank voltage 2.8V, received with tungsten crucible
Collection liquid alloy, ingot casting, peeling obtains Cu-Al-Nd intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 4：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.3V tank voltages, preelectrolysis 1.5h；Then, will
Mass ratio Al2O3:CuO:La2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
2%) electrolytic cell is added, in 800 DEG C of temperature, current density 0.7A/cm2, be electrolysed 6h under the conditions of tank voltage 2.5V, received with tungsten crucible
Collection liquid alloy, ingot casting, peeling obtains Cu-Al-La intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 5：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.4V tank voltages, preelectrolysis 1.3h；Then, will
Mass ratio Al2O3:CuO:La2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
3%) electrolytic cell is added, in 825 DEG C of temperature, current density 0.8A/cm2, be electrolysed 5.5h under the conditions of tank voltage 2.7V, use tungsten crucible
Liquid alloy is collected, ingot casting, peeling obtains Cu-Al-La intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 6：By the mol ratio NaF after 400 DEG C of dehydration 12h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.5V tank voltages, preelectrolysis 1.2h；Then, will
Mass ratio Al2O3:CuO:La2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
4%) electrolytic cell is added, in 850 DEG C of temperature, current density 0.9A/cm2, be electrolysed 5h under the conditions of tank voltage 2.8V, received with tungsten crucible
Collection liquid alloy, ingot casting, peeling obtains Cu-Al-La intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 7：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.3V tank voltages, preelectrolysis 1.5h；Then, will
Mass ratio Al2O3:CuO:Pr2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
2%) electrolytic cell is added, in 800 DEG C of temperature, current density 0.7A/cm2, be electrolysed 6h under the conditions of tank voltage 2.5V, received with tungsten crucible
Collection liquid alloy, ingot casting, peeling obtains Cu-Al-Pr intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 8：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.4V tank voltages, preelectrolysis 1.3h；Then, will
Mass ratio Al2O3:CuO:Pr2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
3%) electrolytic cell is added, in 825 DEG C of temperature, current density 0.8A/cm2, be electrolysed 5.5h under the conditions of tank voltage 2.7V, use tungsten crucible
Liquid alloy is collected, ingot casting, peeling obtains Cu-Al-Pr intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 9：By the mol ratio NaF after 400 DEG C of dehydration 12h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electricity
Solution groove, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.5V tank voltages, preelectrolysis 1.2h；Then, will
Mass ratio Al2O3:CuO:Pr2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for electrolyte gross mass
4%) electrolytic cell is added, in 850 DEG C of temperature, current density 0.9A/cm2, be electrolysed 5h under the conditions of tank voltage 2.8V, received with tungsten crucible
Collection liquid alloy, ingot casting, peeling obtains Cu-Al-Pr intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 10：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into
Electrolytic cell, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.3V tank voltages, preelectrolysis 1.5h；Then,
By mass ratio Al2O3:CuO:Ce2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for the total matter of electrolyte
2%) amount adds electrolytic cell, in 800 DEG C of temperature, current density 0.7A/cm2, be electrolysed 6h under the conditions of tank voltage 2.5V, use tungsten crucible
Liquid alloy is collected, ingot casting, peeling obtains Cu-Al-Ce intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 11：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into
Electrolytic cell, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.4V tank voltages, preelectrolysis 1.3h；Then,
By mass ratio Al2O3:CuO:Ce2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for the total matter of electrolyte
3%) amount adds electrolytic cell, in 825 DEG C of temperature, current density 0.8A/cm2, be electrolysed 5.5h under the conditions of tank voltage 2.7V, use tungsten earthenware
Crucible collects liquid alloy, and ingot casting, peeling obtains Cu-Al-Ce intermediate alloys, through analyzing alloy purity up to more than 99%.
Embodiment 12：By the mol ratio NaF after 400 DEG C of dehydration 12h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into
Electrolytic cell, is heated to 800 DEG C of fusings, and graphite anode is inserted into fused salt, under the conditions of 1.5V tank voltages, preelectrolysis 1.2h；Then,
By mass ratio Al2O3:CuO:Ce2O3=9:2:(400 DEG C are dehydrated 24h to 1 mixed oxide in nitrogen, and total amount accounts for the total matter of electrolyte
4%) amount adds electrolytic cell, in 850 DEG C of temperature, current density 0.9A/cm2, be electrolysed 5h under the conditions of tank voltage 2.8V, use tungsten crucible
Liquid alloy is collected, ingot casting, peeling obtains Cu-Al-Ce intermediate alloys, through analyzing alloy purity up to more than 99%.
Claims (4)
1. a kind of copper-Al-RE intermediate alloys of rare earth modified preparation, it is characterized in that：With the AlF without the crystallization water3、NaF、LiF
It is supporting electrolyte, with the Al without absorption water2O3、CuO、RE2O3It is active material, ratio requirement：Al2O3、CuO、RE2O3It is mixed
Compound accounts for whole electrolyte weight/mass percentage compositions for 2-4%, wherein Al2O3:CuO:RE2O3Mass ratio is 9:2:1；Remaining is
AlF3, NaF, LiF salt-mixture, mixing mol ratio be：NaF:AlF3:LiF=7:4:1,
Wherein RE is the one kind in La, Ce, Pr, Nd element.
2. the method for preparing the rare earth modified copper-Al-RE intermediate alloys described in claim 1, comprises the following steps：
(1) raw material are matched
With the AlF without the crystallization water3, NaF, LiF be supporting electrolyte, with without absorption water Al2O3、CuO、RE2O3It is activity
Material, ratio requirement：Al2O3、CuO、RE2O3Mixture accounts for whole electrolyte weight/mass percentage compositions for 2-4%, wherein Al2O3:
CuO:RE2O3Mass ratio is 9:2:1；Remaining is AlF3, NaF, LiF salt-mixture, mixing mol ratio be：NaF:AlF3:LiF=7:
4:1,
Wherein RE is the one kind in La, Ce, Pr, Nd element；
(2) preelectrolysis
It is moisture and impurity in abundant removing supporting electrolyte, under conditions of 800 DEG C of temperature, 1.3~1.5V of tank voltage, pre- electricity
1.2~1.5h of solution；Wherein negative electrode is tungsten metallic crucible, and anode is graphite rod；
(3) it is electrolysed
The active material of pretreatment and electrolyte are sufficiently mixed, in 800-850 DEG C of temperature, tank voltage 2.5-2.8V, electric current
Density 0.7-0.9A/cm2Under the conditions of be electrolysed, electrolysis time 5-6h；Wherein negative electrode is tungsten metallic crucible, and anode is graphite
Rod；
(4) collection of products
Cathode deposition is collected through tungsten crucible, ingot casting, peeling, packaging.
3. the rare earth modified method for preparing copper-Al-RE intermediate alloys according to claim 2, it is characterized in that：Without knot
The AlF of brilliant water3, NaF, LiF and without absorption water Al2O3、CuO、RE2O3It is by the AlF containing the crystallization water3, NaF, LiF and containing suction
The Al of attached water2O3、CuO、RE2O3Respectively 24h is dehydrated in 400 DEG C of nitrogen of temperature to obtain.
4. the rare earth modified method for preparing copper-Al-RE intermediate alloys according to claim 2, it is characterized in that：It is preferably real
Apply condition：By the mol ratio NaF after 400 DEG C of dehydration 24h in nitrogen:AlF3:LiF=7:4:1 salt-mixture is put into electrolytic cell, heating
To 800 DEG C of fusings, graphite anode is inserted into fused salt, under the conditions of 1.3V tank voltages, preelectrolysis 1.5h；Then, will be in nitrogen
400 DEG C are dehydrated 24h and account for the mass ratio Al of electrolyte gross mass 2%2O3:CuO:Nd2O3=9:2:1 mixed oxide is added
Electrolytic cell, in 800 DEG C of temperature, current density 0.7A/cm2, be electrolysed 6h under the conditions of tank voltage 2.5V, collect liquid with tungsten crucible and close
Gold, ingot casting, peeling obtains Cu-Al-Nd intermediate alloys, through analyzing alloy purity up to more than 99%.
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| CN107761046B (en) * | 2017-11-09 | 2019-07-30 | 江西理工大学 | A kind of fused salt electroreduction method that infiltration yttrium in aluminium copper surface is modified |
| CN107794551B (en) * | 2017-11-13 | 2019-11-08 | 江西理工大学 | A kind of copper dysprosium intermediate alloy and preparation method thereof of fused salt electrolysis codeposition preparation |
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