CN101376992A - Method for preparing magnesium lithium alloy by fused salt electrolysis process - Google Patents
Method for preparing magnesium lithium alloy by fused salt electrolysis process Download PDFInfo
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- CN101376992A CN101376992A CNA2008100134373A CN200810013437A CN101376992A CN 101376992 A CN101376992 A CN 101376992A CN A2008100134373 A CNA2008100134373 A CN A2008100134373A CN 200810013437 A CN200810013437 A CN 200810013437A CN 101376992 A CN101376992 A CN 101376992A
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Abstract
The invention relates to a method for preparing magnesium-lithium alloy through a molten salt electrolytic method, which is characterized in that mixed carbonate or mixed nitrate containing lithium salt serves as electrolyte; the mixed salt is put into an electrobath with the cathode made of magnesium, to be heated to electrolysis temperature; and then the mixed salt is electrolyzed with the current density of 0.05A/cm<2> to 0.3A/cm<2>; after electrolysis, the cathode mixed with metal lithium is taken out; next, a new cathode magnesium plate or a magnesium rod is put in, the electrolysis is continued, to obtain the magnesium-lithium alloy with the content of metal lithium of 1 weight percent to 15 weight percent. In the method, non-chloride series molten salt electrolyte and raw materials are adopted, and no chlorine is produced during the electrolysis process; the electrolysis temperature is no higher than 600 DEG C which is low, the energy consumption is reduced, and the production, operation and management are easy.
Description
Technical field
The invention belongs to material science, be specifically related to the method for preparing magnesium-lithium alloy by molten salt electrolysis.
Background technology
Magnesium lithium alloy is an alloy system the lightest in the structured material.Magnesium lithium alloy is because to have density low, and excellent specific properties such as intensity height become the ideal structure material in fields such as aerospace and weapon industry.
The method of producing magnesium lithium alloy at present mostly is the blending method.High-purity lithium is produced out in the first electrolysis of this method, with the magnesium melting, casts magnesium lithium alloy then.This technical process is long, and the lithium rate of recovery is low, and (lithium density is 0.534g/cm owing to lithium density is little
3, magnesium density is 1.74g/cm
3), fusing point low (the lithium fusing point is 180 ℃, and the magnesium fusing point is 650 ℃), be easy to reunite at one, be difficult to produce the magnesium lithium alloy of stable components.So to the method for mixing not is to produce the most economical reasonable method of magnesium lithium alloy.
Compare with the blending method, one step of direct electrolysis method is produced magnesium lithium mother alloy, utilizes this mother alloy and aluminium melting again, casts the magnesium lithium alloy of required composition, has reduced the oxidational losses of lithium secondary cast, improved the lithium rate of recovery, and technology stability is good.Therefore adopt one step of fused salt electrolysis process to produce that magnesium lithium mother alloy prepares high purity, high performance application magnesium lithium alloy seems particularly attractive.
Fused salt electrolysis process is produced magnesium lithium mother alloy, and to adopt KCl-LiCl usually be basic electrolyte system (weight ratio is 1:1), with liquid magnesium or solid-state magnesium is the negative electrode of electrolyzer, with LiCl is raw material, in 450～630 degrees centigrade temperature range, under galvanic effect, produce chlorine at anode, produce the magnesium lithium alloy of content 11～35% at negative electrode.
Because the vapour pressure of LiCl is very big, when electrolysis temperature was higher, volatilization loss was very big.Also will utilize vacuum unit with the sucking-off of anodic gas product chlorine during electrolysis simultaneously, this can further strengthen the volatilization loss of lithium chloride.And chlorine is very strong to the corrodibility of electrolyzer during high temperature, and shorten the work-ing life of electrolyzer.If the generation chlorine leakage all can cause serious injury to the person and environment.
Summary of the invention
At above technical problem, the invention provides the method for following preparing magnesium-lithium alloy by molten salt electrolysis.
The present invention adopts mixed carbonic acid salt system or mixed nitrate salt system, passes through preparing magnesium-lithium alloy by molten salt electrolysis.Concrete steps are:
1, mixed carbonate system molten salt electrolysis legal system is equipped with magnesium lithium alloy
With salt of wormwood (K
2CO
3) and Quilonum Retard (Li
2CO
3) mix, blending ratio be Quilonum Retard account for the mixed carbonate total mass 26～52%, salt of wormwood accounts for 48～74% of mixed carbonate total mass.
It is the electrolyzer of magnesium that mixed carbonate is placed the negative electrode material, and the electrolyzer that mixed carbonate is housed is heated to 510～600 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.05～0.3A/cm during electrolysis then
2, electrolysis time is 0.4～1.6h; The negative electrode that will be mixed with metallic lithium then takes out, and puts into new negative electrode magnesium plate or magnesium rod, proceeds electrolysis, and obtaining metallic lithium content is the magnesium lithium alloy of 1～15wt%.
Wherein when the change in concentration of the Quilonum Retard in the mixed carbonate reaches 3wt%, replenish Quilonum Retard in mixed carbonate, magnitude of recruitment is no more than 8wt% by the change in concentration of Quilonum Retard in mixed carbonate.
Salt of wormwood and Quilonum Retard be thorough drying before use, requires moisture less than 0.1wt%.
2, mixed nitrate system molten salt electrolysis legal system is equipped with magnesium lithium alloy
With saltpetre (KNO
3) and lithium nitrate (LiNO
3) mix, blending ratio be lithium nitrate account for the mixed nitrate total mass 20～90%, saltpetre accounts for 10～80% of mixed nitrate total mass.Add electrolysis raw material Quilonum Retard then, add-on accounts for 3～8wt% of whole materials by Quilonum Retard, obtains mixed electrolyte.
It is the electrolyzer of magnesium that mixed electrolyte is placed the negative electrode material, and the electrolyzer that mixed electrolyte is housed is heated to 150～400 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.05～0.3A/cm during electrolysis then
2, electrolysis time is 0.15～0.5h, and the negative electrode that will be mixed with metallic lithium then takes out, and puts into new negative electrode magnesium plate or magnesium rod, proceeds electrolysis, and obtaining metallic lithium content is the magnesium lithium alloy of 1～15wt%.
Wherein when the concentration of the Quilonum Retard in the mixed electrolyte is 3wt%, replenish Quilonum Retard in mixed electrolyte, magnitude of recruitment is 3～8wt% by the concentration of Quilonum Retard in mixed electrolyte.
Quilonum Retard, saltpetre and lithium nitrate be thorough drying before use, requires moisture less than 0.1wt%.
3, electrolyzer
The electrolytic cell assembly that the present invention uses is multicavity tray, and the anode material is a graphite, and the negative electrode material is magnesium plate or magnesium rod; Electrolytic cell assembly has two graphite anodes and a negative electrode magnesium plate, and negative electrode is placed on two anodic middles, and the electrolyzer material is a stainless steel, and the corundum insulcrete is laid in the bottom, and electrolyzer adopts outside heat-supplying mode.
The negative electrode magnesium plate that the present invention adopts or the purity of magnesium rod are more than the 99.8wt%.
The quality of lithium content and negative electrode magnesium plate makes the magnesium lithium alloy product reach predeterminated level by regulating current density and electrolysis time in the at first predetermined magnesium lithium alloy of the present invention.
Compared with the prior art, beneficial effect of the present invention is: 1, adopt the molten salt electrolyte and the raw material of achloride system, do not produce chlorine in the electrolytic process; 2, the electrolysis temperature of conventional electrolysis method production magnesium lithium alloy is usually more than 650 ℃, and electrolysis temperature is no more than 600 ℃ in present method, and electrolysis temperature is low, and energy expenditure reduces, and produces easy handling and management; 3, design of electrolysis cells is reasonable, and electrolytic process is stablized easy to control.
Description of drawings
The electrolytic cell assembly synoptic diagram that Fig. 1 adopts for the method for preparing magnesium-lithium alloy by molten salt electrolysis of the present invention, among the figure 1, graphite anode, 2, negative electrode magnesium plate, 3, mixing salt, 4, cell body, 5, contact conductor.
Embodiment
It below is the preferred embodiment of the present invention.
The saltpetre that the present invention adopts and the purity of lithium nitrate are more than the 99wt%.The salt of wormwood that the present invention adopts and the purity of Quilonum Retard are more than the 99wt%.
Salt of wormwood, Quilonum Retard, saltpetre and lithium nitrate thorough drying before use requires moisture less than 0.1wt% among the present invention.
Adopt electrolytic cell assembly as shown in Figure 1, magnesium plate negative electrode 2 is placed on the middle of two graphite anodes 1, and cell body 4 materials are stainless steel, and the corundum insulcrete is laid in the bottom, and electrolyzer adopts outside heat-supplying mode; Anode is connected power supply with negative electrode by contact conductor 5, the cell body 4 inner mixing salts 3 of placing.
Wherein negative electrode magnesium plate area is 200cm
2, thickness is 0.5cm, quality is 87g.
Salt of wormwood and Quilonum Retard are mixed, blending ratio be Quilonum Retard account for the mixed carbonate total mass 26%, salt of wormwood accounts for 74% of mixed carbonate total mass.
The 1000g mixed carbonate is placed electrolyzer, the electrolyzer that mixed carbonate is housed is heated to 550 ℃, the mixed carbonate fusing continues to be heated to 580 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.05A/cm during electrolysis then
2, after electrolysis is finished, the negative electrode that is mixed with metallic lithium is taken out, put into new negative electrode magnesium plate then, proceed electrolysis.The duration of service of each new magnesium plate in electrolyzer is 0.4～0.6h.
When the concentration of the Quilonum Retard in the mixed carbonate is 23wt%, in mixed carbonate, replenish Quilonum Retard, magnitude of recruitment is that every 0.5h adds 6g, and keep Quilonum Retard in mixed carbonate concentration in 18～34wt%.
Metallic lithium content is 1wt% in the magnesium lithium alloy that obtains.
Adopt electrolytic cell assembly with embodiment 1, wherein negative electrode magnesium plate area is 200cm
2, thickness is 0.5cm, quality is 87g.
Salt of wormwood and Quilonum Retard are mixed, blending ratio be Quilonum Retard account for the mixed carbonate total mass 47%, salt of wormwood accounts for 53% of mixed carbonate total mass.
The 1000g mixed carbonate is placed electrolyzer, the electrolyzer that mixed carbonate is housed is heated to 490 ℃, the mixed carbonate fusing continues to be heated to 530 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.1A/cm during electrolysis then
2, after electrolysis is finished, the negative electrode that is mixed with metallic lithium is taken out, put into new negative electrode magnesium plate then, proceed electrolysis.The duration of service of each new magnesium plate in electrolyzer is 1.3～1.6h.
When the concentration of the Quilonum Retard in the mixed carbonate is 44wt%, in mixed carbonate, replenish Quilonum Retard, magnitude of recruitment is that every 0.5h adds 13g, and keep Quilonum Retard in mixed carbonate concentration in 39～55wt%.
Metallic lithium content is 8wt% in the magnesium lithium alloy that obtains.
Adopt electrolytic cell assembly with embodiment 1, wherein negative electrode magnesium plate area is 200cm
2, thickness is 0.5cm, quality is 87g.
Salt of wormwood and Quilonum Retard are mixed, blending ratio be Quilonum Retard account for the mixed carbonate total mass 52%, salt of wormwood accounts for 48% of mixed carbonate total mass.
The 1000g mixed carbonate is placed electrolyzer, the electrolyzer that mixed carbonate is housed is heated to 550 ℃, the mixed carbonate fusing continues to be heated to 580 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.1A/cm during electrolysis then
2, after electrolysis is finished, the negative electrode that is mixed with metallic lithium is taken out, put into new negative electrode magnesium plate then, proceed electrolysis.The duration of service of each new magnesium plate in electrolyzer is 0.9～1.4h.
When the concentration of the Quilonum Retard in the mixed carbonate is 49wt%, in mixed carbonate, replenish Quilonum Retard, magnitude of recruitment is that every 0.5h adds 35g, and keep Quilonum Retard in mixed carbonate concentration in 44～60wt%.
Metallic lithium content is 15wt% in the magnesium lithium alloy that obtains.
Adopt electrolytic cell assembly with embodiment 1, wherein negative electrode magnesium plate area is 200cm
2, thickness is 0.2cm, quality is 35g.
Saltpetre and lithium nitrate are mixed, blending ratio be lithium nitrate account for the mixed nitrate total mass 20%, saltpetre accounts for 80% of mixed nitrate total mass.Add electrolysis raw material Quilonum Retard then, add-on accounts for the 8wt% of whole materials by Quilonum Retard, obtains mixed electrolyte.
The 1000g mixed electrolyte is placed electrolyzer, the electrolyzer that mixed electrolyte is housed is heated to 220 ℃, the mixed electrolyte fusing continues to be heated to 300 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.05A/cm during electrolysis then
2, after electrolysis is finished, the negative electrode that is mixed with metallic lithium is taken out, put into new negative electrode magnesium plate then, proceed electrolysis.The duration of service of each new magnesium plate in electrolyzer is 0.15～0.2h.
When the concentration of the Quilonum Retard in the mixed electrolyte is 3wt%, in mixed electrolyte, replenish Quilonum Retard, magnitude of recruitment is that every 0.5h adds 6g, and keeps Quilonum Retard concentration in mixed electrolyte to be no more than 8wt%.
Metallic lithium content is 1wt% in the magnesium lithium alloy that obtains.
Adopt electrolytic cell assembly with embodiment 1, wherein negative electrode magnesium plate area is 200cm
2, thickness is 0.2cm, quality is 35g.
Saltpetre and lithium nitrate are mixed, blending ratio be lithium nitrate account for the mixed nitrate total mass 32%, saltpetre accounts for 68% of mixed nitrate total mass.Add electrolysis raw material Quilonum Retard then, add-on accounts for the 5wt% of whole materials by Quilonum Retard, obtains mixed electrolyte.
The 1000g mixed electrolyte is placed electrolyzer, the electrolyzer that mixed electrolyte is housed is heated to 135 ℃, the mixed electrolyte fusing continues to be heated to 250 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.2A/cm during electrolysis then
2, after electrolysis is finished, the negative electrode that is mixed with metallic lithium is taken out, put into new negative electrode magnesium plate then, proceed electrolysis.The duration of service of each new magnesium plate in electrolyzer is 0.35～0.5h.
When the concentration of the Quilonum Retard in the mixed electrolyte is 3wt%, in mixed electrolyte, replenish Quilonum Retard, magnitude of recruitment is that every 0.5h adds 25g, and keeps Quilonum Retard concentration in mixed electrolyte to be no more than 8wt%.
Metallic lithium content is 10wt% in the magnesium lithium alloy that obtains.
Embodiment 6
Adopt electrolytic cell assembly with embodiment 1, wherein negative electrode magnesium plate area is 200cm
2, thickness is 0.2cm, quality is 35g.
Saltpetre and lithium nitrate are mixed, blending ratio be lithium nitrate account for the mixed nitrate total mass 90%, saltpetre accounts for 10% of mixed nitrate total mass.Add electrolysis raw material Quilonum Retard then, add-on accounts for the 3wt% of whole materials by Quilonum Retard, obtains mixed electrolyte.
The 1000g mixed electrolyte is placed electrolyzer, the electrolyzer that mixed electrolyte is housed is heated to 245 ℃, the mixed electrolyte fusing continues to be heated to 400 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.3A/cm during electrolysis then
2, after electrolysis is finished, the negative electrode that is mixed with metallic lithium is taken out, put into new negative electrode magnesium plate then, proceed electrolysis.The duration of service of each new magnesium plate in electrolyzer is 0.35～0.5h.
When the concentration of the Quilonum Retard in the mixed electrolyte is 3wt%, in mixed electrolyte, replenish Quilonum Retard, magnitude of recruitment is that every 0.5h adds 35g, and keeps Quilonum Retard concentration in mixed electrolyte to be no more than 8wt%.
Metallic lithium content is 15wt% in the magnesium lithium alloy that obtains.
Claims (8)
1, a kind of method of preparing magnesium-lithium alloy by molten salt electrolysis is characterized in that: salt of wormwood and Quilonum Retard are mixed, blending ratio be Quilonum Retard account for the mixed carbonate total mass 26～52%, salt of wormwood accounts for 48～74% of mixed carbonate total mass; It is the electrolyzer of magnesium that mixed carbonate is placed the negative electrode material, and the electrolyzer that mixed carbonate is housed is heated to 510～600 ℃, begins electrolysis then, and current density is 0.05～0.3A/cm during electrolysis
2, electrolysis time is 0.4～1.6h; The negative electrode that will be mixed with metallic lithium then takes out, and puts into new negative electrode magnesium plate or magnesium rod, proceeds electrolysis, obtains magnesium lithium alloy; Wherein when the change in concentration of the Quilonum Retard in the mixed carbonate reaches 3wt%, replenish Quilonum Retard in mixed carbonate, magnitude of recruitment is no more than 8wt% by the change in concentration of Quilonum Retard in mixed carbonate.
2, the method for a kind of preparing magnesium-lithium alloy by molten salt electrolysis according to claim 1 is characterized in that salt of wormwood and Quilonum Retard thorough drying before use, requires moisture less than 0.1wt%.。
3, a kind of method of preparing magnesium-lithium alloy by molten salt electrolysis is characterized in that: saltpetre and lithium nitrate are mixed, blending ratio be lithium nitrate account for the mixed nitrate total mass 20～90%, saltpetre accounts for 10～80% of mixed nitrate total mass; Add Quilonum Retard then, add-on accounts for 3～8wt% of whole materials by Quilonum Retard, obtains mixed electrolyte; It is the electrolyzer of magnesium that mixed electrolyte is placed the negative electrode material, and the electrolyzer that mixed electrolyte is housed is heated to 150～400 ℃, and to the two poles of the earth energising beginning electrolysis, current density is 0.05～0.3A/cm during electrolysis then
2, electrolysis time is 0.15～0.5h, the negative electrode that will be mixed with metallic lithium then takes out, and puts into new negative electrode magnesium plate or magnesium rod, proceeds electrolysis, obtains magnesium lithium alloy; Wherein when the concentration of the Quilonum Retard in the mixed electrolyte is 3wt%, replenish Quilonum Retard in mixed electrolyte, magnitude of recruitment is 3～8wt% by the concentration of Quilonum Retard in mixed electrolyte.
4, the method for a kind of preparing magnesium-lithium alloy by molten salt electrolysis according to claim 3 is characterized in that saltpetre and lithium nitrate thorough drying before use, requires moisture less than 0.1wt%.。
5, according to the method for claim 1 or 3 described a kind of preparing magnesium-lithium alloy by molten salt electrolysis, it is characterized in that electrolytic cell assembly is a multicavity tray, the anode material is a graphite, the negative electrode material is magnesium plate or magnesium rod; Electrolytic cell assembly has two graphite anodes and a negative electrode magnesium plate, and negative electrode is placed on two anodic middles.
6, according to the method for claim 1 or 3 described a kind of preparing magnesium-lithium alloy by molten salt electrolysis, it is characterized in that the quality of lithium content in the at first predetermined magnesium lithium alloy and negative electrode magnesium plate, make the magnesium lithium alloy product reach predeterminated level by regulating current density and electrolysis time.
7,, it is characterized in that metallic lithium content is 1～15wt% in the described magnesium lithium alloy according to the method for claim 1 or 3 described a kind of preparing magnesium-lithium alloy by molten salt electrolysis.
8, according to the method for claim 1 or 3 described a kind of preparing magnesium-lithium alloy by molten salt electrolysis, the purity that it is characterized in that negative electrode magnesium plate or magnesium rod is more than the 99.8wt%.
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| CNA2008100134373A CN101376992A (en) | 2008-09-27 | 2008-09-27 | Method for preparing magnesium lithium alloy by fused salt electrolysis process |
| CN2009103073450A CN101698951B (en) | 2008-09-27 | 2009-09-21 | Method for preparing magnesium-lithium alloy by molten salt electrolysis |
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| CNA2008100134373A CN101376992A (en) | 2008-09-27 | 2008-09-27 | Method for preparing magnesium lithium alloy by fused salt electrolysis process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768763B (en) * | 2010-01-26 | 2011-10-26 | 东北大学 | Method for preparing magnesium-nickel alloy by molten salt electrolysis and device therefor |
| CN102677098A (en) * | 2012-05-09 | 2012-09-19 | 包头瑞鑫稀土金属材料股份有限公司 | Method for preparing rich cerium misch metal |
| CN109837561A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of metallic lithium powder and its electrochemical preparation method |
| CN110129834A (en) * | 2019-06-26 | 2019-08-16 | 东北大学 | A kind of preparation method of high Li content lithium alloy |
| CN112048737A (en) * | 2020-08-28 | 2020-12-08 | 奉新赣锋锂业有限公司 | Method for improving lithium metal electrolysis current efficiency by controlling water content |
-
2008
- 2008-09-27 CN CNA2008100134373A patent/CN101376992A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768763B (en) * | 2010-01-26 | 2011-10-26 | 东北大学 | Method for preparing magnesium-nickel alloy by molten salt electrolysis and device therefor |
| CN102677098A (en) * | 2012-05-09 | 2012-09-19 | 包头瑞鑫稀土金属材料股份有限公司 | Method for preparing rich cerium misch metal |
| CN109837561A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of metallic lithium powder and its electrochemical preparation method |
| CN110129834A (en) * | 2019-06-26 | 2019-08-16 | 东北大学 | A kind of preparation method of high Li content lithium alloy |
| CN110129834B (en) * | 2019-06-26 | 2020-12-22 | 东北大学 | Preparation method of high-Li-content lithium alloy |
| CN112048737A (en) * | 2020-08-28 | 2020-12-08 | 奉新赣锋锂业有限公司 | Method for improving lithium metal electrolysis current efficiency by controlling water content |
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