CN106756105A - The drop of nitride removes method in lithium metal or lithium alloy - Google Patents
The drop of nitride removes method in lithium metal or lithium alloy Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
Drop the present invention relates to nitride in lithium metal or lithium alloy removes method, belongs to lithium metal technical field.Present invention solves the technical problem that the drop for being to provide nitride in lithium metal or lithium alloy removes method.The method is under vacuum or inert gas shielding atmosphere; lithium metal or lithium alloy are melted and stirred; it is subsequently adding except nitrogen source A is reacted; controlling reaction temperature is 180~1000 DEG C; reaction time is 0.1~10h; settled after the completion of reaction, filtered, filtrate is the lithium metal after denitrogenating or lithium alloy.The present invention is using active metal alloy as except nitrogen source, and practical, low cost, the reaction time is short, easy to operate to be easily achieved.By the lithium metal or the rate of recovery of lithium alloy after the inventive method treatment more than 98%, while active metal alloy less residue, do not influence the purity of lithium metal or lithium alloy after treatment, and the nitrogen content in lithium metal or lithium alloy can be reduced to below 50ppm, far below below the standard value 300ppm in GB.
Description
Technical field
Drop the present invention relates to nitride in lithium metal or lithium alloy removes method, belongs to lithium metal technical field.
Background technology
Lithium is most light metal in nature, is silvery white in color, density 0.534g/cm3, 180.54 DEG C of fusing point, boiling point 1336
℃.Since 1817 Sweden geologist A Fuwei get Song (AArfvedson) find lithium first in lepidolite and lithium feldspar
Since, lithium is obtained in traditional fields such as glass ceramics, petrochemical industry, metallurgy, aluminium metallurgy, weaving, synthetic rubber, lubriation material, medical treatment
Extensive use is arrived.In recent years, the increase with above-mentioned traditional field to lithium demand, and lithium is navigated in nuclear energy power generation, aviation
My god, the development and application research than high-tech sectors such as strong alloys high of high-energy-density electrokinetic cell, lightweight deepen continuously, lithium turns into
Highly important metal in industrial production, is referred to as " energy metal of 21 century ".
Lithium metal, property is active, is a kind of unique gold that can be reacted with nitrogen in air under normal temperature and pressure conditionses
Category, thus, its preservation is very difficult and the shelf-life is generally shorter.In the seventies of 20th century six, U.S. government is extensive
During exploitation nuclear energy, due to a variety of excellent properties of lithium metal, once it was used as the cooling medium of nuclear reactor, but later through engineering reality
Proof is trampled, the nitrogen impurity content in lithium metal liquid can produce serious crystalline substance after exceeding certain limit such as 500ppm to stainless steel
Between corrode, then the problem of denitrogenating of lithium metal is formally proposed.Additionally, lithium metal and its alloy are as secondary battery negative pole material
During material, the exceeded ductility that can reduce lithium metal of nitrogen content so that easy jag, breach during lithium metal pressure zone reduces product and receives
Rate, increases production cost；The electrical property of final battery product can be also influenceed simultaneously.Thus from the point of view of downstream is using angle, Ying Yan
Nitrogen content in lattice control lithium metal product.
But from the point of view of the production method of current lithium metal, the lithium metal in the whole world more than 90% is by fused salt electrolysis process (electricity
Solution lithium chloride and potassium chloride fused salt) prepare, whole electrolytic process is carried out in non-closed container, and lithium metal is from after negative electrode generation
Fused salt surface, inevitable ingress of air are swum in, and is polluted by nitrogen.Thus, all contain in the lithium metal ingot of commerical grade or
Many or few nitrogen impurities, research shows that this impurity is main with Li3N forms are dissolved in lithium metal.For liquid metal lithium liquid,
Nitrogen content increases with the rising of temperature, and its solubility relation is approximately followed：log10(at.%N)=3.2455-2072/T,
Wherein, T<723K, (refers to The Li-N (Lithium-Nitrogen) System, Journal of Phase
Equilibria, Vol.13, No.3,1992).Separately show through dynamics research, the nitrogenization speed of lithium metal is with nitrogen content
Increase and it is quick elevated, typical self-catalysis feature is presented, thus usual to the Control of Nitrogen Content of original metal lithium product
It is very strict, it is desirable to no more than 300ppm.
United States Atomic Energy Agency scientific research personnel E.E.Hoffman once carried out pilot study (THE to the lithium metal method of denitrogenating
SOLUBILITY OF NITROGEN AND OXYGEN IN LITHIUM AND METHODS OF LITHIUM
PURIFICATlON, E.E.Hoffman, ORNL-2894UC-25-Metallurgy and Ceramics), tied as follows
By：Nitrogen content in lithium metal can not be down to desirable level (such as by the methods such as vacuum distillation, filter at low temperature, cold-trap seizure
Below 100ppm), but more than 24h is reacted under 800 DEG C of hot conditions by titanium sponge isoreactivity metal can be by the nitrogen in lithium liquid
Cement out, generate the titanium nitride of stabilization, the nitrogen content in residual metallic lithium liquid can be controlled in below 50ppm.
By the calculating to thermodynamic data, research show, can and Li3The metal that N reacts except titanium, also zirconium,
The metals such as aluminium.But the feasible chemical reaction of thermodynamics, dynamics might not be feasible, thus also needs by testing to reality
Reaction condition makees further research.
United States Patent (USP) US4528032 is proposed use N and Al agent for capturing each other first, by removing N or Al in lithium liquid.If Li liquid
In have Al impurity, by add N formed AlN solids of sedimentation, be then peeled off removal；If there is N impurity in Li liquid, by adding
Al forms AlN solids of sedimentation, is then peeled off removal.The patent is to propose concept, does not have any actual processing information, such as
Temperature, mixed method, process time, processing routine etc..
Then, United States Patent (USP) US4781756 is disclosed and is made silicon source with aluminum shot, and agitation guarantee is carried out to lithium liquid with argon gas bubbles
Reaction is uniform, more than process time 24h, 225~245 DEG C for the treatment of temperature, settlement treatment after 24h, then with 0.5 μm of filter screen mistake
Filter.The patent also states that making lithium source with lithium-aluminium alloy (9wt%Al) can be reduced to 1-4h process time；Use Al content high
Lithium-aluminium alloy (20wt%Li+80wt%Al) makees filter screen can not only remove N but also can be while filtering.The method process time is long,
And denitrogenated just for lithium metal.
United States Patent (USP) US5019158, by adding Al2O3Drop is except the N and Ca in lithium simultaneously.The Al of addition2O3It is first anti-with Li
Li should be generated2O and Al, Al again with Li3N reaction generation AlN precipitations, then remove；And Li2O and Ca reaction generation CaO precipitations, after
And remove.The method is only applicable to N and Ca needs the occasion of removal simultaneously, if being free of Ca in pending lithium metal, uses
The method, it will combustion reaction occurs, it is impossible to remove the N in lithium metal.
Additionally, existing method is to add aluminium isoreactivity metal as except nitrogen source, the remaining active metal aluminium of reaction will
Can remain in cannot be removed in the middle of lithium liquid, cause the residual quantity of aluminium higher.If theoretical amount and actual amount slightly deviation, or analysis
There is larger error in data, then remaining metallic aluminium will influence the quality of lithium metal or alloy.
The content of the invention
For disadvantages described above, the drop that the present invention provides nitride in a kind of lithium metal or lithium alloy removes method, efficiently removal
Nitride in lithium metal or lithium alloy, improves the quality of lithium metal and its alloy.
Present invention solves the technical problem that the drop for being to provide nitride in lithium metal or lithium alloy removes method.
The drop of nitride removes method in lithium metal of the present invention or lithium alloy, comprises the following steps：In vacuum or inert gas
Under protection atmosphere, lithium metal or lithium alloy are melted and stirred, be subsequently adding except nitrogen source A is reacted, controlling reaction temperature is
180~1000 DEG C, the reaction time is 0.1~10h, is settled after the completion of reaction, filtered, and filtrate is the lithium metal after denitrogenating
Or lithium alloy；
Wherein, it is described except nitrogen source A is magnadure, aluminium zircaloy, aluminum titanium alloy or lithium-aluminium alloy；
In molar ratio, except nitrogen source A:N=(1~1.5):1.
Preferably, the vacuum is pressure ＜ 0.1Pa；The inert gas is helium, neon, argon gas or Krypton.
Preferably, heating rate is 100~300 DEG C/h.
Preferably, in molar ratio, except nitrogen source A:N=1:1.
Further, it is preferably described to be shaped as sheet, bulk, foil-like or thread except nitrogen source A, and except the purity of nitrogen source A
More than 99.5%.
Preferably, stirred during reaction, stirring is divided into and rotating and reverse, it is identical with reversing time to rotate forward the time, stirs
Speed is mixed for 100~500rpm.
Preferably, filtration temperature is 200~600 DEG C, and Filter Precision is 3 μm~30 μm.
Stainless steel filter is preferably used during filtering.
Compared with prior art, the present invention has the advantages that：
1) the inventive method, can not only remove the nitride in lithium metal, can also remove the nitride in lithium alloy,
It is widely used.
2) rate of recovery of lithium metal or lithium alloy after the inventive method is processed is more than 98%, and lithium metal or lithium alloy
In nitrogen content can be reduced to below 50ppm, far below below the standard value 300ppm in GB.
3) the inventive method, using active metal alloy as except nitrogen source, both can effectively improve the efficiency of nitrogen retention
And then efficiency is denitrogenated in raising, while active metal alloy less residue, does not influence the purity of lithium metal or lithium alloy after treatment.
4) present invention process is practical, and low cost, the reaction time is short, easy to operate to be easily achieved.
Specific embodiment
The drop of nitride removes method in lithium metal of the present invention or lithium alloy, comprises the following steps：In vacuum or inert gas
Under protection atmosphere, lithium metal or lithium alloy are melted and stirred, be subsequently adding except nitrogen source A is reacted, controlling reaction temperature is
180~1000 DEG C, the reaction time is 0.1~10h, is settled after the completion of reaction, filtered, and filtrate is the lithium metal after denitrogenating
Or lithium alloy；
Wherein, it is described except nitrogen source A is magnadure, aluminium zircaloy, aluminum titanium alloy or lithium-aluminium alloy；
In molar ratio, except nitrogen source A:N=(1~1.5):1.
It has been investigated that, active metal alloy at relatively high temperatures can stoichiometrically coefficient reacts life with lithium nitride
Into nitridation metal, the nitridation metal of generation is crystallized to grow up, and through gravitational settling and filtering with lithium metal liquid or its aluminium alloy
Separate, it is that can obtain the few lithium metal of nitrogen content or its alloy to collect filtrate.Its chemical equation is as follows：
Li3N+A=AN+3Li
Herein, A represents active metal alloy, such as aluminium titanium, aluminium zirconium, magnalium, lithium aluminium.
Lithium alloy of the invention includes but is not limited to lithium-aluminium alloy, Li-Si alloy, lithium magnesium alloy etc..
The inventive method can be exceeded to nitrogen content lithium metal or lithium alloy process, nitrogen therein is removed, for dropping
The nitrogen content of low metal lithium and its alloy, concrete application scope is included but is not limited to：Production preparation, the mistake of lithium metal and its alloy
During phase commerical grade lithium metal and its alloy treatment, lithium metal and its alloy production produce substandard products treatment, lithium metal and its
Exceeded treatment of lithium metal product and lithium system alloy product of the leftover pieces of return, other nitrogen contents etc. after the pressure zone of alloy downstream.
Processed under vacuum or inert atmosphere, primarily to preventing the hair such as moisture, oxygen, nitrogen in lithium and air
Raw reaction, it is preferred that the vacuum is pressure ＜ 0.1Pa；The inert gas is helium, neon, argon gas or Krypton.
Heating rate to reaction tool have a certain impact, heating rate is too fast, each position of lithium liquid will skewness so that
Influence the drop of nitride to remove, heating rate is excessively slow, influence reaction efficiency, accordingly, it is preferred that heating rate is 100~300 DEG C/h.
It is stirred after lithium metal or lithium alloy fusing, primarily to ensureing that the nitrogen content distribution at each position of lithium liquid is equal
It is even.In order to accurately determine the addition except nitrogen source A, can be after stirring, by GB analysis method sampling analysis lithium liquid
Nitrogen content.
Preferably, in molar ratio, except nitrogen source A:N=1:1.
Except nitrogen source A influence of the shape to the inventive method less, except the shape of nitrogen source A can be piece, block, paper tinsel, silk etc.
The source metal of various structure types, need to only ensure that purity is more than 99.5%.
Stirring during reaction is one of key factor of influence reaction, and the present invention preferably mechanical agitation, stirring is divided into rotating forward
And reversion, rotate forward the time it is identical with reversing time, respectively account for the half of total reaction time, stir speed (S.S.) is 100~500rpm, this
Sample can make nitride distribution in lithium metal or its alloy more uniform and add after active metal alloy with the reaction of nitrogen more
Plus it is uniform, ensure that reaction is more efficient, evenly, process time is shorter.It is of the present invention just to switch to initially be stirred during reaction
The direction mixed, it can also be clockwise counterclockwise that can be.If just switching to clockwise, be reversed to counterclockwise, vice versa.
After the completion of reaction, reacted lithium liquid or lithium alloy are also carried out settling and filtered, filtering can remove nitridation metal
(AN) filtrate, lithium metal or lithium alloy after as denitrogenating, are collected.Preferred filtration temperature is 200~600 DEG C, filter essence
Spend is 3 μm~30 μm.
Stainless steel filter is preferably used during filtering, it is longer compared to the lithium alloy filter more cheap and life-span, also not
Filter efficiency can be influenceed.
Can be post-processed using conventional method for filtrate, for example, filtrate can be cast, cool down, sampling, taking out true
Empty, packaging, obtains salable finished product.
Specific embodiment of the invention is further described with reference to embodiment, is not therefore limited the present invention
System is among described scope of embodiments.
The exceeded lithium metal of the nitrogen content of embodiment 1 is denitrogenated
The exceeded Battery grade lithium metal 1.51kg of nitrogen content is placed in a sealed reactor, stabilization is vacuumized to reactor
To ＜ 0.1Pa, heating material is carried out, the rate of heat addition is 200 DEG C/h, stop heating and starting to stir after lithium metal is completely melt
Mix, it is ensured that the nitrogen content at each position of lithium liquid be evenly distributed after by nitrogen content in GB analysis method sampling analysis product, measure and contain
Nitrogen quantity is 982ppm.It is in molar ratio Mg-Al:N=1:1 ratio weighs accurate magnalium and closes to addition in the lithium liquid of fusing
Gold.Again reactor is heated, heating rate is controlled in 100 DEG C/h, and by reaction temperature control at 300 DEG C, stir speed (S.S.) is
300rpm, reaction time 0.1h, rotate and reverse and respectively account for half, settled after the completion of reaction, natural cooling cooling, to metal
Lithium liquid or aluminium alloy are separated by filtration, and filtrate is cast, cool down, sample, vacuumize, packed.Finally reclaim lithium metal 1.49
Kilogram, the rate of recovery is 98.7%.
Analyze data is shown in Table 1, and analysis result shows to be reduced to 46ppm through nitrogen content in the lithium metal after treatment, is far below
The 300ppm of Battery grade lithium metal professional standard, and need the magnadure for adding only to remain 3ppm because denitrogenating, to downstream industry
Substantially without influence.
Table 1
Embodiment 2 processes lithium metal in the case of changing except nitrogen source
Experimental technique as described in Example 1, in experiment except nitrogen source is changed the result obtained under different condition,
These factors are respectively and use metallic aluminium titanium, aluminium zircaloy or magnadure (shape is Alloy Foil).Test arrangement is shown in Table 2,
Nitrogen is shown in Table 3 with the residual quantity and the rate of recovery of lithium metal except nitrogen source in lithium metal after denitrogenating.
Table 2
Table 3
| Test number | The content (ppm) of A | The content (ppm) of N | The rate of recovery (%) of Li |
| 2-1 | (Al-Zr)4 | 41 | 98 |
| 2-2 | (Al-Ti)4 | 38 | 99 |
| 2-3 | (Mg-Al)5 | 44 | 99 |
| 2-4 | (Al-Zr)6 | 41 | 98 |
| 2-5 | (Li-Al)3 | 40 | 99 |
The exceeded lithium-aluminium alloy of the nitrogen content of embodiment 3 is denitrogenated
The exceeded lithium-aluminium alloy of the nitrogen content because of packages in damaged condition (standard aluminium content is 3000ppm) 1.78kg is placed in one close
In envelope reactor, nitrogen being passed through in a kettle., under nitrogen protection, carrying out heating material, the rate of heat addition is 200 DEG C/h, when
Alloy stops heating and starting stirring after being completely melt, it is ensured that the nitrogen content at each position of lithium liquid is divided after being evenly distributed by professional standard
Nitrogen content, aluminium content in analysis method sampling analysis product, measure nitrogen content for 467ppm, and aluminium content is 2915ppm.In molar ratio
It is Al-Zr:N=1:1 ratio weighs accurate aluminium zircaloy grain 1.603g to addition in the lithium liquid of fusing.Again to reactor
Heating, heating rate is controlled in 200 DEG C/h, and by reaction temperature control at 600 DEG C, stir speed (S.S.) is 300rpm, reaction time
10h, rotates and reverse and respectively accounts for half, settled after the completion of reaction, natural cooling cooling, aluminium alloy is separated by filtration,
Filtrate is cast, cool down, sample, vacuumize, packed.The lithium-aluminium alloy for finally reclaiming can reach LITHIUM BATTERY standard, yield
It it is 1.7 kilograms, yield reaches 95%.
Analyze data is shown in Table 4.Result of the test shows to be reduced to by the lithium-aluminium alloy product nitrogen content after the treatment of this method
40ppm, and the change of its aluminium content is little.
Table 4
Comparative example 1 reclaims lithium metal using metallic aluminium as except nitrogen source
Experimental technique as described in Example 1, only to, except nitrogen source is changed, magnadure being replaced by into metallic aluminium in experiment
As except nitrogen source.The lithium metal for finally reclaiming is 1.47 kilograms, and the rate of recovery is 98.7%.
The composition discovery of analysis lithium metal, 40ppm is down to through nitrogen content in the lithium metal after treatment, and need to add because denitrogenating
The aluminium residue 20ppm for entering.According to metallic aluminium as except nitrogen source, the remaining metallic aluminium of reaction will be remained in cannot in the middle of lithium liquid
Removal, causes the residual quantity of aluminium higher.
Further, if larger error occur in theoretical amount and actual amount slightly deviation, or analyze data, then remaining gold
Category aluminium will influence the quality of lithium metal or alloy.
Comparative example 2 reclaims lithium alloy using metallic aluminium as except nitrogen source
Experimental technique as described in Example 3, only to, except nitrogen source is changed, aluminium zircaloy being replaced by into metallic aluminium in experiment
As except nitrogen source.The lithium-aluminium alloy for finally reclaiming is 1.67 kilograms, and the rate of recovery is 94%.
The composition discovery of analysis lithium-aluminium alloy, 45ppm is down to through nitrogen content in the lithium-aluminium alloy after treatment, and need because denitrogenating
The aluminium to be added residue 100ppm.According to metallic aluminium as except nitrogen source, the remaining metallic aluminium of reaction will remain in lithium liquid and work as
In cannot remove, cause the residual quantity of aluminium higher.
If larger error occur in theoretical amount and actual amount slightly deviation, or analyze data, then remaining metallic aluminium will
The quality of influence lithium metal or alloy.
To sum up, the present invention can be more easy to the residual volume that effective control adds metal using alloy as except nitrogen source.
Claims (8)
1. the drop of nitride removes method in lithium metal or lithium alloy, it is characterised in that：Comprise the following steps：
Under vacuum or inert gas shielding atmosphere, lithium metal or lithium alloy are melted and stirred, be subsequently adding except nitrogen source A is carried out
Reaction, controlling reaction temperature is 180~1000 DEG C, and the reaction time is 0.1~10h, is settled after the completion of reaction, filtered, and is filtered
Liquid is the lithium metal after denitrogenating or lithium alloy；
Wherein, it is described except nitrogen source A is magnadure, aluminium zircaloy, aluminum titanium alloy or lithium-aluminium alloy；
In molar ratio, except nitrogen source A:N=(1~1.5):1.
2. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：The vacuum
It is pressure ＜ 0.1Pa；The inert gas is helium, neon, argon gas or Krypton.
3. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：Heating rate
It is 100~300 DEG C/h.
4. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：By mole
Than except nitrogen source A:N=1:1.
5. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：It is described to denitrogenate
Source A's is shaped as sheet, bulk, foil-like or thread, and purity is more than 99.5%.
6. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：Stirred during reaction
Mix, stirring is divided into and rotating and reverse, rotate forward that the time is identical with reversing time, stir speed (S.S.) is 100~500rpm.
7. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：Filtration temperature
It it is 200~600 DEG C, Filter Precision is 3 μm~30 μm.
8. the drop of nitride removes method in lithium metal according to claim 1 or lithium alloy, it is characterised in that：The filtering
Using stainless steel filter.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528032A (en) * | 1984-01-10 | 1985-07-09 | The United States Of America As Represented By The United States Department Of Energy | Lithium purification technique |
| US4781756A (en) * | 1987-07-02 | 1988-11-01 | Lithium Corporation Of America | Removal of lithium nitride from lithium metal |
| US5019158A (en) * | 1989-06-09 | 1991-05-28 | Metaux Speciaux S.A. | Process for the separation of calcium and nitrogen from lithium |
| CN102409174A (en) * | 2010-09-23 | 2012-04-11 | 株式会社半导体能源研究所 | Method for recovering metallic lithium |
| CN103379972A (en) * | 2010-09-28 | 2013-10-30 | 罗克伍德锂有限责任公司 | Stabilized, pure lithium metal powder and method for producing the same |
-
2016
- 2016-12-19 CN CN201611177870.1A patent/CN106756105B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528032A (en) * | 1984-01-10 | 1985-07-09 | The United States Of America As Represented By The United States Department Of Energy | Lithium purification technique |
| US4781756A (en) * | 1987-07-02 | 1988-11-01 | Lithium Corporation Of America | Removal of lithium nitride from lithium metal |
| US5019158A (en) * | 1989-06-09 | 1991-05-28 | Metaux Speciaux S.A. | Process for the separation of calcium and nitrogen from lithium |
| CN102409174A (en) * | 2010-09-23 | 2012-04-11 | 株式会社半导体能源研究所 | Method for recovering metallic lithium |
| CN103379972A (en) * | 2010-09-28 | 2013-10-30 | 罗克伍德锂有限责任公司 | Stabilized, pure lithium metal powder and method for producing the same |
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