CN106756067A - A kind of method for reclaiming lithium metal and the technique for preparing lithium metal - Google Patents
A kind of method for reclaiming lithium metal and the technique for preparing lithium metal Download PDFInfo
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- CN106756067A CN106756067A CN201611162031.2A CN201611162031A CN106756067A CN 106756067 A CN106756067 A CN 106756067A CN 201611162031 A CN201611162031 A CN 201611162031A CN 106756067 A CN106756067 A CN 106756067A
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- lithium metal
- lithium
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- molten liquid
- liquid
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Links
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 157
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 81
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical class [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 49
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 48
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 48
- 238000002844 melting Methods 0.000 claims abstract description 39
- 230000008018 melting Effects 0.000 claims abstract description 39
- 239000012535 impurity Substances 0.000 claims abstract description 28
- 239000002893 slag Substances 0.000 claims abstract description 26
- 239000001103 potassium chloride Substances 0.000 claims abstract description 24
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 24
- 239000000654 additive Substances 0.000 claims abstract description 16
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 38
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 17
- 230000000996 additive effect Effects 0.000 claims description 15
- 239000000155 melt Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 235000010333 potassium nitrate Nutrition 0.000 claims description 8
- 239000004323 potassium nitrate Substances 0.000 claims description 8
- 238000012546 transfer Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000000746 purification Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- -1 lithium metals Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 241000722270 Regulus Species 0.000 description 1
- NMLQNVRHVSWEGS-UHFFFAOYSA-N [Cl].[K] Chemical compound [Cl].[K] NMLQNVRHVSWEGS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- 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
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to chemical purification field, and in particular to a kind of method of recovery lithium metal and the technique for preparing lithium metal.The method for reclaiming lithium metal, comprises the following steps：By 50 60 parts of lithium chlorides and the mixed melting of 40 50 parts of potassium chloride, the first mixed molten liquid is obtained.Melting is heated after adding lithium slag in the first mixed molten liquid, the second mixed molten liquid is obtained.Melted after to adding 8 10 parts of additives after the second mixed molten liquid removal of impurities, when supernatant liquid is changed into silvery white, lithium metal is reclaimed from supernatant liquid.It is the method short flow, simple to operate, the production time is saved, the lithium metal purity that can directly and quickly obtain lithium metal and obtain is high, quality better.
Description
Technical field
The present invention relates to chemical purification field, and in particular to using it is a kind of reclaim lithium metal method and prepare lithium metal
Technique.
Background technology
Lithium slag be in lithium metal manufacturing process produce contain a large amount of lithium metals and a small amount of potassium, sodium and its oxide, carbon
The residue of compound etc..According to production leadtime, 1t lithium metal output lithium slags about 40kg is often produced.Lithium metal is as a kind of noble metal and newly
Energy metal, with economic worth very high.Therefore, the recycling of lithium slag is particularly important.Because lithium metal property is non-
It is often active, cause from the view of safety, regulus storage and removal process it occur frequently that catching fire, burn play even occurs
Strong blast, not only results in the waste in metal, but also can cause major safety risks to related facility, personnel, environment.
At present, successfully report is little for the recycling of lithium slag, all or burns or gives up and throw away mostly, rare, is to pass through
Complicated operation converts it into lithium-containing solution.But such processing mode flow is cumbersome, inferior quality, with high costs.
The content of the invention
It is an object of the invention to provide a kind of method for reclaiming lithium metal, the method need not prepare lithium-containing solution and flow
Short, the easily operated, rate of recovery is high.
Another object of the present invention is to provide a kind of technique for preparing lithium metal, purity can be obtained using the technique
The high, lithium metal of quality better, the technological operation is simple, reaction condition is gentle.
The present invention is solved its technical problem and is realized using following technical scheme：
A kind of method for reclaiming lithium metal, comprises the following steps：By weight, 50-60 parts of lithium chloride and 40- will be contained
50 parts of mixtures of potassium chloride carry out heating melting for the first time, obtain the first mixed molten liquid.Lithium is added in the first mixed molten liquid
Second heating melting is carried out after slag, the second mixed molten liquid is obtained.8-10 parts of additive will be added after second mixed molten liquid removal of impurities
After carry out third time heating melting, when supernatant liquid is changed into silvery white, lithium metal is reclaimed from above-mentioned supernatant liquid.
It is by the centre of above-mentioned second mixed molten liquid by above-mentioned second mixed molten liquid removal of impurities in present pre-ferred embodiments
Layer liquid is shifted.
In present pre-ferred embodiments, above-mentioned second mixed molten liquid is put into intermediate layer liquid by with mesh-structured
Stainless steel spoon is shifted.
In present pre-ferred embodiments, above-mentioned additive includes at least one in potassium nitrate, lithium nitrate.
In present pre-ferred embodiments, in parts by weight, the above-mentioned lithium slag of addition is 3-7 parts.
In present pre-ferred embodiments, the melt temperature of above-mentioned first time heating melting and second heating melting is
420℃-450℃。
In present pre-ferred embodiments, the melt temperature of above-mentioned third time heating melting is 330 DEG C -380 DEG C.
In present pre-ferred embodiments, lithium metal is reclaimed from above-mentioned supernatant liquid includes the above-mentioned supernatant liquid of transfer simultaneously
Carry out pouring shaping.
In present pre-ferred embodiments, the above-mentioned above-mentioned supernatant liquid of transfer enters by with mesh-structured stainless steel spoon
Row transfer.
A kind of technique for preparing lithium metal, including the method for above-mentioned recovery lithium metal prepares impurity content seldom,
Quality better, purity lithium metal high.
The present invention reclaim lithium metal embodiment of the method beneficial effect be：Lithium chloride is mixed and melted with potassium chloride can drop
Low lithium slag melts out the fusing point of lithium metal, so as to reduce reaction temperature, reduces the demand to high-temperature service, and then attenuating is produced into
This.By the mixed molten liquid of lithium slag, lithium chloride, potassium chloride, to carry out removal of impurities be to ensure the purity of molten place's lithium, it is to avoid molten surface
Impurity combined with the lithium metal for melting out, reduce lithium metal purity.Addition additive is in order to further reduction melts out lithium
Fusing point, reduce energy consumption, reduce production cost.The method short flow, simple to operate, can directly and quickly obtain gold simultaneously
Category lithium.The lithium metal purity that obtains is high, quality better.
The preparation technology of lithium metal of the present invention as the method that tradition prepares lithium without being first prepared containing the molten of lithium
The operation of liquid and generation lithium salts, and molten lithium slag can be directly heated and obtain that purity is high, quality better lithium metal.Use simultaneously
The method prepares lithium metal and lithium slag can be recycled, and the utilization rate of lithium, reduces the wasting of resources in lifting lithium slag.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
The accompanying drawing for needing to use is briefly described.
Fig. 1 is the method flow diagram for reclaiming lithium metal.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional product that can be obtained by commercially available purchase
Product.
The recovery method of lithium metal and the preparation method of lithium metal to the embodiment of the present invention are specifically described below.
A kind of method for reclaiming lithium metal：
S1, will be carried out in heating furnace containing 50-60 parts of lithium chloride and the 40-50 parts of mixture of potassium chloride by weight
First heating melting, obtains the first mixed molten liquid.
Wherein, lithium chloride is the crystal of white, with hygroscopy.Taste is salty.Soluble in water, ethanol, acetone, pyridine etc. are organic
Solvent.Lower toxicity.Lithium chloride is mainly used in filed of air conditioning, as scaling powder, drier, chemical reagent, and for flame processed
Fire, dry cell and lithium metal etc..Its fusing point is 605 DEG C.
Potassium chloride is a kind of colourless elongated rhombus or into a cubic crystal, or white crystals small particle powder, outward appearance as
Salt, odorless, taste are salty.Soluble in water, ether, glycerine and bases, are slightly soluble in ethanol, but insoluble in absolute ethyl alcohol, have hygroscopicity, easily
Caking.Fusing point is 776 DEG C.Can be seethed with excitement when being heated to 1420 DEG C.
It is to reduce the fusing point of the two melting that lithium chloride carries out mixed melting with potassium chloride.And the lithium chloride for using for
50-60 parts, potassium chloride is 40-50 parts, because fusing point of the fusing point of lithium chloride less than potassium chloride.Use more lithium chloride energy
It is enough that the fusing point of mixture is reduced to smaller scope, and then cause that reaction temperature tends to gentle, it is not necessary to too high temperature.Root
The ratio mixed according to lithium chloride and potassium chloride deduces the fusing point of the two mixture, and then determines melt temperature.And preferably, the
The melt temperature of one heating melting is 420 DEG C -450 DEG C.The mixture of lithium chloride and potassium chloride can be melted using the temperature
Completely, it is not necessary to use temperature higher, and then do not result in the waste of energy, resource.
S2, add lithium slag in the first mixed molten liquid after carry out second heating melting, obtain the second mixed molten liquid.
Using the lithium slag containing lithium metal for subsequently melting out lithium metal provides raw material.After lithium slag being added in first mixed molten liquid
Continue to heat, lithium slag slowly melts, and has lithium metal to melt out.And most white oil is mineral oil in the second mixed molten liquid
Volatilized with high temperature, only remaining a small amount of white oil floats on the second mixed molten liquid surface, while the less stone of non-volatile and density
Ink powder also floats on the second mixed molten liquid surface.Have compared with the lithium chloride, potassium chloride of molten condition due to having melted out lithium metal
There is smaller density, the lithium metal for melting out is positioned at lithium chloride and the upper strata of potassium chloride mixed molten liquid, and lithium chloride and potassium chloride
Mixed molten liquid then positioned at the second mixed molten liquid bottom.
S3, will after the second mixed molten liquid removal of impurities add 8-10 part additive after carry out third time heating melt, treat upper liquid
When body is changed into silvery white, lithium metal is reclaimed from above-mentioned supernatant liquid.
Second mixed molten liquid is carried out into removal of impurities because add lithium slag be contained within insoluble material, these materials some
Evaporated, some remain unchanged and float on the surface of the second mixed molten liquid, if not by these Impurity removals, it will influence melts out the product of lithium
Matter and purity.The removal of impurities mode that this step is used is that the lithium metal liquid in the second mixed molten liquid intermediate layer is scooped from heating furnace
Go out.Scooping out lithium metal liquid can remove the impurity on surface while will not scoop out the impurity of heating furnace bottom deposit, be easy to follow-up
Lithium metal is melted out, it is ensured that the purity of lithium metal.
Preferably, using being the lithium metal that melts out to the intermediate layer of the second mixed molten liquid with mesh-structured stainless steel spoon
Shifted.To carry out slight rocking and shaking spoon week on the second mixed molten liquid surface with mesh-structured spoon
Enclose and float on the impurity on the second mixed molten liquid surface and arrange so that the subsurface liquid of the second mixed molten liquid can smoothly enter spoon
It is sub internal.Simultaneously as the density of lithium metal is small, its upper strata for floating on transfer liquid, and proportion is the larger lithium chloride of density
Mixed molten liquid with potassium chloride is then outflowed back in heating furnace by the mesh inside spoon.And the fusing point of lithium metal is relatively low,
It passes through heat exchange during spoon mesh, and moment forms liquid film, prevents lithium metal from being flowed out from spoon inside, in lithium metal liquid quilt
Pour into when in salt bath, the liquid film is transferred with lithium metal.Spoon is made of stainless steel because stainless steel have it is resistance to
Burn into fusing point is higher, be readily cleaned, the advantages of surface is smooth.Its surface is smooth to enable to lithium metal smooth, quick from spoon
Mark sub- inside.Its corrosion-resistant, fusing point high temperature that liquid can will not be transferred during lithium metal is shifted high is melted
Or melt out impurity.
Addition additive is to further reduce out the fusing point of lithium.Due to existing lithium metal in now the 3rd mixed molten liquid
The presence of liquid, it is necessary to the temperature for reducing is without excessive, therefore, the additive of addition is 8-10 parts.8-10 parts of additive not shadow
Ring purity, the quality of lithium, meanwhile, the use of raw material is reduced, reduce cost.
Preferably, additive is at least one in potassium nitrate, lithium nitrate.Addition potassium nitrate, lithium nitrate or the two
Mixture can further reduce out lithium fusing point, and then cause that reaction condition is gentleer.Wherein, potassium nitrate is, without chlorine potassium, to be
Water white transparency prism-shaped or white particle or crystalline powder.Taste is pungent is peppery and salty cool feeling.Micro- deliquescence, hygroscopy is more micro- than sodium nitrate
It is small.Its fusing point is 334 DEG C.Lithium nitrate physical property be colourless crystallization, easy moisture absorption, be heated to 600 DEG C decompose, be dissolved in about 2 parts of water,
Ethanol, the aqueous solution are dissolved in neutral, about 255 DEG C of relative density 2.38, fusing point.It has strong oxidizing property, irritant, with organic matter
Friction or impact energy cause burning or explode.Can be used for the manufacture of analytical reagent, heat exchange carrier, fluorophor and its lithium salts, ceramics
Industry.
The melt temperature of third time heating melting compares the temperature reduction of heating melting for the first time and second heating melting,
Determine the melt temperature that third time heating is melted according to additivated component is added.Preferably, the melting of third time heating melting
Temperature is 330 DEG C -380 DEG C.During using the melt temperature, the additive of addition can be melted all just, without using higher
Temperature, cause unnecessary energy dissipation.
The density of lithium metal liquation is compared with the density of additive liquation, and its density is lower, therefore lithium metal liquation floats on
The upper strata of mixed molten liquid.Lithium metal is silvery white, therefore, naked-eye observation is changed into limpid silvery white to mixed molten liquid supernatant liquid
When, show there is pure metal lithium to generate.So, it is preferable that using has mesh-structured stainless steel spoon by upper strata silvery white
Lithium liquid be scooped into mould, cooling causes that the solidification of lithium metal liquation obtains pure lithium metal, and the yield of lithium metal is 85%-
90%, the content of the impurity of lithium metal meets standard GB/T 4369-84-Li-01.
Preferably, above-mentioned operation is carried out in atmospheric conditions.Metal lithium chemistry is active, under atmospheric pressure state,
As far as possible lithium metal can be avoided from being chemically reacted with the oxygen in air, in turn result in unnecessary danger.
A kind of preparation technology of lithium metal：The operating procedure of the method including above-mentioned recovery lithium metal.By aforesaid operations
Step can obtain high-quality, individual impurities content and reach the lithium metal of high-purity rank, high income.
The method of the recovery lithium metal that the present invention is provided, by adding lithium chloride and potassium chloride reduction lithium slag in go out the molten of lithium
Point, so as to reduce reaction temperature so that reaction condition tends to gentle.Shifting the second mixed molten liquid is mixed to largely remove second
Close the impurity of molten surface attachment.Addition additive can further reduce out lithium fusing point, reduce energy consumption, reduce production cost.
It is whole method flow short flow, simple to operate, it is easy to industrialized production, can directly and quickly obtain lithium metal.Meanwhile, it is right
Recycled in lithium slag, reduced the waste of resource.
Feature of the invention and performance are described in further detail with reference to embodiments.
Embodiment 1
Shown in reference picture 1, under condition of normal pressure, by 5.6Kg lithium chlorides and the stirring mixing of 4.4Kg potassium chloride in heating furnace,
And the first heating melting is carried out under the conditions of 440 DEG C so that all melting obtains first for 5.6Kg lithium chlorides and 4.4Kg potassium chloride
Mixed molten liquid.5Kg lithium slags are added in heating furnace, 440 DEG C of temperature is kept, second heating are carried out and is melted so that lithium slag is complete
Full-fusing obtains the second mixed molten liquid.
Now, the second mixed molten liquid surface flotation is in graphite powder and a small amount of white oil, and the potassium chloride of molten condition and
Lithium chloride is sunken to heating furnace bottom i.e. positioned at the lower floor of the second mixed molten liquid, and the lithium metal for melting out then is situated between on heating furnace upper strata
Between the surface of the second mixed molten liquid and lower floor.This part liquation color is canescence or faint yellow.
The impurity on the second mixed molten liquid surface is skimmed using with mesh-structured stainless steel spoon, by the metal in intermediate layer
Lithium liquid is scooped into salt bath.Due to the larger i.e. potassium chloride of the proportion of the first mixed molten liquid.The density of lithium chloride is more than lithium metal, two
Person is outflowed back in heating furnace by the mesh of stainless steel spoon, and lithium metal is then transferred in salt bath, obtains removal big absolutely
The liquation of partial impurities.
0.9Kg lithium nitrates are added in liquation, third time heating melting are carried out under conditions of being 350 DEG C in temperature so that
Lithium nitrate is melted, and is always maintained at the state of heating melting.Supernatant liquor is inner silver in by naked-eye observation to salt bath
During white fused solution, enter in mould using with mesh-structured stainless steel spoon transfer upper strata silvery white liquation, cooling so that
Silvery white liquation condenses into white solid, and finally, the white solid for obtaining is lithium metal, and the yield of lithium metal is 88%.
The purity of lithium metal and the type of its impurity and content that obtain are detected by ICP-AES, testing result is shown in
Table 1.
The lithium metal purity detecting result of table 1
The compound national standard of lithium metal for obtaining, the content of lithium metal is more than 99%.With standard GB/T 4369-84-Li-
01 compared to impurity natrium tenor well below standard value, impurity calcium, silicon, iron, the content of nickel are close to standard GB/T 4369-
84-Li-04's is required to meet the other requirement of lithium metal high-purity-grade.
Embodiment 2
It is that the lithium chloride for using is 6.0Kg that embodiment 2 is distinguished compared with Example 1, and potassium chloride is 4.0Kg, lithium slag
3Kg, additive is 1Kg potassium nitrate, and heating for the first time is melted and the temperature of the second heating melting is 420 DEG C, and third time adds
The temperature of heat fusing is 330 DEG C, and remaining mode of operation and operating condition do not change.The receipts of the lithium metal for finally giving
Rate is 90%.
Defects inspecting is carried out to the lithium metal that embodiment 2 is obtained, what is obtained the results are shown in Table 2.
The lithium metal purity detecting result of table 2
The compound national standard of lithium metal for obtaining, the content of lithium metal is more than 99%.And with standard GB/T 4369-
84-Li-01 is compared to impurity natrium tenor well below standard value.And the content and national standard of impurity calcium, silicon, iron, nickel
The requirement of GB4369-84-Li-04 is consistent, meets the other requirement of lithium metal high-purity-grade.
Embodiment 3
Embodiment 3 is compared with Example 1 that the lithium chloride for using is 5.0Kg compared to difference, and potassium chloride is 6.0Kg, lithium
Slag 7Kg, additive is the mixture of 0.8Kg potassium nitrate and lithium nitrate, the temperature of heating melting for the first time and the second heating melting
450 DEG C are, and the temperature that third time heats melting is 380 DEG C, remaining mode of operation and operating condition do not change.
The yield of the lithium metal for finally giving is 85%.
Defects inspecting is carried out to the lithium metal that embodiment 3 is obtained, what is obtained the results are shown in Table 3.
The lithium metal purity detecting result of table 3
The compound national standard of lithium metal for obtaining, the content of lithium metal is more than 99%.And with standard GB/T 4369-
84-Li-01 is compared to impurity natrium tenor well below standard value.
In sum, the method for the recovery lithium metal of the embodiment of the present invention and the method for lithium metal is prepared to each condition
Research show, directly by heat melting cause lithium metal melted out from lithium slag, it is not necessary to prepare lithium solution or lithium salts be molten
Liquid, shortens preparation process, and it is simpler easy to operate.Lithium fusing point is reduced out by adding lithium chloride, potassium chloride, reaction is reduced
Temperature so that reaction condition tends to gentle, reduces the requirement to production equipment.Addition lithium nitrate, potassium nitrate or the two
Mixture, further reduces the fusing point for melting out lithium, reduces reaction temperature, so as to reduce energy consumption, reduces production cost.And pass through
The method prepares the low lithium metal of the purity that can efficiently obtain high, quality better, impurity content.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. it is a kind of reclaim lithium metal method, it is characterised in that comprise the following steps：
By weight, heating melting for the first time will be carried out containing 50-60 parts of lithium chloride and the 40-50 parts of mixture of potassium chloride,
Obtain the first mixed molten liquid；
Second heating melting is carried out after adding lithium slag in first mixed molten liquid, the second mixed molten liquid is obtained；
8-10 parts of additive will be added after the second mixed molten liquid removal of impurities carries out third time heating melting, treats that supernatant liquid is changed into
During silvery white, lithium metal is reclaimed from the supernatant liquid.
2. it is according to claim 1 reclaim lithium metal method, it is characterised in that be by the second mixed molten liquid removal of impurities
The intermediate layer liquid of second mixed molten liquid is shifted.
3. it is according to claim 2 reclaim lithium metal method, it is characterised in that second mixed molten liquid it is described in
Interbed liquid is shifted by with mesh-structured stainless steel spoon.
4. it is according to claim 1 reclaim lithium metal method, it is characterised in that the additive include potassium nitrate, nitre
At least one in sour lithium.
5. it is according to claim 1 reclaim lithium metal method, it is characterised in that in parts by weight, the lithium of addition
Slag is 3-7 parts.
6. the method for reclaiming lithium metal according to claim 1, it is characterised in that first time heating melting and described
The melt temperature of second heating melting is 420 DEG C -450 DEG C.
7. the method for reclaiming lithium metal according to claim 6, it is characterised in that the melting of third time heating melting
Temperature is 330 DEG C -380 DEG C.
8. it is according to claim 1 reclaim lithium metal method, it is characterised in that from the supernatant liquid reclaim lithium metal
Including shifting the supernatant liquid and carrying out cast molding.
9. the method for reclaiming lithium metal according to claim 8, it is characterised in that the transfer supernatant liquid is by having
Mesh-structured stainless steel spoon is shifted.
10. a kind of technique for preparing lithium metal, it is characterised in that including the recovery as described in any one in claim 1-9
The method of lithium metal.
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| CN109264750A (en) * | 2018-10-22 | 2019-01-25 | 天齐锂业（江苏）有限公司 | A kind of method for innocent treatment of lithium metal waste residue |
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| US4758316A (en) * | 1987-04-20 | 1988-07-19 | Aluminum Company Of America | Aluminum-lithium scrap recovery |
| US4822412A (en) * | 1986-11-17 | 1989-04-18 | The Boeing Company | Method of removing lithium from aluminum-lithium alloys |
| CN103205774A (en) * | 2013-05-02 | 2013-07-17 | 新疆骏强科技发展有限公司 | Method of preparing metallic lithium by one-step fusion electrolysis of lithium salt |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4822412A (en) * | 1986-11-17 | 1989-04-18 | The Boeing Company | Method of removing lithium from aluminum-lithium alloys |
| US4758316A (en) * | 1987-04-20 | 1988-07-19 | Aluminum Company Of America | Aluminum-lithium scrap recovery |
| CN103205774A (en) * | 2013-05-02 | 2013-07-17 | 新疆骏强科技发展有限公司 | Method of preparing metallic lithium by one-step fusion electrolysis of lithium salt |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264750A (en) * | 2018-10-22 | 2019-01-25 | 天齐锂业（江苏）有限公司 | A kind of method for innocent treatment of lithium metal waste residue |
| CN109264750B (en) * | 2018-10-22 | 2020-12-29 | 天齐锂业（江苏）有限公司 | Harmless treatment method for metal lithium waste residue |
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