CN103409648B - Low-temperature metal lithium distillation equipment and distillation method thereof - Google Patents
Low-temperature metal lithium distillation equipment and distillation method thereof Download PDFInfo
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- CN103409648B CN103409648B CN201310348064.6A CN201310348064A CN103409648B CN 103409648 B CN103409648 B CN 103409648B CN 201310348064 A CN201310348064 A CN 201310348064A CN 103409648 B CN103409648 B CN 103409648B
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- distillation
- retort
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- lithium
- potassium
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 78
- 238000004821 distillation Methods 0.000 title claims abstract description 68
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 40
- 239000002184 metal Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 39
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002893 slag Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 31
- 239000011734 sodium Substances 0.000 claims description 27
- 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 claims description 24
- 229910052708 sodium Inorganic materials 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 11
- 238000009835 boiling Methods 0.000 claims description 11
- 239000012212 insulator Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000009776 industrial production Methods 0.000 claims description 6
- 239000011344 liquid material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000002093 peripheral effect Effects 0.000 claims description 4
- 239000002699 waste material Substances 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to metal lithium distillation equipment, particularly to low-temperature metal lithium distillation equipment and a distillation method thereof. The low-temperature metal lithium distillation equipment comprises a distillation retort, a heating furnace, a heat-insulating body, a potassium-sodium slag collecting tank, a U-shaped vacuum tube, a control cabinet and a vacuum pump, wherein a distillation pool is arranged at the bottom of the distillation retort, and the distillation pool is provided with a discharge pipe, a feeding pipe and a slagging pipe from the top down; an umbrella-shaped reflow cover is mounted in the middle of the distillation retort; a temperature detector is arranged below the umbrella-shaped reflow cover; a cooling zone is arranged at the upper part of the distillation retort; the potassium-sodium collector is arranged at the upper part of the distillation retort; a cooling jacket is arranged at the exterior of the potassium-sodium collector; the potassium-sodium collector is in pipe connection with the potassium-sodium slag collecting tank arranged at the exterior of the distillation retort; the control cabinet is independently arranged at the exterior of the distillation retort. The distillation method comprises the steps of starting the heating furnace and the vacuum pump, and adding commercial grade metal lithium; materials inside the distillation pool are stirred for sufficient convection up and down; after three hours of distillation operation, high-purity battery grade metal lithium can be obtained; waste material is discharged, and next batch operation is continued.
Description
Technical field
The present invention relates to a kind of metallic lithium distillation plant, particularly a kind of low-temperature metal lithium distillation plant and distillating method thereof.
Background technology
In recent years, along with the continuous progress of technical grade metallic lithium production technology, in the scope that all Control of Impurities outside removal of impurity sodium Metal 99.5 can be required at cell-grade metallic lithium, therefore low-temperature metal lithium distillation plant is then raw mutually.Be characterized under lower temperature conditions, only the lower-boiling impurity sodium Metal 99.5 in metallic lithium need be removed and just can be obtained cell-grade metallic lithium.And needn't adopt traditional pyrogenic distillation method: first need metallic lithium to separate with high-boiling-point impurity (Ca, Mg, Al, Si, Fe and oxide compound etc.) together with lower-boiling impurity potassium metal, sodium simultaneously, the difference of recycling material characteristic, by metallic lithium and lower-boiling impurity potassium metal, sodium secondary separation.Therefore low, the output of low-temperature metal lithium distil process energy consumption is large and be widely used in industrial production.
But this cryogenic distillation apparatus is thorough in order to realize the evaporation of foreign metal sodium, specific mechanical stirring device and corresponding dynamic sealing device need be set, can not realize the full-static sealing operation of device fabrication process, in distillation production process, vacuum tightness is lower and unstable, is normally 5 × 10
-2-5pa, can not stablize and reach more condition of high vacuum degree 5 × 10
-3-5 × 10
-4pa.Therefore, metallic lithium quality product is difficult to ensure and less stable, has the potential safety hazard of sealing leak simultaneously.
Summary of the invention
The object of the invention is provides a kind of low-temperature metal lithium distillation plant and distillating method thereof for above-mentioned weak point, utilizes this equipment without any mechanical stirring device, can realize in low temperature (450 DEG C) and high vacuum (5 × 10
-4pa) operation under condition, produces the high purity battery level metallic lithium of 99.9-99.95%.
A kind of low-temperature metal lithium distillation plant and distillating method thereof take following technical scheme to realize:
A kind of low-temperature metal lithium distillation plant comprises retort, process furnace, thermal insulator, potassium sodium slag holding tank, U-shaped valve tube, housing and vacuum pump, described retort bottom is provided with distillation pond, is connected with from top to bottom discharge nozzle, feed-pipe and scum pipe in distillation pond; At retort middle part, umbrella shape back cover is installed, below umbrella shape back cover, is provided with thermoscope; Retort top is cooling zone, is provided with potassium sodium collector on retort top; Be provided with watercooling jacket in potassium sodium collector outside; Potassium sodium collector is connected with the potassium sodium slag holding tank pipeline that is arranged on retort outside; Be provided with material liquid surface control altitude line in retort bottom, described material liquid surface control altitude line comprises a line and b line, and a line and discharge nozzle lower end are contour, simultaneously contour with the heating region height of process furnace, and b line is positioned at a line top, higher than thermal insulator; The top of retort is connected with vacuum pump by U-shaped valve tube; Housing is independently arranged on retort outside; Process furnace, vacuum pump and the high temperature Liquid sealing valve being connected with discharge nozzle with feed-pipe are all connected with housing, thereby realize the safety in production that whole process is controlled automatically.
Described b line is no less than 600mm higher than a line, is no less than 300mm higher than thermal insulator upper end simultaneously.
The height of described feed-pipe is lower than the height 50-100mm of discharge nozzle.
Described watercooling jacket is welded on potassium sodium collector outside.
Described retort all adopts high temperature Liquid sealing valve flange to be connected with peripheral equipment, to ensure the sealing of retort.
Described thermoscope is higher than b line 50 ~ 100mm, and the change list of its temperature understands the variation of metal vapor amount, thereby provides foundation for the controlled operation of low-temperature metal lithium distillation foreign metal sodium content.
Described thermoscope adopts commercially available industrial thermoscope.
A distillating method that adopts low-temperature metal lithium distillation plant, comprises the steps:
1) start process furnace and vacuum pump, furnace temperature reaches 450 DEG C, and vacuum tightness is 5 × 10
-4under pa condition, add technical grade metallic lithium by feed-pipe, the add-on of controlling metallic lithium material makes in retort more than material liquid surface at least reaches b line place, and now the upper and lower temperature of material differs at least 50 DEG C;
2) material fully convection current stirring up and down in distillation pond, the lower-boiling impurity potassium metal of metallic lithium inside, sodium are constantly brought to material surface and are evaporated;
3) distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtains 99.95% high purity battery level metallic lithium;
4) in retort, lithium liquid material is emitted by discharge nozzle, continues to add technical grade metallic lithium to carry out next batch operation by feed-pipe, thereby realizes serialization industrial production.
Principle of work: when a kind of low-temperature metal lithium distillation plant uses, under condition of high vacuum degree and lower temperature conditions, by controlling material liquid surface height, adopt the method in distillation tank body lower part local heating, utilize the difference of the upper and lower temperature of material in distillation pond to realize the abundant convection current stirring of material, the lower-boiling impurity potassium metal of metallic lithium inside, sodium are constantly brought to material surface and are evaporated, thereby realize separating of lower-boiling impurity metal and metallic lithium.
In distillation operation process, because distillation temperature is lower, metallic lithium stays substantially in distillation pond.After a small amount of metallic lithium evaporating with potassium, sodium is preliminary cooling by umbrella shape back cover, be back in distillation pond, when lower-boiling impurity potassium metal, sodium arrive tank body top cooled region, become liquid metal and retain in potassium sodium collector, be regularly disposed to potassium sodium slag holding tank.
A kind of low-temperature metal lithium of the present invention distillation plant is simple in structure, easy and simple to handle, and production run is safe and reliable, can realize the automatic production control of whole process.Because this equipment is without any mechanical stirring device, tank body all adopts high temperature Liquid sealing valve flange to be connected with peripheral equipment, and metallic lithium is in low-temperature distillation operation process, and tank body is all the time in static seal state.Therefore can realize more condition of high vacuum degree (5 × 10
-4pa) operation under condition, the cell-grade metallic lithium constant product quality obtaining, electrical property excellence.
Brief description of the drawings
Below with reference to accompanying drawing, the invention will be further described:
Fig. 1 is the structural representation of a kind of low-temperature metal lithium of the present invention distillation plant.
In figure: 1, retort, 2, process furnace, 3, thermal insulator, 4, potassium sodium slag holding tank, 5, U-shaped valve tube, 6, distillation pond, 7, umbrella shape back cover, 8, potassium sodium collector, 9, watercooling jacket, 10, thermoscope, 11, discharge nozzle, 12, feed-pipe, 13, scum pipe, 14, housing, 15, vacuum pump.
Embodiment
With reference to accompanying drawing 1, a kind of low-temperature metal lithium distillation plant comprises retort 1, process furnace 2, thermal insulator 3, potassium sodium slag holding tank 4, U-shaped valve tube 5, housing 14 and vacuum pump 15.Described retort 1 bottom is provided with distillation pond 6, is connected with from top to bottom discharge nozzle 11, feed-pipe 12 and scum pipe 13 in distillation pond 6; At retort 1 middle part, umbrella shape back cover 7 is installed, below umbrella shape back cover 7, is provided with thermoscope 10; Retort 1 top is cooling zone, is provided with potassium sodium collector 8 on retort 1 top; Be provided with watercooling jacket 9 in potassium sodium collector 8 outsides; Potassium sodium collector 8 is connected with potassium sodium slag holding tank 4 pipelines that are arranged on retort 1 outside.Be provided with material liquid surface control altitude line in retort 1 bottom, described material liquid surface control altitude line comprises a line and b line, and a line and discharge nozzle 11 lower ends are contour, simultaneously contour with the heating region height of process furnace 2, and b line is positioned at a line top, higher than thermal insulator 3; The top of retort 1 is connected with vacuum pump 15 by U-shaped valve tube 5; Housing 14 is independently arranged on retort 1 outside; Process furnace 2, vacuum pump 15 and the high temperature Liquid sealing valve being connected with discharge nozzle 11 with feed-pipe 12 are all connected with housing 14, thereby realize the safety in production that whole process is controlled automatically.
Described b line is no less than 600mm higher than a line, is no less than 300mm higher than thermal insulator 3 upper ends simultaneously.
The height of described feed-pipe 12 is lower than the height 50-100mm of discharge nozzle 11.
Described watercooling jacket 9 is welded on potassium sodium collector 8 outsides.
Described retort 1 all adopts high temperature Liquid sealing valve flange to be connected with peripheral equipment, to ensure the sealing of retort 1.
Described thermoscope 10 is higher than b line 50 ~ 100mm, and the change list of its temperature understands the variation of metal vapor amount, thereby provides foundation for the controlled operation of low-temperature metal lithium distillation foreign metal sodium content.
Described thermoscope 10 adopts commercially available industrial thermoscope.
A distillating method that adopts low-temperature metal lithium distillation plant, comprises the steps:
1) start process furnace 2 and vacuum pump 15, when furnace temperature reaches 450 DEG C, vacuum tightness is 5 × 10
-4under pa condition, add technical grade metallic lithium by feed-pipe 12, the add-on of controlling metallic lithium material makes in retort more than material liquid surface at least reaches b line place, and now the upper and lower temperature of material differs at least 50 DEG C;
2) the interior material in distillation pond 6 fully convection current stirring up and down, the lower-boiling impurity potassium metal of metallic lithium inside, sodium are constantly brought to material surface and are evaporated;
3) distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtains 99.95% high purity battery level metallic lithium;
4) in retort, lithium liquid material is emitted by discharge nozzle 12, continues to add technical grade metallic lithium to carry out next batch operation by feed-pipe 13, thereby realizes serialization industrial production.
Embodiment 1: start process furnace 2 and vacuum pump 15, when furnace temperature reaches 450 DEG C, in tank, vacuum tightness reaches 5 × 10
-4when pa, add the technical grade metallic lithium (Na content 0.2%) of 50kg by feed-pipe 12, now in retort, material liquid surface reaches a line place, and liquid level is suitable with heating region height, and the upper and lower temperature of material is substantially equal.Distillation operation is after 3 hours, and in lithium liquid, foreign metal sodium content, between 0.1 ~ 0.2%, continues time expand, except sodium DeGrain.
Embodiment 2: start process furnace 2 and vacuum pump 15, when furnace temperature reaches 450 DEG C, vacuum tightness reaches 5 × 10
-4when pa, add the technical grade metallic lithium (Na content 0.2%) of 100kg by feed-pipe 12, now in retort, material liquid surface reaches b line place, and material liquid surface height b line is at least higher than heating region height 600mm, and the upper and lower temperature of material differs at least 50 DEG C.Distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtains 99.95% high purity battery level metallic lithium.In retort, lithium liquid material is emitted by discharge nozzle 11, and now in retort, material liquid surface is got back to a line place.Continue to add the technical grade metallic lithium of 50kg to carry out next batch operation by feed-pipe 12, thereby realize serialization industrial production.
In distillation operation process, because distillation temperature is lower, metallic lithium stays substantially in distillation pond.Lower boiling foreign metal potassium, sodium are along with the upper and lower convection current stirring of material in retort is constantly brought to material surface evaporation, after a small amount of metallic lithium evaporating with potassium, sodium is preliminary cooling by umbrella shape back cover 7, be back in distillation pond 6, when lower-boiling impurity potassium metal, sodium arrive tank body top cooled region, become liquid metal and retain in potassium sodium collector 8, be regularly disposed to potassium sodium slag holding tank 4.
Embodiment 3: start process furnace 2 and vacuum pump 15, when furnace temperature reaches 500 DEG C, vacuum tightness reaches 5 × 10
-3under pa condition, add the high sodium level of 100kg metallic lithium (Na content 1%) by feed-pipe 12, now in retort, material liquid surface reaches b line place, and material liquid surface height b line is at least higher than heating region height 600mm, and the upper and lower temperature of material differs at least 50 DEG C.Distillation operation is after 3 hours, and foreign metal sodium content≤0.02% in lithium liquid, obtains 99.9% cell-grade metallic lithium.In retort, lithium liquid material is emitted by discharge nozzle 11, and now in retort, material liquid surface is got back to a line place.Continue to add the high sodium level of 50kg metallic lithium to carry out next batch operation by feed-pipe 12, thereby realize high sodium level metallic lithium low-temperature distillation serialization industrial production.
Claims (6)
1. a low-temperature metal lithium distillation plant, it is characterized in that: comprise retort, process furnace, thermal insulator, potassium sodium slag holding tank, U-shaped valve tube, housing and vacuum pump, described retort bottom is provided with distillation pond, is connected with from top to bottom discharge nozzle, feed-pipe and scum pipe in distillation pond; At retort middle part, umbrella shape back cover is installed, below umbrella shape back cover, is provided with thermoscope; Retort top is cooling zone, is provided with potassium sodium collector on retort top; Be provided with watercooling jacket in potassium sodium collector outside; Potassium sodium collector is connected with the potassium sodium slag holding tank pipeline that is arranged on retort outside; Be provided with material liquid surface control altitude line in retort bottom, described material liquid surface control altitude line comprises a line and b line, and a line and discharge nozzle lower end are contour, simultaneously contour with the heating region height of process furnace, and b line is positioned at a line top, higher than thermal insulator; The top of retort is connected with vacuum pump by U-shaped valve tube; Housing is independently arranged on retort outside; Process furnace, vacuum pump and the high temperature Liquid sealing valve being connected with discharge nozzle with feed-pipe are all connected with housing, thereby realize the safety in production that whole process is controlled automatically;
Described b line is no less than 600mm higher than a line, is no less than 300mm higher than thermal insulator upper end simultaneously.
2. a kind of low-temperature metal lithium distillation plant according to claim 1, is characterized in that: the height of described feed-pipe is lower than the height 50-100mm of discharge nozzle.
3. a kind of low-temperature metal lithium distillation plant according to claim 1, is characterized in that: described watercooling jacket is welded on potassium sodium collector outside.
4. a kind of low-temperature metal lithium distillation plant according to claim 1, is characterized in that: described retort all adopts high temperature Liquid sealing valve flange to be connected with peripheral equipment, to ensure the sealing of retort.
5. a kind of low-temperature metal lithium distillation plant according to claim 1, is characterized in that: described thermoscope is higher than b line 50 ~ 100mm.
6. a distillating method that adopts low-temperature metal lithium distillation plant claimed in claim 1, is characterized in that, comprises the steps:
1) start process furnace and vacuum pump, furnace temperature reaches 450 DEG C, and vacuum tightness is 5 × 10
-4under pa condition, add technical grade metallic lithium by feed-pipe, the add-on of controlling metallic lithium material makes in retort more than material liquid surface at least reaches b line place, and now the upper and lower temperature of material differs at least 50 DEG C;
2) material fully convection current stirring up and down in distillation pond, the lower-boiling impurity potassium metal of metallic lithium inside, sodium are constantly brought to material surface and are evaporated;
3) distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtains 99.95% high purity battery level metallic lithium;
4) in retort, lithium liquid material is emitted by discharge nozzle, continues to add technical grade metallic lithium to carry out next batch operation by feed-pipe, thereby realizes serialization industrial production.
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| CN201310348064.6A CN103409648B (en) | 2013-08-12 | 2013-08-12 | Low-temperature metal lithium distillation equipment and distillation method thereof |
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|---|---|---|---|
| CN201310348064.6A CN103409648B (en) | 2013-08-12 | 2013-08-12 | Low-temperature metal lithium distillation equipment and distillation method thereof |
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| CN103409648B true CN103409648B (en) | 2014-09-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150232964A1 (en) * | 2014-02-20 | 2015-08-20 | Guizhou Province Product Quality Supervision And Inspection Institute | Method of purifying sodium metal |
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| CN103667708B (en) * | 2013-12-06 | 2015-09-09 | 内蒙古兰太实业股份有限公司 | Process and device for recovering solid sodium metal waste residues |
| CN104388688B (en) * | 2014-11-17 | 2016-07-06 | 东北大学 | A kind of device and method of vacuum metal thermal reduction refining lithium |
| CN108950208B (en) * | 2018-06-04 | 2023-09-29 | 山东习尚喜新材料科技股份有限公司 | Continuous production device and process of metal potassium |
| CN109371240B (en) * | 2018-10-23 | 2024-04-30 | 天齐锂业（江苏）有限公司 | Metal lithium slag recycling equipment and method |
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| CN1184857A (en) * | 1997-11-05 | 1998-06-17 | 北京市吉利源系统工程公司 | Method and equipment for vacuum distillation puritying metallic lithium |
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Effective date of registration: 20191225 Address after: 226400 No.9, Zhenxing 1st Road, juegang Town, Rudong County, Nantong City, Jiangsu Province Patentee after: Nantong Shengneng New Material Technology Co.,Ltd. Address before: 214121 Wuxi high school, Wuxi Institute of Technology, West Road, Jiangsu, No. 1600 Patentee before: Wuxi Institute of Technology |
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