CN103409648A - 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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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, all Control of Impurities that can removal of impurity sodium Metal 99.5 is outer are in the scope that the cell-grade metallic lithium requires, so low-temperature metal lithium distillation plant is given birth to mutually then.Be characterized under lower temperature conditions, only the lower-boiling impurity sodium Metal 99.5 in metallic lithium just need be removed and can be obtained the cell-grade metallic lithium.And needn't adopt traditional pyrogenic distillation method: at first need metallic lithium is separated with high-boiling-point impurity (Ca, Mg, Al, Si, Fe and oxide compound etc.) together simultaneously with lower-boiling impurity potassium metal, sodium, the difference of recycling material characteristic, by metallic lithium and lower-boiling impurity potassium metal, sodium secondary separation.Therefore low-temperature metal lithium distil process energy consumption is low, output large and be widely used in industrial production.
But this cryogenic distillation apparatus is thorough for the evaporation that realizes 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 the 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, the metallic lithium quality product is difficult to guarantee and less stable, has simultaneously the potential safety hazard of sealing leak.
Summary of the invention
The objective 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 ℃) and high vacuum (5 * 10
-4Pa) operation under condition, produce 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 the distillation pond, is connected with from top to bottom discharge nozzle, feed-pipe and scum pipe in the distillation pond; At the retort middle part, the umbrella shape back cover is installed, is provided with thermoscope below the umbrella shape back cover; Retort top is cooling zone, on retort top, is provided with potassium sodium collector; In potassium sodium collector outside, be provided with watercooling jacket; Potassium sodium collector is connected with the potassium sodium slag holding tank pipeline that is arranged on the retort outside; In the retort bottom, be provided with material liquid surface and control altitude line, described material liquid surface is controlled altitude line and is comprised 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 the 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 independently is arranged on the retort outside; Process furnace, vacuum pump reach and all with housing, are connected with the high temperature Liquid sealing valve that feed-pipe is connected with discharge nozzle, thereby realize the safety in production that whole process is controlled automatically.
Described b line is no less than 600mm higher than a line, higher than the thermal insulator upper end, is no less than 300mm 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 guarantee 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 kind of distillating method that adopts low-temperature metal lithium distillation plant, comprise the steps:
1) start process furnace and vacuum pump, furnace temperature reaches 450 ℃, and vacuum tightness is 5 * 10
-4Under the pa condition, add the technical grade metallic lithium by feed-pipe, the add-on of controlling the metallic lithium material makes in retort more than material liquid surface reaches b line place at least, and now the upper and lower temperature of material differs at least 50 ℃;
2) material fully convection current stirring up and down in the distillation pond, the lower-boiling impurity potassium metal of metallic lithium inside, sodium constantly are brought to the material surface and are evaporated;
3) the distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtain 99.95% high purity battery level metallic lithium;
4) in retort, lithium liquid material is emitted by discharge nozzle, continues to add the technical grade metallic lithium to carry out the next batch operation by feed-pipe, thereby realizes the 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 the material liquid surface height, employing is in the method for distillation tank body lower part local heating, utilize the difference of distilling the upper and lower temperature of material in pond to realize the abundant convection current stirring of material, the lower-boiling impurity potassium metal of metallic lithium inside, sodium constantly are brought to material surface and are evaporated, thereby realize separating of lower-boiling impurity metal and metallic lithium.
In the distillation operation process, because distillation temperature is lower, metallic lithium stays substantially in the distillation pond.After a small amount of metallic lithium evaporated with potassium, sodium is preliminary cooling by the umbrella shape back cover, be back in the distillation pond, when lower-boiling impurity potassium metal, sodium arrive tank body top cooled region, become liquid metal and retain in potassium sodium collector, regularly be 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.Without any mechanical stirring device, tank body all adopts high temperature Liquid sealing valve flange to be connected with peripheral equipment due to this equipment, and metallic lithium is in the low-temperature distillation operation process, and tank body is in the static seal state all the time.Therefore can realize more condition of high vacuum degree (5 * 10
-4Pa) operation under condition, the cell-grade metallic lithium constant product quality obtained, electrical property excellence.
The accompanying drawing explanation
The invention will be further described below with reference to accompanying drawing:
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, the 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; In potassium sodium collector 8 outsides, be provided with watercooling jacket 9; Potassium sodium collector 8 is connected with potassium sodium slag holding tank 4 pipelines that are arranged on retort 1 outside.In retort 1 bottom, be provided with material liquid surface and control altitude line, described material liquid surface is controlled altitude line and is comprised 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 the 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 independently is arranged on retort 1 outside; Process furnace 2, vacuum pump 15 reach and all with housing 14, are connected with the high temperature Liquid sealing valve that feed-pipe 12 is connected with discharge nozzle 11, thereby realize the safety in production that whole process is controlled automatically.
Described b line is no less than 600mm higher than a line, higher than thermal insulator 3 upper ends, is no less than 300mm 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 guarantee 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 kind of distillating method that adopts low-temperature metal lithium distillation plant, comprise the steps:
1) start process furnace 2 and vacuum pump 15, when furnace temperature reaches 450 ℃, vacuum tightness is 5 * 10
-4Under the pa condition, add the technical grade metallic lithium by feed-pipe 12, the add-on of controlling the metallic lithium material makes in retort more than material liquid surface reaches b line place at least, and now the upper and lower temperature of material differs at least 50 ℃;
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 constantly are brought to the material surface and are evaporated;
3) the distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtain 99.95% high purity battery level metallic lithium;
4) in retort, lithium liquid material is emitted by discharge nozzle 12, continues to add the technical grade metallic lithium to carry out the next batch operation by feed-pipe 13, thereby realizes the serialization industrial production.
Embodiment 1: start process furnace 2 and vacuum pump 15, when furnace temperature reaches 450 ℃, in tank, vacuum tightness reaches 5 * 10
-4During pa, by feed-pipe 12, add the technical grade metallic lithium (Na content 0.2%) of 50kg, now in retort, material liquid surface reaches a line place, and liquid level is suitable with the heating region height, and the upper and lower temperature of material is substantially equal.The distillation operation is after 3 hours, and in lithium liquid, the foreign metal sodium content, between 0.1 ~ 0.2%, continues time expand, except the sodium DeGrain.
Embodiment 2: start process furnace 2 and vacuum pump 15, when furnace temperature reaches 450 ℃, vacuum tightness reaches 5 * 10
-4During pa, by feed-pipe 12, add the technical grade metallic lithium (Na content 0.2%) of 100kg, 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 ℃.The distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtain 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.Continuation adds the technical grade metallic lithium of 50kg to carry out the next batch operation by feed-pipe 12, thereby realizes the serialization industrial production.
In the distillation operation process, because distillation temperature is lower, metallic lithium stays substantially in the distillation pond.Lower boiling foreign metal potassium, sodium are along with the upper and lower convection current stirring of material in retort constantly is brought to the material surface evaporation, after a small amount of metallic lithium evaporated 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, regularly be disposed to potassium sodium slag holding tank 4.
Embodiment 3: start process furnace 2 and vacuum pump 15, when furnace temperature reaches 500 ℃, vacuum tightness reaches 5 * 10
-3Under the 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 ℃.The distillation operation is after 3 hours, and foreign metal sodium content≤0.02% in lithium liquid, obtain 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.Continuation adds the high sodium level of 50kg metallic lithium to carry out the next batch operation by feed-pipe 12, thereby realizes high sodium level metallic lithium low-temperature distillation serialization industrial production.
Claims (7)
1. 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 the distillation pond, is connected with from top to bottom discharge nozzle, feed-pipe and scum pipe in the distillation pond; At the retort middle part, the umbrella shape back cover is installed, is provided with thermoscope below the umbrella shape back cover; Retort top is cooling zone, on retort top, is provided with potassium sodium collector; In potassium sodium collector outside, be provided with watercooling jacket; Potassium sodium collector is connected with the potassium sodium slag holding tank pipeline that is arranged on the retort outside; In the retort bottom, be provided with material liquid surface and control altitude line, described material liquid surface is controlled altitude line and is comprised 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 the 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 independently is arranged on the retort outside; Process furnace, vacuum pump reach and all with housing, are connected with the high temperature Liquid sealing valve that feed-pipe is connected with discharge nozzle, thereby realize the safety in production that whole process is controlled automatically.
2. a kind of low-temperature metal lithium distillation plant according to claim 1, it is characterized in that: described b line is no less than 600mm higher than a line, higher than the thermal insulator upper end, is no less than 300mm simultaneously.
3. a kind of low-temperature metal lithium distillation plant according to claim 1, it is characterized in that: the height of described feed-pipe is lower than the height 50-100mm of discharge nozzle.
4. a kind of low-temperature metal lithium distillation plant according to claim 1, it is characterized in that: described watercooling jacket is welded on potassium sodium collector outside.
5. a kind of low-temperature metal lithium distillation plant according to claim 1, it is characterized in that: described retort all adopts high temperature Liquid sealing valve flange to be connected with peripheral equipment, to guarantee the sealing of retort.
6. a kind of low-temperature metal lithium distillation plant according to claim 1, it is characterized in that: described thermoscope is higher than b line 50 ~ 100mm.
7. 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 ℃, and vacuum tightness is 5 * 10
-4Under the pa condition, add the technical grade metallic lithium by feed-pipe, the add-on of controlling the metallic lithium material makes in retort more than material liquid surface reaches b line place at least, and now the upper and lower temperature of material differs at least 50 ℃;
2) material fully convection current stirring up and down in the distillation pond, the lower-boiling impurity potassium metal of metallic lithium inside, sodium constantly are brought to the material surface and are evaporated;
3) the distillation operation is after 3 hours, and foreign metal sodium content≤0.005% in lithium liquid, obtain 99.95% high purity battery level metallic lithium;
4) in retort, lithium liquid material is emitted by discharge nozzle, continues to add the technical grade metallic lithium to carry out the next batch operation by feed-pipe, thereby realizes the serialization industrial production.
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CN103667708A (en) * | 2013-12-06 | 2014-03-26 | 内蒙古兰太实业股份有限公司 | Process and device for recovering solid sodium metal waste residues |
CN104388688A (en) * | 2014-11-17 | 2015-03-04 | 东北大学 | Device and method for smelting lithium through vacuum thermal reduction of metal |
CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
CN109371240A (en) * | 2018-10-23 | 2019-02-22 | 天齐锂业(江苏)有限公司 | A kind of lithium metal slag recycling equipment and method |
CN114199936A (en) * | 2021-11-22 | 2022-03-18 | 北京动力机械研究所 | Tester for small evaporation/combustion heat exchange |
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CN103667708A (en) * | 2013-12-06 | 2014-03-26 | 内蒙古兰太实业股份有限公司 | Process and device for recovering solid sodium metal waste residues |
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CN104388688A (en) * | 2014-11-17 | 2015-03-04 | 东北大学 | Device and method for smelting lithium through vacuum thermal reduction of metal |
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 |
CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
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CN109371240A (en) * | 2018-10-23 | 2019-02-22 | 天齐锂业(江苏)有限公司 | A kind of lithium metal slag recycling equipment and method |
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 |
WO2022111228A1 (en) * | 2020-11-30 | 2022-06-02 | 深圳市研一新材料有限责任公司 | Method and device for preparing ultrathin metal lithium foil |
CN114199936A (en) * | 2021-11-22 | 2022-03-18 | 北京动力机械研究所 | Tester for small evaporation/combustion heat exchange |
CN114199936B (en) * | 2021-11-22 | 2024-04-02 | 北京动力机械研究所 | Tester for small evaporation/combustion heat exchange |
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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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