The specific equipment of very-pure metal lithium refining and purification process
Technical field
The utility model relates to the device that the device that a kind of metallic lithium is purified, particularly metallic lithium vacuum distillation are purified.
Background technology
The known technology of metallic lithium method of purification is an electrolytic process.This method can be purified to 96%-99% with the purity of metallic lithium, produces the technical grade metallic lithium.The technical grade metallic lithium is refined to purity 99.9%-99.99%, and Chinese patent metallic lithium vacuum distillation method of purification and device disclose a kind of distillation the purify metals technological process and the equipment of lithium.The technical characterictic of this technological process is: a kind of metallic lithium vacuum distillation method of purification, in the feed stove, the solid feed metallic lithium of heating purity 96%-99%, when temperature is controlled at 200-500 ℃, form liquid penta feed states, pressure is smaller or equal to 0.1 holder, in the evaporation crucible of vacuum distillation furnace, heat liquid feed metal lithium, when temperature is controlled at 600-850 ℃, form the gaseous feed metallic lithium, be evaporated to the heat preservation zone of vacuum distillation furnace, knot matter heavy metal element still keeps liquid state to stay in the evaporation crucible, when the heat preservation zone temperature is controlled at 400-500 ℃, and gaseous state high-purity lithium and impurity element sodium Metal 99.5, potassium separates, condensation forms liquid state, flow into high-purity lithium collector and sodium Metal 99.5 by Liquid sealing valve respectively, the potassium collector is stayed the impurity heavy metal element of evaporation crucible, flows into the waste residue collector by Liquid sealing valve.The circulation of control Liquid sealing valve opens and closes, and feed, heating, insulation, separation, purification and the collection of feed metal lithium are carried out continuously, and the purity of solid feed metallic lithium also can be 99%-99.9%.
Be the custom-designed metallic lithium vacuum distillation purification device of above-mentioned method of purification, comprise feed stove, vacuum distillation furnace, vacuum diffusion facilities, waste residue collector, high-purity lithium collector, sodium Metal 99.5, potassium collector and Liquid sealing valve, airtight valve, pipeline etc., the feed stove is provided with the feed heating installation, and is communicated with vacuum distilling by Liquid sealing valve, pipeline; Vacuum distillation furnace is communicated with the vacuum diffusion facilities by airtight valve, pipeline, the bottom of vacuum distillation furnace is an evaporator crucible, be communicated with the waste residue collector by Liquid sealing valve, pipeline, and be provided with evaporation heating and establish dish, be communicated with the high-purity lithium collector by Liquid sealing valve, pipeline, the top of heat preservation zone is sodium Metal 99.5, potassium cooling zone, and is provided with sodium Metal 99.5, potassium catch tray, and sodium Metal 99.5, potassium catch tray are communicated with sodium Metal 99.5, potassium collector by Liquid sealing valve, pipeline.
Summary of the invention
The purpose of this utility model is to propose a kind of under the optional condition of raw material, can carry out 99.95% and 99.995% content refining simultaneously purification branch receives, adopt the removal of impurities in advance of millipore filtration flowing water branch, secondary repeats removal of impurities, thoroughly remove visible impurity, and improve the speed and the time of high temperature removal of impurities, thereby improved product production, purity can reach more than 99.995%, reaches as high as the specific equipment of 99.999% very-pure metal lithium refining and purification process.
The purpose of this utility model is achieved through the following technical solutions.
The ultimate principle that the distillation of the technical program is purified is: various metals do not have element at a certain temperature, has different vapour pressures, utilize the difference characteristic of velocity of evaporation and condensing rate, impurity element (mainly being sodium Metal 99.5, potassium element and other heavy metals) is separated with metallic lithium, thereby reach the purification purpose.Under differing temps, the ratio of the vapour pressure of impurity element and the vapour pressure of metallic lithium is called relative evaporation rate, represents it with A.Its formula is A=Px/PLi, Px: the vapour pressure of impurity element, PLi: the vapour pressure of metallic lithium.When A>1, the impurity element evaporation rate is greater than the evaporation rate of metallic lithium; When A<1, the impurity element evaporation rate is less than the evaporation rate of metallic lithium; When A=1, the impurity element evaporation rate equals the evaporation rate of metallic lithium.In the process of heating raw lithium, the vaporization vaporization temperature in control different operating zone can be come out separation of foreign elements contained in the raw material lithium, thereby reaches the purpose of distilling the lithium of purifying metals.
Very-pure metal lithium refining and purification process divides three big step flowing water purifications:
A, low-temperature condition filtering and impurity removing,
By change the material stove with the technical grade metallic lithium at 200~300 ℃, vacuum tightness 2.5 * 10-2Pa is with interior melt into liquid state, carry out coarse filtration by strainer, first portion removes with visible foreign material, be transported to sedimentation furnace No. one by the chimney filter road, and guarantee to carry the pipe valve temperature between 200~300 ℃, feed liquid is advanced a sedimentation furnace by change material stove must stop sedimentation in 1-3 hour, temperature is controlled at 200~300 ℃ and is incubated, the vacuum tightness of material stove requires the vacuum tightness less than a sedimentation furnace in the time of punishment in advance, deliver to sedimentation furnace No. two by the smart feed liquid of filtering of sedimentation furnace middle filtrator again, insulation, negative pressure, feed liquid enters to observe the watch-keeping cubicle by pipe-line transportation after the sedimentation, examine by visor, adjusting control valve control feed liquid drop flow was not more than 40-90 and drips warm the heating except that potassium during the watch-keeping cubicle feed liquid flows into by pipeline in per 1 minute, sodium equipment;
Preliminary removal of impurity potassium metal, sodium under b, the middle temperature environment,
Temperature heating in entering, temperature is controlled between 450~480 ℃, make potassium, sodium in the feed liquid become steam, enter refining furnace, and the metallic lithium shape that is in a liquid state flows into the groove that spirals, rotary mobile increase surface-area effectively volatilizees potassium, sodium, holding tray spin slot ditch regional temperature is between 500~580 ℃, feed liquid flows into bearing container through the pipeline of disc type groove end opening, again through pipeline flow into 99.95% outer pure lithium receptor of refining furnace or close carry the pipe valve feed liquid to overflow bearing container inflow refining furnace at the bottom of crucible heat;
C, high temperature refining purifying lithium metal, removal of impurity potassium metal, sodium and impurity heavy metal element once more,
Temperature is controlled between 700~750 ℃ during high temperature, at this moment lithium liquid forms lithium vapor, volatilization rises to the umbrella hood condensation and receives, the umbrella hood regional temperature is controlled between 450~480 ℃, 99.995% pure lithium receptor outside pipeline flows into refining furnace, the heat preservation zone regional temperature is controlled between 200~250 ℃, and potassium, sodium condensation are received, flow into refining furnace outer potassium, sodium receptor through pipeline, the impurity heavy metal element sinks stays crucible heating region at the bottom of the refining furnace.
The specific equipment of described very-pure metal lithium refining and purification process: comprising material stove, refining furnace, vacuum diffusion facilities, deslagging receptor, 99.95% pure lithium receptor, potassium, sodium receptor and conveying pipe valve, pipeline etc., change the material stove and be provided with the feed heating installation, and by carrying pipe valve, pipeline to be communicated with refining furnace; Refining is jealous of by carrying pipe valve, pipeline is communicated with the vacuum diffusion facilities, the bottom of refining furnace is an evaporator crucible, by carrying pipe valve, pipeline is communicated with the deslagging receptor, and be provided with the evaporation heating installation, by carrying pipe valve, pipeline is communicated with the very-pure metal lithium collector, the top of heat preservation zone is sodium Metal 99.5, the potassium cooling zone, by carrying pipe valve, pipeline and potassium, the sodium receptor is communicated with, it also comprises sedimentation furnace of cascade filtration removal of impurities precipitation apparatus, No. two sedimentation furnace, middle temperature heating removes potassium, sodium equipment and 99.995% pure lithium receptor, be provided with strainer in describedization material stove and a sedimentation furnace, strainer is communicated with a sedimentation furnace and No. two sedimentation furnace respectively by filter pipe, the conveying pipe valve is set on the described filter pipe, described No. two sedimentation furnace are removed potassium by pipeline and the heating of middle temperature, sodium equipment is communicated with, and described middle temperature heating removes potassium, sodium equipment is connected with refining furnace by pipeline; Be provided with the disc type groove in the described refining furnace, the refining furnace top is provided with the umbrella hood condenser; The pipeline opening that the temperature heating is connected with refining furnace except that potassium, sodium equipment in described is arranged on the place suitable for reading of refining furnace disc type groove, and the end opening of disc type groove is communicated with transfer lime, and described transfer lime is corresponding with the bearing container that is connected with pipe connecting in refining furnace; Described pipe connecting is provided with the conveying pipe valve and is connected with refining furnace 99.95% pure lithium receptor outward; The end opening place of described umbrella hood condenser is connected with transport pipe, and described transport pipe is provided with the conveying pipe valve, and communicates with refining furnace 99.995% pure lithium receptor outward; The bottom of a described sedimentation furnace, No. two sedimentation furnace, refining furnace is by pipeline and carry pipe valve to be connected with the deslagging receptor separately.
The specific equipment of described very-pure metal lithium refining and purification process comprises that also one observes the watch-keeping cubicle, described No. two sedimentation furnace are connected with the observation watch-keeping cubicle by pipeline, described pipeline is provided with control valve, described observation watch-keeping cubicle also is provided with visor, and described observation watch-keeping cubicle is connected except that potassium, sodium equipment with middle temperature heating by pipeline.
The specific equipment of described very-pure metal lithium refining and purification process comprises that also one observes the liquid level stove, and described observation liquid level stove communicates with refining furnace by pipeline.
The utility model has the advantages that: propose a kind of under the optional condition of raw material, can carry out 99.95% and 99.995% content refining simultaneously purification branch receives, adopt the removal of impurities in advance of millipore filtration flowing water branch, secondary repeats removal of impurities, thoroughly remove visible impurity, and improve the speed and the time of high temperature removal of impurities, thereby improved product production, purity can reach more than 99.995%, reaches as high as the specific equipment of 99.999% very-pure metal lithium refining and purification process.Low-temperature condition adopts millipore filtration thoroughly to remove visible impurity in advance, and keeping away to exert oneself influences purifying velocity; In select for use under the warm environment groove formula of spiraling to increase that the lithium solution surface is long-pending to reach the effect of removing potassium, sodium fast, for the high temperature refining provides the good premise condition; The high temperature refining is purified the lithium metal is become lithium vapor, becomes column to rise through the cooling of umbrella hood zone, makes lithium vapor become lithium solution and directly receives on top.
Description of drawings
Accompanying drawing 1 is the structural representation of the utility model very-pure metal lithium refining and purification process specific equipment;
Sequence number among the figure: 1, change the material stove, 2, strainer, 3, filter pipe, 4, a sedimentation furnace, 5, carry pipe valve, 6, No. two sedimentation furnace, 7, pipeline, 8, observe the watch-keeping cubicle, 9, visor, 10, control valve, 11, middle temperature heating removes potassium, sodium equipment, 12, refining furnace, 13, the groove that spirals, 14, bearing container, 15,99.95% pure lithium receptor, 16, evaporator crucible, 17, the umbrella hood condenser, 18,99.995% pure lithium receptor, 20, potassium, the sodium receptor, 21, the deslagging receptor, 23, the vacuum diffusion facilities, 24, transfer lime, 25, pipe connecting, 26, transport pipe, 27, observe the liquid level stove.
Embodiment
The embodiment of the utility model device is described below in conjunction with accompanying drawing.
Very-pure metal lithium refining and purification process divides three big step flowing water purifications:
A, low-temperature condition filtering and impurity removing,
By change material stove 1 with content 85% technical grade metallic lithium at 260 ℃, vacuum tightness 2.5 * 10-2Pa is with interior melt into liquid state, carry out coarse filtration by strainer 2, first portion removes with visible foreign material, be transported to sedimentation furnace 4 No. one by chimney filter road 3, and guarantee to carry pipe valve 5 temperature at 260 ℃, feed liquid is advanced a sedimentation furnace by change material stove must stop sedimentation in 2 hours, temperature is controlled at 260 ℃ and is incubated, the negative pressure of material stove requires the pressure less than a sedimentation furnace in the time of punishment in advance, deliver to sedimentation furnace 6 No. two by the sedimentation furnace middle filtrator 2 smart feed liquids of filtering again, insulation, negative pressure, feed liquid is delivered into by pipeline 7 and observes watch-keeping cubicle 8 after the sedimentation, examine by visor 9, adjusting control valve 10 control feed liquid drop flows, per 1 minute 60, the temperature heating removed potassium during the watch-keeping cubicle feed liquid flowed into by pipeline 7, sodium equipment 11;
Preliminary removal of impurity potassium metal, sodium under b, the middle temperature environment,
Temperature heating in entering, temperature is controlled at 460 ℃, make potassium, sodium in the feed liquid become steam, enter refining furnace 12, and the metallic lithium shape that is in a liquid state flows into the groove 13 that spirals, rotary mobile increase surface-area effectively volatilizees potassium, sodium, holding tray spin slot ditch regional temperature is at 560 ℃, feed liquid flows into bearing containers 14 through the pipeline 7 of disc type groove 13 end openings, again through pipeline 7 flow into 99.95% outer pure lithium receptor 15 of refining furnaces or close carry pipe valve 5 feed liquids to overflow bearing container 14 inflow refining furnaces at the bottom of crucible 16 heat;
C, high temperature refining purifying lithium metal, removal of impurity potassium metal, sodium and impurity heavy metal element once more,
Temperature is controlled at 730 ℃ during high temperature, at this moment lithium liquid forms lithium vapor, volatilization rises to umbrella hood 17 condensations and receives, the umbrella hood regional temperature is controlled at 460 ℃, through the 99.995% pure lithium receptor 18 that pipeline 7 flows into outside the refining furnace, the heat preservation zone regional temperature is controlled at 230 ℃, and potassium, sodium condensation are received, flow into refining furnaces outer potassium, sodium receptor 20 through pipeline 7, the impurity heavy metal element sinks stays crucible 16 heating regions at the bottom of the refining furnace.
The specific equipment of described very-pure metal lithium refining and purification process: comprising material stove 1, refining furnace 12, vacuum diffusion facilities 23, deslagging receptor 21,99.95% pure lithium receptor 15, potassium, sodium receptor 20 and conveying pipe valve 5, pipeline 7 etc., change material stove 1 and be provided with the feed heating installation, and by carrying pipe valve 5, pipeline 7 to be communicated with refining furnace 12; Refining furnace 12 is by carrying pipe valve 5, pipeline 7 is communicated with vacuum diffusion facilities 23, the bottom of refining furnace 12 is an evaporator crucible 16, by carrying pipe valve 5, pipeline 7 is communicated with deslagging receptor 21, and be provided with the evaporation heating installation, by carrying pipe valve 5, pipeline 7 is communicated with the very-pure metal lithium collector, the top of heat preservation zone is sodium Metal 99.5, the potassium cooling zone, by carrying pipe valve 5, pipeline 7 and potassium, sodium receptor 20 is communicated with, it also comprises sedimentation furnace 4 of cascade filtration removal of impurities precipitation apparatus, No. two sedimentation furnace 6, middle temperature heating removes potassium, sodium equipment 11 and 99.995% pure lithium receptor 18, be provided with strainer 2 in describedization material stove 1 and a sedimentation furnace 4, strainer 2 is communicated with a sedimentation furnace 4 and No. two sedimentation furnace 6 respectively by filter pipe 3, be provided with on the described filter pipe 3 and carry pipe valve 5, described No. two sedimentation furnace 6 are removed potassium by pipeline 7 and middle temperature heating, sodium equipment 11 is communicated with, and described middle temperature heating removes potassium, sodium equipment 11 is connected with refining furnace 12 by pipeline 7; Be provided with disc type groove 13 in the described refining furnace, the refining furnace top is provided with umbrella hood condenser 17; The pipeline opening that the temperature heating is connected with refining furnace 12 except that potassium, sodium equipment 11 in described is arranged on the place suitable for reading of refining furnace disc type groove 13, the end opening of disc type groove 13 is communicated with transfer lime 24, and described transfer lime 24 is corresponding with the bearing container 14 that is connected with pipe connecting 25 in refining furnace; Described pipe connecting 25 is provided with conveying pipe valve 5 and is connected with refining furnace 99.95% pure lithium receptor 15 outward; The end opening place of described umbrella hood condenser 17 is connected with transport pipe 26, and described transport pipe 26 is provided with carries pipe valve 5, and communicates with refining furnace 99.995% pure lithium receptor 18 outward; The bottom of a described sedimentation furnace, No. two sedimentation furnace, refining furnace is by pipeline and carry pipe valve to be connected with deslagging receptor 21 separately, the specific equipment of described very-pure metal lithium refining and purification process, comprise that also one observes watch-keeping cubicle 8, described No. two sedimentation furnace 6 are connected with observation watch-keeping cubicle 8 by pipeline 7, described pipeline 7 is provided with control valve 10, described observation watch-keeping cubicle 8 also is provided with visor 9, and described observation watch-keeping cubicle 8 is connected except that potassium, sodium equipment 11 with middle temperature heating by pipeline 7; The specific equipment of described very-pure metal lithium refining and purification process comprises that also one observes liquid level stove 27, and described observation liquid level stove 27 communicates with refining furnace 12 by pipeline 7.
Divide three big step flowing water purifications:
1, low-temperature condition adopts millipore filtration to adopt the removal of impurities in advance of millipore filtration flowing water branch, and secondary repeats removal of impurities, thoroughly removes visible impurity, through the twice precise microfiltration, carry out a sedimentation after removing visible impurity, the secondary settlement heavy metal element, keeping away to exert oneself influences purifying velocity.
2, select for use the groove formula increase lithium solution surface of spiraling to amass under the middle temperature environment and reach the effect of removing potassium, sodium fast, for the high temperature refining provides the good premise condition; By the heating of middle temperature remove potassium, sodium equipment is auxiliary heats up, and makes potassium, sodium form steam in the dish chamber and slightly goes on foot separation, removes potassium, sodium, this moment, lithium liquid flow to the groove that spirals, and potassium, sodium vapor enter the volatilization of refining furnace chamber, for once removing sodium; The temperature in groove zone of spiraling is controlled between 500~580 ℃, carries out secondary and removes potassium, sodium; The spiral effect of groove, it is long-pending to be intended to increase the lithium solution surface, stays lithium solution trickling speed, prolongs the time of removing potassium, sodium, because of being that continuous flow does not influence under the preceding topic of output and fully removes potassium, sodium.
3, the high temperature refining is purified the lithium metal is become lithium vapor, becomes column to rise through the cooling of umbrella hood zone, makes lithium vapor become lithium solution and directly receives on top; Temperature is controlled between 700~750 ℃ during high temperature, at this moment lithium liquid is under the situation of removing visible impurity and potassium, sodium, directly form lithium vapor, volatilization rises to the umbrella hood condensation and receives, the umbrella hood regional temperature is controlled between 450~480 ℃, be convenient to potassium, sodium vapor and evaporate into heat preservation zone and receive potassium, sodium, form liquid best effect after reaching the lithium vapor condensation simultaneously; The regional temperature of heat preservation zone is controlled between 200~250 ℃, and potassium, sodium condensation are received.