CN203639529U - Rare earth distillation and purification device - Google Patents

Rare earth distillation and purification device Download PDF

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Publication number
CN203639529U
CN203639529U CN201320816203.9U CN201320816203U CN203639529U CN 203639529 U CN203639529 U CN 203639529U CN 201320816203 U CN201320816203 U CN 201320816203U CN 203639529 U CN203639529 U CN 203639529U
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China
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crucible
surge drum
collector
longitudinal
heater shell
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CN201320816203.9U
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Chinese (zh)
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黄美松
成维
贾帅广
杨露辉
樊玉川
王志坚
苏正夫
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HUNAN RESEARCH INSTITUTE OF RARE EARTH METAL MATERIALS
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HUNAN RESEARCH INSTITUTE OF RARE EARTH METAL MATERIALS
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The utility model provides a rare earth distillation and purification device, which comprises a furnace body shell, a furnace cover, and a crucible, as well as a collecting drum, a transverse collector and a longitudinal collector, wherein the furnace cover covers the top end of the furnace body shell, the crucible is arranged in the furnace body shell; the collecting tube is sheathed at the top of the crucible; the transverse collector can be driven to the top of the collecting drum along with a horizontal direction; and the longitudinal collector can be driven to the top of the collecting drum along a longitudinal direction. The device can realize the impurity removal, metal distillation and black removal by one step instead of three steps, so that the production procedures can be decreased and the production efficiency can be improved. In the distillation process, the majority of impurities with high steam pressure are collected on the transverse collector, impurities with low steam pressure are left in the crucible, metal is collected in the longitudinal collector, so that cross pollution can be decreased, and the purity of the metal can be improved.

Description

Rare earth distilation device
Technical field
The utility model relates to Rare earth metal metallurgy field, especially, relates to a kind of rare earth distilation device.
Background technology
Existing rare earth metal distil process adopts multi-stage type distil process more.First under the fusing point lower than metal to be distilled, carry out low-temperature distillation removal of impurities.This method is particularly suitable for the purification of metals that calciothermic reduction is obtained.In the metal that calciothermic reduction obtains, calcium contents is higher, before distillation metal, needs first deliming.And calcium vapour pressure is larger, calcium just can separate at low temperatures from metal, and volatilization is attached on collector, then cooling coming out of the stove.The distilation technique of for example rare earth metal scandium need to be distilled deliming in 1.5 hours at 1200~1400 ℃.After metal is come out of the stove after deliming, need the collector of changing crucible top again to carry out the distillation of metal.First volatilize and be condensate on collector owing to again distilling the high impurity of time part vapour pressure, peeling off metallic surface that collector obtains has some impurity to embed wherein to form some spots, and gained metal need to be except black toward contact.This technique is through distilling calcium, distillation metal, removing black three process, and the production time is long, and labour intensity is large, and production cost is high.Peel off the loss that also can cause metal in product process in order to remove sub-fraction impurity, reduce this very low distillation rate.
Utility model content
The utility model object is to provide a kind of rare earth distilation device, and to solve, in prior art, to distill in rare earth metal process the production time long, and labour intensity is large, and production cost is high, and rare earth metal loses large technical problem.
For achieving the above object, provide a kind of rare earth distilation device according to the utility model, comprise body of heater shell, be covered on body of heater shell top bell, be installed on the crucible in body of heater shell, also comprise surge drum, lateral collection device and longitudinal collector; Surge drum is sheathed on crucible top, and lateral collection device can along continuous straight runs be urged to the top of surge drum; Longitudinally collector can longitudinally be urged to the top of surge drum.
Further, longitudinally collector (3) bottom surface is provided with the first groove, and the bottom surface of lateral collection device is provided with the second groove, and the outer rim of the first groove and the second groove is alignd with the top outer rim of surge drum respectively.
Further, longitudinally in collector and lateral collection device, condensing works is all installed.
Further, also comprise screen cloth, screen cloth be installed on the top of crucible and be sandwiched in crucible and the abutted surface of surge drum on.
Further, the top outer rim of crucible and the bottom outer rim of surge drum are alignd.
Further, longitudinally collector comprises longitudinal drive, and longitudinal drive is installed on bell center; Lateral collection device comprises horizontal driving mechanism, and laterally driving mechanism is installed on the sidewall of body of heater shell near bell.
Further, outwardly formation tongue on the sidewall of body of heater shell near one end of bell, laterally driving mechanism is installed in tongue.
Further, also comprise heating element, thermoscreen, heating element arranges around crucible outer wall, and thermoscreen is put in the winding of heating element outer ring.
Further, also comprise thermal baffle, the top of surge drum is installed on thermal baffle center, and thermal baffle outside joins fixing with the inside of body of heater shell.
The utlity model has following beneficial effect:
Device one step that the utility model provides realizes removal of impurities, metal distillation, removes black three-procedure, has reduced production process, has improved production efficiency.The impurity that in still-process, most of vapour pressure is high is collected on lateral collection device, and the impurity that steam forces down remains in crucible, and metal is collected on longitudinal collector, has reduced crossed contamination, has improved the purity of metal.
Except object described above, feature and advantage, the utility model also has other object, feature and advantage.Below with reference to figure, the utility model is described in further detail.
Accompanying drawing explanation
The accompanying drawing that forms the application's a part is used to provide further understanding of the present utility model, and schematic description and description of the present utility model is used for explaining the utility model, does not form improper restriction of the present utility model.In the accompanying drawings:
Fig. 1 is the schematic diagram of the utility model preferred embodiment.
Marginal data:
1, longitudinal drive; 2, bell; 3, longitudinal collector; 4, lateral collection device; 5, horizontal driving mechanism; 6, thermal baffle; 7, surge drum; 8, screen cloth; 9, thermoscreen; 10, heating element; 11, crucible; 12, body of heater shell; 120, tongue; 31, the first groove; 41, the second groove.
Embodiment
Below in conjunction with accompanying drawing, embodiment of the present utility model is elaborated, but the multitude of different ways that the utility model can be defined by the claims and cover is implemented.
Referring to Fig. 1, the utility model provides rare earth distilation device to comprise bell 2, body of heater shell 12, longitudinal drive 1, longitudinal collector 3, horizontal driving mechanism 5, lateral collection device 4, thermal baffle 6, surge drum 7, screen cloth 8 thermoscreens 9, heating element 10 and crucible 11.
Body of heater shell 12 is positioned on ground, and the end face of body of heater shell 12 is uncovered, covers bell 2 on it.Bell 2 installation of aliging with body of heater shell 12 outer walls.Longitudinal drive 1 is installed in bell 2 centers.One end of longitudinal drive 1 is fixed on bell 2, and the other end stretches in bell 2 and is connected with longitudinal collector 3, and controls longitudinal collector 3 and move.Longitudinally the bottom of collector 3 is installed on longitudinal drive 1, and longitudinally the end face of collector 3 is provided with the first groove 31.Longitudinally collector 3 inside are provided with multiple prolongs or condensation loop, in prolong or condensation loop, be connected with water coolant, so that longitudinal collector 3 temperature are reduced, when having steam to move up to longitudinal collector 3 and being gathered in the first groove 31, meet cold coagulating, be convenient to follow-up collection.
Body of heater shell 12 is outwardly near a side sidewall of bell 2, forms tongue 120.Laterally one end of driving mechanism 5 is fixedly installed in tongue 120, and the other end stretches into body of heater shell 12 and lateral collection device 4 is installed.Lateral collection device 4 one sides are fixedly installed on horizontal driving mechanism 5.The bottom surface of lateral collection device 4 is provided with the second groove 41.Inner multiple prolongs or the condensation loop of installing of lateral collection device 4, passes into water coolant in prolong or condensation loop.
As long as obviously longitudinal drive 1, longitudinally collector 3, laterally driving mechanism 5, lateral collection device 4, installation site can guarantee longitudinal drive 1 and laterally driving mechanism 5 not at same position, and can move along the vertical and lateral respectively to surge drum 7 tops, as horizontal driving mechanism 5 is installed on body of heater shell 12 inwalls higher than surge drum 7, longitudinal drive 1 is installed on just on the bell 2 of surge drum 7.Laterally driving mechanism 5 locks mutually with longitudinal drive 1, in the time that horizontal driving mechanism 5 drives lateral collection device 4 to move, longitudinal drive 1 transfixion, treat that lateral collection device 4 completes collection process, laterally driving mechanism 5 drives lateral collection device 4 from surge drum 7 top mobile to static enlightenment position, after static, longitudinal drive 1 just starts to drive longitudinal collector 3 to move to surge drum 7 tops, starts the process that longitudinal collector 3 is collected.
Body of heater shell 12 is installed thermal baffle 6 near bell 2 one sides.The installation site of thermal baffle 6 is lower than tongue 120.Thermal baffle 6 centers are for being provided with surge drum 7 open holess, and one end of surge drum 7 is sheathed in thermal baffle 6 open holess, and protrudes from thermal baffle 6.Surge drum 7 is tubulose, and two-port is uncovered.The outer rim of the protruding end of surge drum 7 is alignd with the outer rim of the first groove 31 and the second groove 41 respectively.
Surge drum 7 bottoms are installed on screen cloth 8.Screen cloth 8 is sheet cover plate, and screen cloth 8 is installed on crucible 11 end faces.Surge drum 7 bottom outer rims, screen cloth 8 outer rims and crucible 11 top outer rim alignment.Crucible 11 is installed on the support of body of heater shell 12 bottoms.The outer side wall of crucible 11 is attached with the heating element 10 of tubular.The outside of heating element 10 is provided with thermoscreen 9.Thermoscreen 9 end faces and thermal baffle 6 bottom surfaces join, and thermoscreen 9 bottom surfaces and body of heater shell 12 inner bottom surfaces join.
When use, reaction raw materials is dropped in crucible 11, crucible 11 is put into body of heater shell 12.On crucible 11 end faces, screen cloth 8 is installed, surge drum 7 is installed on screen cloth 8.Cover thermal baffle 6, then cover bell 2.Drive lateral collection device 4 to be covered on surge drum 7 end faces, vacuumize, make the interior vacuum tightness of stove higher than 5*10 -2pa.Be warming up to the first distillation temperature (1150~1300 ℃) insulation (0.5~2 hour).The impurity that now vapour pressure is higher distills out from rare earth metal, is moved upward on the second groove 41 of lateral collection device 4 with steam, separates out on lateral collection device 4 after running into the second groove 41 condensations.Treat that the material distilling is separated out under the first distillation temperature after, stop insulation.Lateral collection device 4 is driven and leaves surge drum 7, longitudinal collector 3 is driven and is covered on surge drum 7.By heating element 10, interior crucible 11 temperature is increased to the second temperature (1600~1750 ℃) insulation 2~5 hours, with by the rare earth fractionation by distillation in crucible 11.The metal vapors now distilling out moves up and runs into the second groove 41 condensations of longitudinal collector 3, is attached on the second groove 41.After treating the distillation of this material, close heating power supply, stop heating, after being cooled to room temperature, open bell 2, take the impurity that in crucible 11, entrained steam forces down after each parts apart.In above-mentioned still-process, on screen cloth 8, be provided with hole, can rise to collector with the steam of distillation generation by some dust impurity of baffle element, caught by collector, improve the purity of gained scandium.Adopt this device distillation scandium, the purity 99.99% of gained scandium.Before and after distillation, material damage is less, has improved production efficiency, only needs single flash just plurality of impurities and scandium can be separated, and has reduced follow-up processing links again.
Screen cloth 8 used can be by tungsten, tantalum is arbitrary makes.The screen cloth 8 that these materials make can be high temperature resistant, can not produce other impurity again.
Embodiment
Embodiment 1
Carry out the distilation of scandium by this device.Raw material is the as-reduced metal scandium of 1.3kg, and raw material is packed in crucible, and upper cover screen cloth, puts surge drum, shove charge.Wherein collector is tantalum matter, and screen cloth adopts tantalum matter.Cover after bell, regulate laterally and drive, make the closely sealed top that is placed on surge drum of lateral collection device.After adjusting, be warming up to 1250 ℃ of insulations 1 hour.After insulation finishes, regulate laterally to drive to make lateral collection device leave surge drum top, regulate longitudinally to drive to make that longitudinal collector is closely sealed to be placed on surge drum.Then continue to be warming up to 1600 ℃ of insulations 3 hours.
Each foreign matter content analysis contrast before and after table 1 embodiment 1 distillation
? Fe/% Al/% Ca/% W/% Si/% Ta/%
Before distillation 0.0200 0.0035 0.1000 6.000 0.0024 0.0005
After distillation 0.0015 0.0007 0.0005 0.0001 0.0014 0.0001
The scandium metal net weight that distillation obtains is 1080g.After distillation, the purity of scandium reaches 99.99%.
Embodiment 2
Adopt this device to carry out the distilation of terbium metal, concrete implementation step is as follows: the as-reduced metal terbium that raw material is 1.1kg, raw material is packed in crucible, and upper cover screen cloth, puts surge drum, shove charge.Regulate laterally and drive, make the closely sealed top that is placed on surge drum of lateral collection device.After adjusting, be warming up to 1200 ℃ of insulations 1 hour.After insulation finishes, regulate laterally to drive to make lateral collection device leave surge drum top, regulate longitudinally to drive to make that longitudinal collector is closely sealed to be placed on surge drum.Then continue to be warming up to 1800 ℃ of insulations 3 hours.
Each foreign matter content analysis contrast before and after table 2 embodiment 2 distillations
? Fe/% Ca/% Ni/% Si/% O/% C/%
Before distillation 0.0900 0.2000 0.0100 0.0032 0.1200 0.0100
After distillation 0.0095 0.0027 0.0030 0.0014 0.0160 0.0060
The terbium metal total amount that distillation obtains is 820g.After distillation, the purity of terbium reaches 99.94%.
Embodiment 3
Adopt this device to carry out the distillation of metal holmium, concrete implementation step is as follows: the as-reduced metal holmium that raw material is 1.5kg, raw material is packed in crucible, and upper cover screen cloth, puts surge drum, shove charge.Wherein collector is tantalum matter, and screen cloth adopts tantalum matter.Regulate laterally and drive, make the closely sealed top that is placed on surge drum of lateral collection device.After adjusting, be warming up to 1250 ℃ of insulations 1 hour.After insulation finishes, regulate laterally to drive to make lateral collection device leave surge drum top, regulate longitudinally to drive to make that longitudinal collector is closely sealed to be placed on surge drum.Then continue to be warming up to 1680 ℃ of insulations 3 hours.
Each foreign matter content analysis contrast before and after table 3 embodiment 3 distillations
? Fe/% Ca/% C/% Si/% O/% Ni
Before distillation 0.0310 0.2400 0.0180 0.0064 0.1600 0.0250
After distillation 0.0085 0.0018 0.0037 0.0014 0.0090 0.0080
The holmium total metal content that distillation obtains is 1250g.After distillation, the purity of holmium reaches 99.95%.
From embodiment 1~3 acquired results, adopt the generator distillation of the utility model institute to process after the rare-earth metal material that contains scandium, terbium, holmium, the rare earth metal loss that distillation obtains is little, purity is high, impurity good separating effect, and there is no subsequent treatment process, thereby can improve industrial production efficiency, once make purity and reach 99.95% above high pure rare earth metals.
These are only preferred embodiment of the present utility model, be not limited to the utility model, for a person skilled in the art, the utility model can have various modifications and variations.All within spirit of the present utility model and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection domain of the present utility model.

Claims (9)

1. a rare earth distilation device, comprise body of heater shell (12), be covered on described body of heater shell (12) top bell (2), be installed on the crucible (11) in body of heater shell (12), it is characterized in that, also comprise surge drum (7), lateral collection device (4) and longitudinal collector (3);
Described surge drum (7) is sheathed on described crucible (11) top, and described lateral collection device (4) can along continuous straight runs be urged to the top of described surge drum (7); Described longitudinal collector (3) can longitudinally be urged to the top of described surge drum (7).
2. device according to claim 1, it is characterized in that, described longitudinal collector (3) bottom surface is provided with the first groove (31), the bottom surface of described lateral collection device (4) is provided with the second groove (41), and the outer rim of described the first groove (31) and described the second groove (41) is alignd with the top outer rim of described surge drum (7) respectively.
3. device according to claim 1, is characterized in that, in described longitudinal collector (3) and described lateral collection device (4), condensing works is all installed.
4. according to the device described in claim 2 or 3, it is characterized in that, also comprise screen cloth (8), described screen cloth (8) is installed on the top of described crucible (11) and is sandwiched on the abutted surface of described crucible (11) and described surge drum (7).
5. device according to claim 4, is characterized in that, the top outer rim of described crucible (11) is alignd with the bottom outer rim of described surge drum (7).
6. device according to claim 5, is characterized in that, described longitudinal collector (3) comprises longitudinal drive (1), and described longitudinal drive (1) is installed on described bell (2) center; Described lateral collection device (4) comprises horizontal driving mechanism (5), and described horizontal driving mechanism (5) is installed on described body of heater shell (12) near on the sidewall of bell (2).
7. device according to claim 6, it is characterized in that, described body of heater shell (12) is near outwardly formation tongue (120) on the sidewall of one end of bell (2), and described horizontal driving mechanism (5) is installed in described tongue (120).
8. device according to claim 7, it is characterized in that, also comprise heating element (10), thermoscreen (9), described heating element (10) is around described crucible (11) outer wall setting, and thermoscreen (9) is put in described heating element (10) outer ring winding.
9. device according to claim 8, it is characterized in that, also comprise thermal baffle (6), the top of described surge drum (7) is installed on described thermal baffle (6) center, and described thermal baffle (6) outside joins fixing with the inside of described body of heater shell (12).
CN201320816203.9U 2013-12-11 2013-12-11 Rare earth distillation and purification device Expired - Lifetime CN203639529U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107937738A (en) * 2017-12-21 2018-04-20 李本根 A kind of new purifying plant for rare earth feed liquid
CN109517997A (en) * 2018-12-12 2019-03-26 湖南稀土金属材料研究院 A kind of rare earth distilation device
CN110538478A (en) * 2018-10-29 2019-12-06 天津包钢稀土研究院有限责任公司 High-quality anhydrous rare earth halide purification device
CN111235398A (en) * 2020-03-13 2020-06-05 河南国玺超纯新材料股份有限公司 Distillation plant is used in high-purity zinc production
CN115522079A (en) * 2022-05-17 2022-12-27 鲍少聪 Recovery device for recovering rare earth metal from rare earth metal slag

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107937738A (en) * 2017-12-21 2018-04-20 李本根 A kind of new purifying plant for rare earth feed liquid
CN110538478A (en) * 2018-10-29 2019-12-06 天津包钢稀土研究院有限责任公司 High-quality anhydrous rare earth halide purification device
CN109517997A (en) * 2018-12-12 2019-03-26 湖南稀土金属材料研究院 A kind of rare earth distilation device
CN111235398A (en) * 2020-03-13 2020-06-05 河南国玺超纯新材料股份有限公司 Distillation plant is used in high-purity zinc production
CN115522079A (en) * 2022-05-17 2022-12-27 鲍少聪 Recovery device for recovering rare earth metal from rare earth metal slag

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Granted publication date: 20140611