CN108118167A - The purification devices of ultrapure rare earth metal and the method using its progress rare earth purifying - Google Patents
The purification devices of ultrapure rare earth metal and the method using its progress rare earth purifying Download PDFInfo
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- CN108118167A CN108118167A CN201810156643.3A CN201810156643A CN108118167A CN 108118167 A CN108118167 A CN 108118167A CN 201810156643 A CN201810156643 A CN 201810156643A CN 108118167 A CN108118167 A CN 108118167A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention discloses a kind of purification devices of ultrapure rare earth metal, and including furnace body, the bottom of furnace body is equipped with heating unit, and the furnace body further includes coldplate, gas vent, bottom feeding port and temperature control equipment；The present invention also provides the method that ultrapure rare earth purifying is carried out using the device, including crushing, heating and temperature-fall period；The device of the invention is simple in structure, it is easy to disassemble maintenance, temperature control controllable precise can carry out different Heating Zone Temperatures according to different rare earth oxides and control, so as to achieve the purpose that separating-purifying rare earth metal, the purification process of the present invention is simple, process is easily controllable, and the whole process cycle is short, environment friendly and pollution-free, the Purity of Rare Earth of preparation is high, can isolate and purify 13 kinds of different rare earth oxides simultaneously.The present invention is suitable for preparing ultrapure rare earth metal.
Description
Technical field
The invention belongs to new energy materials field, it is related to purification devices of a kind of ultrapure rare earth metal and dilute using its progress
The method of soil purifying.
Background technology
Rare earth metal is become with its active chemical property and good atom cosolvency can not in modern new material system
Or scarce important composition element.At present rare earth metal is used to be concentrated mainly on new energy materials body as the field of main raw material(s)
In system, such as：Rare earth hydrogen storage material, rare earth permanent-magnetic material and RE treatment steel etc..Rare earth metal, especially ultrapure simple substance rare earth
For metal as " miraculous cure " of metal material properties is improved by attention, development potentiality is huge.
The production technology of current ultrapure rare earth metal based on being electrolysed, the process inevitably generate substantial amounts of dust and
Toxic and harmful gas, and influenced be subject to electrolytic environments and equipment, producing to usually contain in simple substance rare earth metal largely has
Transition metal impurity and other rare earth element impurity make it easily cause properties of product unstable when being used as additive
Situation occur, and this kind of method can not large-scale industrial production.Rare earth oxide is passed through in firing in addition, also having
Coal, mountain grass are heated, and are melted its impurity, are finally left rare-earth products, however this method temperature is difficult to control, firing
Can not precise control of temperature and different rare earth oxide generation area, caused by Purity of Rare Earth it is not high, product quality is inferior, rare earth
The rate of recovery is low, the wasting of resources, and environmental pollution is serious.Therefore, such as how environmentally friendly, efficient production technology prepares low impurity, height
The simple substance rare earth metal of purity, become restrict rare earth metal manufacturing industry even rare earth new material industry an important factor for.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of purification devices of ultrapure rare earth metal, apparatus structure letter
It is single, it is easy to disassemble maintenance, temperature control controllable precise can carry out different Heating Zone Temperatures according to different rare earth oxides and control,
So as to achieve the purpose that separating-purifying rare earth metal.
It is yet another object of the present invention to provide a kind of method that rare earth purifying is carried out using above device, the party
Method is simple, and process is easily controllable, and the whole process cycle is short, environmental protection, and the Purity of Rare Earth of preparation is high, can isolate and purify 1-3 kinds simultaneously
Different rare earth oxides.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of purification devices of ultrapure rare earth metal, including furnace body, the bottom of furnace body is equipped with heating unit, and the furnace body also wraps
Include coldplate, gas vent, bottom feeding port and temperature control equipment；
Through hole is equipped with centered on the coldplate and coincide with the furnace body inner cavity and is set along the short transverse of furnace body, it is described
Coldplate be equipped with it is several can make metallic vapour by steam hole, the through hole has the collection box that can collect rare earth；Institute
It states furnace body inside wall and is equipped with wall surface heating chamber and wall surface waterway successively between coldplate and furnace body roof, the coldplate
Bottom surface is additionally provided with the coldplate waterway being connected with the wall surface waterway, and the side wall of the furnace body is in coldplate waterway
Place is respectively equipped with the water inlet pipe and outlet pipe being connected with wall surface waterway, and the water inlet pipe passes through pipeline via water pump and pond
It is connected, the outlet pipe is connected with pond by pipeline；
The temperature control equipment on furnace body inside wall and below coldplate including detecting lower steam temperature
First temperature sensor of degree and on furnace body inside wall and above the coldplate for detecting upper steam temperature
Temp sensor device；The furnace body lateral surface is equipped with what is be electrically connected respectively with the first temperature sensor and temp sensor device
Controller, the input panel for being electrically connected with the controller and being used to receiving the instruction of user's input temp and with the control
The display of device electrical connection, the controller are also electrically connected with the heating unit and are used to adjust the heating temperature of heating unit
Degree.
As a kind of restriction of apparatus of the present invention,
The coldplate is included along furnace body short transverse spaced the first horn-like graphite cake, the successively from the bottom to top
Two graphite cakes, the 3rd graphite cake.
As the further restriction of apparatus of the present invention,
The wall surface heating chamber includes being arranged on furnace body inside wall corresponding to the 3rd heating at the top of furnace body between the 3rd graphite cake
Chamber, arranged on furnace body inside wall corresponding between the 3rd graphite cake and the second graphite cake the second heating chamber and arranged on furnace body inside
Wall is corresponding to the first heating chamber between the second graphite cake and the first graphite cake；
The collection box include be arranged on the first graphite cake under the first collection box, the second collection box under the second graphite cake,
And the 3rd collection box under the 3rd graphite cake.
As the further restriction of apparatus of the present invention,
The wall surface waterway include be arranged on the 3rd heating chamber on the inside of the 3rd waterway, second on the inside of the second heating chamber
Waterway and the first waterway on the inside of the first heating chamber.
As the further restriction of apparatus of the present invention,
The temp sensor device includes the second temperature sensor being arranged on the first waterway, on the second waterway
Three-temperature sensor and the 4th temperature sensor on the 3rd waterway.
The present invention also provides the sides that the purification devices using any one above-mentioned ultrapure rare earth metal carry out rare earth purifying
Method carries out successively according to steps order：
（1）It crushes
Rare earth oxide is taken, with reducing metal simple substance according to 1-2.3 after being crushed:1 weight ratio is uniformly mixed, in 10-
15MPa lower lock blocks, obtain A；
（2）Heating
A is sent into the purification devices of ultrapure rare earth metal, is evacuated to vacuum degree 3Pa, heated at 800-1200 DEG C, keep the temperature 25h,
Obtain B；
In this step, the temperature of heating and soaking time be vital, when heating temperature is less than 800 DEG C, can cause most
Na, K, Cl in finished product-Wait impurity contents excessively high, when heating temperature is higher than 1200 DEG C, can drop makes beavy metal impurity in raw material
Being mingled in the product, reduces the product purity of B；
When soaking time is less than 25h, product collecting amount can be reduced, causes the wasting of resources, while make in product impurity phase to containing
Amount rise, reduces product quality；When soaking time is higher than 25h, unreacted reducing metal can be made to be transformed into steam rising, from
And be mixed into the metal-rare-earth of purifying, can settle cooling together with the rare earth of purifying during cooling is collected, and makes B purity
It reduces；
（3）Cooling
At a temperature of purified rare earth metal fusing point is 10-50 DEG C low, cool down to B, rare earth after purification is collected on coldplate.
As a kind of restriction of the method for the present invention, the rare earth oxide is Pr6O11、Nd2O3、Sm2O3、Eu2O3、Gd2O3、
Tb4O7、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3Or Lu2O3One or more of composition.
Another kind as the method for the present invention limits, and the reducing metal simple substance is in La, Ce, Y, Mg, Li and Na
It is a kind of.
As a result of above-mentioned technical solution, compared with prior art, the present invention acquired technological progress is：
A kind of purification devices of ultrapure rare earth metal provided by the invention, have the following advantages that：
1. the apparatus structure is simple, it is easy to disassemble maintenance；
2. temperature control controllable precise, interior the first graphite cake, the second graphite cake and the 3rd graphite cake set of furnace body divides furnace body inner cavity
Into four heating zones, can different Heating Zone Temperatures be carried out according to different rare earth oxides and controlled, the rare earth point of cooling-sedimentation
Layer is settled on the cooling plate, so as to achieve the purpose that separating-purifying rare earth metal；
3. settle horn-like structure of the rare earth metal on the cooling plate due to rare earth plate so that rare earth metal after purification is automatic
It comes together in collection box, dramatically saves manual time, while also avoid the dust pollution during collecting；
4. saving the energy, labour is saved, avoids the waste and pollution of rare earth；
A kind of method of rare earth purifying provided by the invention, step is simple, and process is easily controllable, and the whole process cycle is short, environmental protection
It is pollution-free, the different rare earth oxide of 1-3 kinds can be isolated and purified simultaneously, each rare earth metal purity after purification is high, industrialization
It is efficient.
The present invention is suitable for the preparation of ultrapure rare earth metal.
The present invention is described in further detail below in conjunction with specific embodiment.
Description of the drawings
Fig. 1 is the structure diagram of the embodiment of the present invention 1；
Fig. 2 is the structure diagram of the first graphite cake in Fig. 1；
In figure：1- furnace bodies, the first graphite cakes of 2-, the second graphite cakes of 3-, the 3rd graphite cakes of 4-, 5- gas vents, 6- water pumps, 7- water
Pond, 8- input panel, 9- controllers, 10- displays, 21- heating units, 22- feeding ports, the first temperature sensors of 23-, 24-
First collection box, 31- second temperature sensors, the second collection boxes of 32-, the first waterways of 33-, the first heating chambers of 34-, 41-
Three-temperature sensor, the 3rd collection boxes of 42-, the second waterways of 43-, the second heating chambers of 44-, the 4th temperature sensors of 51-, 52-
3rd waterway, the 3rd heating chambers of 53-.
Specific embodiment
Parts and device described in following embodiments are existing device unless otherwise specified, between each component
Control planning and connection relation be existing control planning and connection relation unless otherwise specified.
A kind of purification devices of ultrapure rare earth metal of embodiment 1
The present embodiment is a kind of purification devices of ultrapure rare earth metal, as shown in Figure 1, it includes furnace body 1, the top of furnace body 1 is set
There is gas vent 5, the lower part of furnace body 1 is equipped with the feeding port 22 that the rare earth oxide material purified will be needed to be sent into furnace body 1, stove
Heating unit 21, coldplate, temperature control equipment are additionally provided in body 1.
（One）Heating unit 21
Heating unit 21 is arranged on the bottom of furnace body 1, for the rare earth heating purified to needs, that is, needs the rare earth oxide purified
Be placed on the heating kettle of bottom, heating unit 21 is located under heating kettle, heating unit 21 by it is automatically controlled control its heating temperature and
Time.
（Two）Coldplate
Coldplate is set along the short transverse of furnace body 1, and coldplate matches with the inner wall of furnace body 1, i.e., it is fixed on furnace body 1
On inner wall, in order to which the rare earth steam that lower part is heated is enable to pass through coldplate, coldplate can make metallic vapour equipped with several
By steam hole；The center of coldplate is equipped with through hole, and through hole, which has, can collect cooling in the ultrapure rare earth gold on coldplate
The collection box of category.
In actual purification process, the rare earth oxide of mixing is mostly 2 kinds or 3 kinds different rare earth kind type oxides
Mixture, in order to simultaneously a variety of rare earth oxides are purified, coldplate be along 1 short transverse of furnace body from the bottom to top according to
The first graphite cake 2, the second graphite cake 3, the 3rd graphite cake 4 of minor tick setting, the first graphite cake 2, the second graphite cake the 3, the 3rd
The shape of graphite cake 4 is identical, their material is graphite cake, and thickness 3-5mm, they are horn-like structure, certainly
It can increase or reduce the number of coldplate according to the rare earth metal species isolated and purified simultaneously.As shown in Fig. 2, collection box is to set
The first collection box 24 being threadedly coupled with it under the first graphite cake 2, being threadedly coupled with it under the second graphite cake 3
Second collection box 32 and the 3rd collection box 42 being threadedly coupled with it under the 3rd graphite cake 4, the first graphite cake 2, second
Graphite cake 3, the 3rd graphite cake 4 be equipped with for metallic vapour by steam hole.
First graphite cake 2, the second graphite cake 3, the 3rd graphite cake 4 furnace body 1 is divided into successively from the bottom to top the first heating zone,
Second heating zone, the 3rd heating zone and the 4th heating zone, rare earth oxide and reducing metal on the heating kettle of 1 bottom of furnace body
Simple substance reacts after being heated, and rare earth metal, which is reduced, becomes rare earth simple substance, and is heated and becomes rare earth metal steam, and steam is upward
Sequentially pass through the first graphite cake 2, the second graphite cake 3, the 3rd graphite cake 4.
1 madial wall of furnace body is equipped with wall surface heating chamber and wall surface waterway successively between 1 roof of coldplate and furnace body, i.e.,：
Furnace body 1 corresponds to is equipped with wall surface heating chamber and wall surface waterway successively on the inner wall between 1 roof of the first graphite cake 2 and furnace body；
The bottom surface of coldplate is additionally provided with the coldplate waterway being connected with wall surface waterway, i.e.,：First graphite cake 2, the second graphite
Plate 3, the bottom surface of the 3rd graphite cake 4 are respectively provided with the coldplate waterway to cool down to it, and coldplate waterway is set
Have with steam hole site on coldplate it is corresponding can for bottom-heated metallic vapour by coldplate waterway through hole, stove
The side wall of body 1 is respectively equipped with the water inlet pipe and outlet pipe being connected with wall surface waterway, water inlet pipe warp at coldplate waterway
It is connected by water pump 6 with pond 7 by pipeline, outlet pipe is connected with pond 7 by pipeline, and heater strip is equipped in wall surface heating chamber,
Coldplate waterway and wall surface waterway are filled with the cooling water being pumped by water pump 6 from pond 7.
Wall surface heating chamber is included arranged on 1 madial wall of furnace body corresponding to the 3rd between 1 top of furnace body and the 3rd graphite cake 4
Heating chamber 53 corresponding to the second heating chamber 44 between the 3rd graphite cake 4 and the second graphite cake 3 and is set arranged on 1 madial wall of furnace body
In 1 madial wall of furnace body corresponding to the first heating chamber 34 between the second graphite cake 3 and the first graphite cake 2；3rd heating chamber 53,
Two heating chambers 44 and the first heating chamber 34 do not connect mutually, and respective control mode is individually control.
Wall surface waterway includes being arranged on 53 madial wall of the 3rd heating chamber（I.e. close to 1 central side of furnace body）The 3rd waterway
52nd, arranged on 44 madial wall of the second heating chamber（I.e. close to 1 central side of furnace body）The second waterway 43 and arranged on the first heating chamber 34
First waterway 33 of madial wall, the 3rd waterway 52, the second waterway 43 and the first waterway 33 do not connect mutually, the 3rd water cooling
Chamber 52, the second waterway 43 and the first waterway 33 respectively with the first graphite cake 2, the second graphite cake 3 and 4 following table of the 3rd graphite cake
The coldplate waterway that face is set is connected, since the material of the first graphite cake 2, the second graphite cake 3 and the 3rd graphite cake 4 is stone
During water cooling temperature moment on plate will not decline ink, ensure that the control of 1 different heating area temperature of furnace body.Stove
1 wall surface both sides of body are respectively at the first graphite cake 2, the respective coldplate waterway of the second graphite cake 3 and 4 lower surface of the 3rd graphite cake
Place is equipped with water inlet pipe and outlet pipe, ensures cooling water Efficient Cycle of knowing clearly, in order to rationally control in the flowmeter furnace body 1 of cooling water
The cooling temperature in different heating area, 1 wall surface of furnace body three at be respectively equipped with valve and flowmeter on water inlet pipe, cooling water is from water inlet
It is pumped at mouthful, is flowed out from water outlet pipe part at the three of 1 wall surface of furnace body, in pond 7 is back to, water cooling plant is equipped in pond 7, is used
In carrying out cooling processing to recirculated water.
（Three）Temperature control equipment
For the ease of the heating temperature to the first heating zone, the second heating zone, the 3rd heating zone and the 4th heating zone and cooling temperature
Degree is precisely controlled, and makes the Purity of Rare Earth higher of purification, and temperature control equipment includes being arranged on 1 madial wall of furnace body and positioned at cold
But the first temperature sensor 23 for being used to detect lower steam below plate that is, in the middle part of the first heating zone side wall and is arranged on
The temp sensor device for being used to detect upper steam temperature on 1 madial wall of furnace body and above coldplate.1 outside of furnace body
Face is electrically connected simultaneously equipped with the controller 9 being electrically connected respectively with the first temperature sensor 23 and temp sensor device, with controller 9
For receiving the input panel 8 of user's input temp instruction and the display 10 that is electrically connected with controller 9, controller 9 also with
The heating unit 21 of 1 bottom of furnace body is electrically connected and the heating temperature for adjusting heating unit 21.
In the present embodiment, temp sensor device include be arranged on the first waterway 33 on second temperature sensor 31,
Three-temperature sensor 41 on the second waterway 43 and the 4th temperature sensor 51 on the 3rd waterway 52.
In order to ensure temperature precise acquisition, second temperature sensor 31,41 and the 4th temperature sensor 51 of three-temperature sensor are set
In the middle part of the second heating chamber, the 3rd heating chamber and the 4th heating chamber interior sidewall surface, for gathering the temperature of the heating zone at place；The
Two temperature sensors 31,41 and the 4th temperature sensor 51 of three-temperature sensor are electrically connected respectively with controller 9.
When carrying out ultrapure rare earth metal purifying using the device of the present embodiment, by rare earth oxide mixture by feeding port 22
Send to 1 bottom-heated pot of furnace body, mouthfuls 5 at the gas at vacuumize, operating personnel according to the fusing point of the rare earth to be purified, in
The temperature of the first heating zone, the second heating zone, the 3rd heating zone and the 4th heating zone is set in input panel 8, controller 9 is connecing
After the instruction inputted, heating unit 21, heater strip in the first heating chamber 34, heater strip in the second heating chamber 44 are controlled respectively
And the 3rd heater strip in heating chamber 53 heated, temperature synchronization settings are a temperature, i.e.,：Ensure the whole temperature in furnace body 1
Degree is uniform, after target temperature to be achieved, after held for some time, opens valve and water at water inlet pipe at the three of 1 wall surface of furnace body
Pump 6, the first waterway 33, the second waterway 43 and the 3rd waterway 52 are interior full of recirculated cooling water, the second heating zone, the 3rd
Heating zone and the 4th heating zone start to cool down respectively, different according to the fusing point of the rare earth metal isolated and purified, by furnace body 1 it is outer into
Cooling temperature in the second heating zone of flowmeter adjusting control, the 3rd heating zone and the 4th heating zone set on water pipe passes through
Two temperature sensors 31,41 and the 4th temperature sensor of three-temperature sensor, 51 real-time collecting temperature and in display 10
It has been shown that, by controlling heating unit 21, heater strip in the first heating chamber 34, heater strip, the 3rd heating chamber in the second heating chamber 44
Flowmeter in 53 on heater strip and three water inlet pipes, controls respectively in the second heating zone, the 3rd heating zone and the 4th heating zone
Temperature, when cooling ensures the temperature of each heating zone less than institute's 10-50 DEG C of rare earth metal fusing point to be separated, and rare earth metal sinks
Drop is on the coldplate of the heating zone.In cooling, in order to make total energy approach, the second heating zone, the 3rd heating zone and the
Temperature gradient in four heating zones successively decreases, and the ultrapure of collection is settled on the first graphite cake 2, the second graphite cake 3 and the 3rd graphite cake 4
The fusing point of rare earth metal successively decreases for gradient, is deposited in ultrapure dilute on the first graphite cake 2, the second graphite cake 3 and the 3rd graphite cake 4
Earth metal is collected in respectively in the first collection box 24, the second collection box 32 and the 3rd collection box 42, and bottom is residue, i.e., cold
But corresponding cooling temperature is set according to the fusing point for the rare earth metal to be purified during, the during cooling
One graphite cake 2, the second graphite cake 3, the cooling temperature of the 3rd graphite cake 4 reduce successively, i.e.,：Purify three kinds of different rare-earth oxidations
Object, the high rare earth metal of fusing point be purified be collected in the first collection box 24, low-melting rare earth metal is purified and is collected in the
In three collection boxes 42, the rare earth metal that fusing point is in intermediate is collected in the second collection box 32.
The apparatus structure of the present embodiment is simple, is easy to disassemble maintenance, temperature control controllable precise can be according to different rare-earth oxidations
Object carries out different Heating Zone Temperature control, so as to achieve the purpose that separating-purifying rare earth metal.
A kind of purification devices of ultrapure rare earth metal of embodiment 2
The present embodiment is similar to Example 1, the difference is that only the first graphite cake 2, the second graphite cake 3 and the 3rd graphite cake
4th, the structure of the first collection box 24, the second collection box 32 and the 3rd collection box 42 is different, in the present embodiment, the first graphite cake 2,
The structure of second graphite cake 3 and the 3rd graphite cake 4 is identical, the first collection box 24, the second collection box 32 and the 3rd collection box 42
Structure is identical.
By taking the structure of the first graphite cake 2 as an example, the first graphite cake 2 is horn-like structure, and middle part is offered along its diameter side
To the straight slot of the strip of extension, straight slot extends downwardly, and the lower part outside wall surface of straight slot is equipped with the sliding slot extended along straight slot length direction,
Straight slot have be adapted with straight slot shape can be in the first collection box 24 slided on sliding slot.
The apparatus structure of the present embodiment is simple, is easy to disassemble maintenance, temperature control controllable precise can be according to different rare-earth oxidations
Object carries out different Heating Zone Temperature control, so as to achieve the purpose that separating-purifying rare earth metal.
A kind of purification process of ultrapure rare earth metal of embodiment 3
It is carried out using a kind of purification devices of ultrapure rare earth metal of above-described embodiment 1 or 2, purification process is according to the steps
Order carries out successively：
（31）It crushes
Take rare earth oxide Pr6O11、Nd2O3And Sm2O3, 100-200 mesh is crushed to, is mixed with reducing metal simple substance La
Uniformly, the weight ratio of rare earth oxide and reducing metal simple substance is 1:1, in 12MPa lower lock blocks, obtain A1；
（32）Heating
A1 is sent into the purification devices of ultrapure rare earth metal, is evacuated to vacuum degree 3Pa, heated at 1200 DEG C, kept the temperature 25h, obtain
B1；
（33）Cooling
At a temperature of purified rare earth metal fusing point is 10-50 DEG C low, cool down to B, i.e.,：According to the height of fusing point, fusing point is low
Rare earth metal collection is cooled down on uppermost 3rd graphite cake 4, the high rare earth metal of fusing point is in nethermost first graphite
It cools down and collects on plate 2, what is collected on the 3rd graphite cake 4 is rare earth metal praseodymium；What is collected on second graphite cake 3 is rare earth metal
Neodymium, what is collected on the first graphite cake is rare earth metal samarium, and three kinds of rare earth metals of collection emit light by inductively coupled plasma
Spectrum analysis learns that the purity of three kinds of rare earth metals of purifying is respectively greater than 99.9999%.
The purification process of the ultrapure rare earth metals of embodiment 4-8
It is respectively a kind of method of rare earth purifying in embodiment 4-8, step is similar to Example 3, the difference is that only：Separation
Metal, reducing metal, the pressure of briquetting and the temperature of heating of purifying are different, specific as follows：
4 rare earth oxide of embodiment is Tm2O3、Yb2O3Or Lu2O3, reducing metal Ce, rare earth oxide and reducing metal list
The weight ratio of matter is 2:1, briquetting pressure 10MPa, the temperature of heating is 800 DEG C；
5 rare earth oxide of embodiment is Eu2O3、Gd2O3、Tb4O7, reducing metal Y, rare earth oxide and reducing metal simple substance
Weight ratio be 1.5:1, briquetting pressure 15MPa, the temperature of heating is 1000 DEG C；
6 rare earth oxide of embodiment is Eu2O3、Gd2O3、Tb4O7, reducing metal Mg, rare earth oxide and reducing metal simple substance
Weight ratio be 2.3:1, briquetting pressure 14MPa, the temperature of heating is 1000 DEG C；
7 rare earth oxide Dy of embodiment2O3、Ho2O3、Er2O3,Reducing metal Li, rare earth oxide and reducing metal simple substance
Weight ratio is 1.3:1, briquetting pressure 12MPa, the temperature of heating is 1200 DEG C；
8 rare earth oxide Sm of embodiment2O3,Reducing metal Na, briquetting pressure 11MPa, the temperature of heating is 1100 DEG C.
Purified rare earth metal in embodiment 4-8, is collected in respectively in different collection boxes, by inductive coupling etc.
Ion emission spectroscopy analysis learns that the purity of each metal after purification is all higher than 99.9999%
Influence of the temperature that cools down in the purification process of 9 ultrapure rare earth metal of embodiment to final rare earth purification effect
During rare earth purifies, it is necessary to cool down to different heating zones after heat preservation so that the rare earth of different melting points
Metal is enriched on the coldplate in the area, and during cooling, the temperature control of heating zone is vital, and different is cold
But temperature directly with finally the purity of rare earth is related after purification, it is specific as follows.In following researchs, the purification process and reality of rare earth
It is similar to apply example 3, the difference is that only：The temperature of cooling is different.
A groups：The cooling temperature that this group is provided at a temperature of purified rare earth fusing point is 10-50 DEG C low, cools down
Cooling, i.e., the temperature that embodiment 1 is provided；
B groups：At a temperature of purified rare earth fusing point is 3-9 DEG C low, cooling down is carried out；
C groups：At a temperature of purified rare earth fusing point is 51-80 DEG C low, cooling down is carried out；
D groups：At a temperature of purified rare earth fusing point is 100 DEG C low, cooling down is carried out；
The results show that the purity of three kinds of metals of A groups is more than 99.9999%, and 0.3% metal is mixed in B group rare earth Nds
The metal Pr of Sm and 0.5%；The metal Nd of 0.4% metal Sm and 0.2% is mixed in C group rare earths Pr；It is mixed in D group rare earths Pr
There is the metal Nd of 1.1% metal Sm and 0.4%；
It can thus be seen that although the cooling temperature of A-D groups is below the rare earth metal fusing point of purifying, different drops
Temperature significantly impacts the purity of final rare earth after purification, and this is mainly due to rare earth metal fusing point to be separated and volatility
Matter approaches, and when cooling temperature is higher, low-melting-point metal steam easily diffuses to other collecting zones, causes collected metal
Purity reduces；And when cooling temperature is too low, it is condensed on the coldplate that volatile metallic vapour is easily trapped in diffusion path,
And then result in this phenomenon.
Embodiment 1-8 is only presently preferred embodiments of the present invention, is not the limit of other forms made for the present invention
Fixed, any person skilled in the art is changed or is modified as equivalent change possibly also with above-mentioned technology contents as enlightenment
The equivalent embodiment of change.In every case it is the technical spirit without departing from the claims in the present invention, to simple made by above example
Modification, equivalent variations and remodeling still fall within the scope of the claims in the present invention protection.
Claims (9)
1. a kind of purification devices of ultrapure rare earth metal, including furnace body（1）, the furnace body（1）Bottom is equipped with heating unit（21）,
It is characterized in that：The furnace body（1）Further include coldplate, gas vent（5）, bottom feeding port（22）And temperature control equipment；
Centered on the coldplate be equipped with through hole and with the furnace body（1）Inner cavity coincide and along furnace body（1）Short transverse set
Put, the coldplate be equipped with it is several can make metallic vapour by steam hole, the through hole has the receipts that can collect rare earth
Collect box；The furnace body（1）Madial wall is in coldplate and furnace body（1）Wall surface heating chamber and wall surface water cooling are equipped between roof successively
Chamber, the bottom surface of the coldplate are additionally provided with the coldplate waterway being connected with the wall surface waterway, the furnace body（1）'s
Side wall is respectively equipped with the water inlet pipe and outlet pipe being connected with wall surface waterway at coldplate waterway, the water inlet pipe via
Water pump（6）With pond（7）It is connected by pipeline, the outlet pipe and pond（7）It is connected by pipeline；
The temperature control equipment includes being arranged on furnace body（1）On madial wall and below the coldplate for detecting lower steam
First temperature sensor of temperature（23）And arranged on furnace body（1）On madial wall and above the coldplate for detecting top
The temp sensor device of vapor (steam) temperature；The furnace body（1）Lateral surface be equipped with respectively with the first temperature sensor（23）And temperature
The controller of sensor device electrical connection（9）And the controller（9）It is electrically connected and is used to receive the instruction of user's input temp
Input panel（8）And with the controller（9）The display of electrical connection（10）, the controller（9）Also filled with the heating
It puts（21）It is electrically connected and is used to adjust heating unit（21）Heating temperature.
2. the purification devices of ultrapure rare earth metal according to claim 1, it is characterised in that：The coldplate include along
Furnace body（1）Short transverse spaced the first horn-like graphite cake successively from the bottom to top（2）, the second graphite cake（3）, the 3rd
Graphite cake（4）.
3. the purification devices of ultrapure rare earth metal according to claim 2, it is characterised in that：The wall surface heating chamber includes
Arranged on furnace body（1）Madial wall corresponds to furnace body（1）Top and the 3rd graphite cake（4）Between the 3rd heating chamber（53）, arranged on stove
Body（1）Madial wall corresponds to the 3rd graphite cake（4）With the second graphite cake（3）Between the second heating chamber（44）And arranged on furnace body
（1）Madial wall corresponds to the second graphite cake（3）With the first graphite cake（2）Between the first heating chamber（34）.
4. the purification devices of ultrapure rare earth metal according to claim 3, it is characterised in that：The wall surface waterway includes
Arranged on the 3rd heating chamber（53）3rd waterway of madial wall（52）, arranged on the second heating chamber（44）Second waterway of madial wall
（43）And arranged on the first heating chamber（34）First waterway of madial wall（33）.
5. the purification devices of ultrapure rare earth metal according to claim 4, it is characterised in that：The temp sensor device
Including being arranged on the first waterway（33）On second temperature sensor（31）, arranged on the second waterway（43）On the 3rd temperature pass
Sensor（41）And arranged on the 3rd waterway（52）On the 4th temperature sensor（51）.
6. the purification devices of ultrapure rare earth metal according to claim 2, it is characterised in that：The collection box includes being arranged on
First graphite cake（2）Under the first collection box（24）, arranged on the second graphite cake（3）Under the second collection box（32）And arranged on
Three graphite cakes（4）Under the 3rd collection box（42）.
7. a kind of purification devices using ultrapure rare earth metal as described in any one in claim 1-6 carry out rare earth purifying
Method, it is characterised in that carried out successively according to steps order：
（1）It crushes
Rare earth oxide is taken, with reducing metal simple substance according to 1-2.3 after being crushed:1 weight ratio is uniformly mixed, in 10-
15MPa lower lock blocks, obtain A；
（2）Heating
A is sent into the purification devices of ultrapure rare earth metal, is evacuated to vacuum degree 3Pa, heated at 800-1200 DEG C, keep the temperature 25h,
Obtain B；
（3）Cooling
At a temperature of purified rare earth fusing point is 10-50 DEG C low, cool down to B, rare earth after purification is collected on coldplate.
8. the method for rare earth purifying according to claim 7, it is characterised in that：The rare earth oxide is Pr6O11、
Nd2O3、Sm2O3、Eu2O3、Gd2O3、Tb4O7、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3Or Lu2O3One or more of group
Into.
9. the method for the rare earth purifying according to claim 7 or 8, it is characterised in that：The reducing metal simple substance for La,
One kind in Ce, Y, Mg, Li and Na.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604667A (en) * | 2021-07-26 | 2021-11-05 | 重庆赛迪热工环保工程技术有限公司 | Multi-metal vapor vacuum step condensation method and system |
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2018
- 2018-02-24 CN CN201810156643.3A patent/CN108118167A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604667A (en) * | 2021-07-26 | 2021-11-05 | 重庆赛迪热工环保工程技术有限公司 | Multi-metal vapor vacuum step condensation method and system |
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Inventor after: Zhao Xin Inventor after: Liu Yongqing Inventor after: Ke Dan Dan Inventor after: Tong Zhiyong Inventor after: Luo Qiwen Inventor after: He Tao Inventor before: Zhao Xin Inventor before: Liu Yongqing Inventor before: Ke Dan Dan Inventor before: Liu Yubao Inventor before: Tong Zhiyong Inventor before: Luo Qiwen Inventor before: He Tao |
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Application publication date: 20180605 |