CN107513730A - The continuous device and method for preparing tungsten powder and cobalt powder - Google Patents
The continuous device and method for preparing tungsten powder and cobalt powder Download PDFInfo
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- CN107513730A CN107513730A CN201710772262.3A CN201710772262A CN107513730A CN 107513730 A CN107513730 A CN 107513730A CN 201710772262 A CN201710772262 A CN 201710772262A CN 107513730 A CN107513730 A CN 107513730A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/04—Electrolytic production, recovery or refining of metal powders or porous metal masses from melts
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
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Abstract
The present invention relates to electrochemical technology field, there is provided a kind of continuous device and method for preparing tungsten powder and cobalt powder, the device include storage compartment, reative cell, reaction member, dosage unit, driver element, the first power supply and second source；The both ends of reaction member are respectively equipped with the first graphite cuvette and the second graphite cuvette；Suspension has first anode basket and second plate basket respectively in first graphite cuvette and the second graphite cuvette, the both ends of the bottom of first graphite cuvette offer the first collection pit and the second collection pit respectively, and the both ends of the bottom of the second graphite cuvette offer the 3rd collection pit and the 4th collection pit respectively；First power supply and second source are respectively arranged on the both sides of reative cell；Driver element is used to drive reaction member to rotate by the center of circle of its center.Application way of the present invention not only can continuously obtain cobalt in the first collection pit and the 4th collection pit, tungsten is obtained in the second collection pit and the 3rd collection pit, but also significantly improve the rate of recovery and separative efficiency, avoid electrode conversion.
Description
Technical field
The present invention relates to electrochemical technology field, more particularly to a kind of continuous device and side for preparing tungsten powder and cobalt powder
Method.
Background technology
Refractory metals tungsten and rare metal cobalt are particularly important strategic elements generally acknowledged in the world, to improving country's warp
Ji, military competition power have very important influence.Worldwide the tungsten resource with extraction value is very limited, but tungsten
The usage amount of resource is but increasing year by year, so as to further cause the shortage of tungsten resource.In addition, China's cobalt resource also pole
For shortage, a large amount of imports are leaned on to maintain to need every year, these have all largely threatened holding for Cemented Carbide Industry
Supervention exhibition.Hard alloy be by refractory metals tungsten carbide and binding metal through powder metallurgy process made of have it is high hard
Degree, the material of high-flexural strength, it is obtained in fields such as machine-building, mining, communications and transportation, energy exploration, building decorations
To being widely applied.At present, tungsten resource of the whole world more than 50% is used to manufacture hard alloy, and the tungsten in hard alloy scraps contains
Amount has just reached 74%~91%.Therefore, recovery hard alloy scraps are recovery tungsten, a kind of very effective approach of cobalt.
The method of existing recovery hard alloy scraps mainly has mechanical crushing method, zinc to melt method, electrochemical process, redox
Method, acid leaching process.However, mechanical crushing method is low with the organic efficiency of the molten method of zinc, and easily bring some impurity elements into；Electrification
Method, oxidation-reduction method can not be reclaimed continuously, and organic efficiency is relatively low；Acid leaching process can produce some waste gas such as SO2、
NO2。
The content of the invention
The present invention is to solve tungsten, the rate of recovery of cobalt are low in the prior art, the technical problem that can not continuously reclaim.
To solve the above problems, the invention provides a kind of continuous device for preparing tungsten powder and cobalt powder, the device includes：
Storage compartment, the storage compartment are provided with the first vacuum orifice and the charging aperture and discharging opening that can open and close；
Reative cell, the reative cell are located at the lower section of the storage compartment, and the reative cell is provided with the second vacuum orifice, air inlet
Mouth, gas outlet and heater；
Reaction member, for the reaction member in the reative cell, the both ends of the reaction member are respectively equipped with first
Graphite cuvette and the second graphite cuvette；Suspension has first anode basket and second respectively in first graphite cuvette and second graphite cuvette
The top of anode basket, the first anode basket and the second plate basket is respectively connected with anode conducting post；First graphite cuvette
The both ends of bottom offer the first collection pit and the second collection pit respectively, the both ends of the bottom of second graphite cuvette are opened respectively
Provided with the 3rd collection pit and the 4th collection pit, first collection pit, second collection pit, the 3rd collection pit and described
The bottom of 4th collection pit is inserted with negative electrode conductive pole；The first anode basket is received with the second plate basket, described first
Ji Keng is with the 4th collection pit and second collection pit with the 3rd collection pit on the reaction member center
Symmetrically；
Dosage unit, the import of the dosage unit are located at the first anode located at the lower section of the discharging opening, outlet
The top of circumference where basket and the second plate basket；
First power supply and second source, first power supply and the second source are respectively arranged on the two of the reative cell
The positive pole of side, first power supply and the second source is connected with the first sheet metal, first sheet metal by wire
On the circumference where the top of the anode conducting post；The negative pole of first power supply and the second source is by leading
Line is connected with the second sheet metal, and second sheet metal is on the circumference where the bottom of the negative electrode conductive pole；And
Driver element, the driver element be used for drive the reaction member using its center be the center of circle rotate, so that each
First sheet metal and second sheet metal are electrically connected with the corresponding anode conducting post and the negative electrode conductive pole respectively
Connect.
Wherein, it is covered with the first corundum plate for suspending the first anode basket on first graphite cuvette, described
The second corundum plate for suspending the second plate basket is covered with two graphite cuvettes.
Wherein, the first siphon port is offered on the first corundum plate and the second corundum plate, on the reative cell
Offer the second siphon port for closing on first siphon port.
Wherein, the reaction member include be embedded with the first corundum plate and the second corundum plate upper groove body and
Lower groove provided with first graphite cuvette and second graphite cuvette.
Wherein, corundum is filled between the lower groove and first graphite cuvette and second graphite cuvette.
Wherein, the import of the dosage unit is in infundibulate, and the size of the import is more than the size of the discharging opening.
Wherein, first collection pit, second collection pit, the 3rd collection pit and the 4th collection pit difference
With the corresponding pluggable connection of negative electrode conductive pole.
Wherein, the negative electrode conductive pole includes nickel rod and the corundum set being arranged on the nickel rod.
Wherein, the driver element include be plugged in the reaction member bottom centre drive link and with the transmission
The motor of bar electrical connection.
To solve the above problems, present invention also offers a kind of continuous method for preparing tungsten powder and cobalt powder, this method includes
Following steps：
S1, material is added into storage compartment by charging aperture, and redirect and perform step S2；Wherein, the material includes zinc
Grain, hard alloy scraps and NaF-KF fused salts；
S2, charging aperture is closed, storage compartment is vacuumized by the first vacuum orifice, until the pressure in storage compartment reaches the
One specified pressure, and redirect and perform step S3；
S3, discharging opening is opened to first anode basket addition material, after the first specified time, close discharging opening, and jump
Turn to perform step S4；
S4, driving reaction member rotate 180 °, and redirect and perform step S5；
S5, discharging opening is opened to second plate basket addition material, after the first specified time, close discharging opening, and jump
Turn to perform step S6；
S6, by the second vacuum orifice reative cell is vacuumized, until the pressure in reative cell reaches the second specified pressure,
Start heater simultaneously, until reaction indoor temperature reaches the first assigned temperature, and redirect and perform step S7；
S7, inert gas is passed through to reative cell by air inlet, until the pressure in reative cell reaches the 3rd specified pressure
Afterwards, gas outlet is opened, and starts heater, until the temperature in reative cell reaches the second assigned temperature, and redirects execution step
S8；
S8, start the first power supply to first anode basket and the first collection pit application 0.6V voltages, while start second source
2V voltages are applied to second plate basket and the 3rd collection pit, and redirects and performs step S9；
S9, after the second specified time, driving reaction member rotates 180 ° so that the first power supply to second plate basket and
4th collection pit applies 0.6V voltages, second source applies 2V voltages to first anode basket and the second collection pit, and redirects execution
Step S10；
S10, after the second specified time, driving reaction member rotates 180 °, and redirects and perform step S8.
The present invention utilizes first anode basket and second plate basket, the first collection pit and the 4th collection pit and the second collection pit
The characteristics of with the 3rd collection pit on reaction member Central Symmetry, drive reaction member to rotate by driver element, make reaction
When unit rotational is to specified location, the first power supply applies 0.6V voltages, second source applies 2V voltages, so that the first power supply, the
One anode basket and the first collection pit collectively form an electrolysis loop, while collect second source, second plate basket and the 3rd
Hole collectively forms another electrolysis loop；After reaction member is rotated further 180 °, a power supply, second plate basket and can be made again
Four collection pits collectively form an electrolysis loop, while second source, first anode basket and the second collection pit is collectively formed separately
One electrolysis loop, so as to different with the precipitation coefficient of cobalt using tungsten, so that it may continuously in the first collection pit and the 4th collection pit
Obtain cobalt, obtain tungsten in the second collection pit and the 3rd collection pit, so as to not only significantly improve the rate of recovery and separative efficiency, and
And electrode conversion is also avoid, extend the service life of the device.
Brief description of the drawings
Fig. 1 is a kind of structural representation of the continuous device for preparing tungsten powder and cobalt powder in the embodiment of the present invention 1；
Fig. 2 is the structural representation of reaction member in the embodiment of the present invention 1；
Fig. 3 is the structural representation of negative electrode conductive pole in the embodiment of the present invention 1；
Fig. 4 is the structural representation of lower groove in the embodiment of the present invention 1；
Fig. 5 is the structural representation of upper groove body in the embodiment of the present invention 1；
Fig. 6 is the XRD of the cobalt powder and tungsten powder prepared in the embodiment of the present invention 2, wherein, Fig. 6 (a) is the XRD of cobalt powder；
6 (b) is the XRD of tungsten powder；
Fig. 7 is the SEM figures of the cobalt powder and tungsten powder prepared in the embodiment of the present invention 2, wherein, Fig. 7 (a) is that the SEM of cobalt powder schemes；
7 (b) is that the SEM of tungsten powder schemes.
Reference：
1st, storage compartment；1-1, the first vacuum orifice；2nd, reative cell；2-1, air inlet；
2-2, gas outlet；2-3, the second vacuum orifice；2-4, the second siphon port；
3rd, dosage unit；4th, reaction member；4-1, upper groove body；4-11, the first corundum plate；
4-12, the second corundum plate；4-13, the first siphon port；4-2, lower groove；
4-21, the first graphite cuvette；4-211, the first collection pit；4-212, the second collection pit；
4-22, the second graphite cuvette；4-221, the 3rd collection pit；4-222, the 4th collection pit；
4-23, corundum；4-3, first anode basket；4-4, second plate basket；
4-5, anode conducting post；4-6, negative electrode mounting hole；4-71, nickel rod；
4-72, corundum set；5th, the first sheet metal；6th, the second sheet metal；7th, drive link.
Embodiment
To make the purpose, technical scheme and advantage of invention clearer, below in conjunction with the accompanying drawing in invention, in invention
Technical scheme be explicitly described, it is clear that described embodiment is invention part of the embodiment, rather than whole realities
Apply example.Based on the embodiment in invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belong to the scope of invention protection.
In the description of the invention, unless otherwise indicated, the orientation or position of the instruction such as term " on ", " under ", " top ", " bottom "
It is based on orientation shown in the drawings or position relationship to put relation, is for only for ease of the description present invention and simplifies description, rather than
Indicate or imply that signified device or element there must be specific orientation, with specific azimuth configuration and operation, therefore can not
It is interpreted as limitation of the present invention.
It should be noted that unless otherwise clearly defined and limited, term " connection " should be interpreted broadly, for example, can
To be to be fixedly connected or be detachably connected, or it is integrally connected；Can be joined directly together, middle matchmaker can also be passed through
Jie is indirectly connected.For the ordinary skill in the art, tool of the above-mentioned term in invention can be understood with concrete condition
Body implication.
Embodiment 1
With reference to shown in Fig. 1 to Fig. 5, the invention provides a kind of continuous device for preparing tungsten powder and cobalt powder, the device includes：
Storage compartment 1, the side wall of storage compartment 1 is provided with the first vacuum orifice 1-1, top and bottom offer respectively to open and close
Charging aperture and discharging opening；
Reative cell 2, reative cell 2 are located at the lower section of storage compartment 1, and reative cell 2 is provided with the second vacuum orifice 2-3, air inlet 2-
1st, gas outlet 2-2 and heater；Wherein, air inlet 2-1 and gas outlet 2-2 is separately positioned on the both sides of reative cell 2, and air inlet
2-1 is located at gas outlet 2-2 top；Heater is preferably the heater strip for the outer wall for being wrapped in reative cell 2.
Reaction member 4, for reaction member 4 in reative cell 2, the both ends of reaction member 4 are respectively equipped with the first graphite cuvette 4-
The 21 and second graphite cuvette 4-22；In first graphite cuvette 4-21 and the second graphite cuvette 4-22 respectively suspension have first anode basket 4-3 and
Second plate basket 4-4, first anode basket 4-3 and second plate basket 4-4 top are respectively connected with anode conducting post 4-5；First stone
The both ends of ink tank 4-21 bottom offer the first collection pit 4-211 and the second collection pit 4-212, the second graphite cuvette 4-22 respectively
The both ends of bottom offer the 3rd collection pit 4-221 and the 4th collection pit 4-222 respectively, the first collection pit 4-211, second are received
Collection hole 4-212, the 3rd collection pit 4-221 and the 4th collection pit 4-222 bottom are inserted with negative electrode conductive pole；First anode basket
4-3 and second plate basket 4-4, the first collection pit 4-211 and the 4th collection pit 4-222 and the second collection pit 4-212 and the 3rd
Collection pit 4-221 is on the Central Symmetry of reaction member 4；
Dosage unit 3, the import of dosage unit 3 are located at first anode basket 4-3 and second located at the lower section of discharging opening, outlet
The top of circumference where anode basket 4-4；
First power supply and second source, the first power supply and second source are respectively arranged on the both sides of reative cell 2, the first power supply and
The positive pole of second source is connected with the first sheet metal 5 by wire, and the first sheet metal 5 is located at anode conducting post 4-5 top
On the circumference at place；The negative pole of first power supply and second source is connected with the second sheet metal 6, the second sheet metal 6 by wire
On the circumference where the bottom of negative electrode conductive pole；And
Driver element, driver element are used to drive reaction member 4 to rotate, so that each first metal by the center of circle of its center
The sheet metal 6 of piece 5 and second electrically connects with corresponding anode conducting post 4-5 and negative electrode conductive pole respectively, that is to say, that when reaction is single
Member 4 is when turning to specified location, the anode on the first sheet metal 5 and first anode basket 4-3 be connected with the positive pole of the first power supply
Conductive pole 4-5 contacts, the second sheet metal 6 being connected with the negative pole of the first power supply and the moon being plugged on the first collection pit 4-211
Pole conductive pole contact, i.e. the first power supply, first anode basket 4-3 and the first collection pit 4-211 collectively form an electrolysis loop；With
This simultaneously, the first sheet metal 5 connected with the positive pole of second source contacts with the anode conducting post 4-5 on second plate basket 4-4,
The second sheet metal 6 connected with the negative pole of second source contacts with the negative electrode conductive pole being plugged on the 3rd collection pit 4-221, i.e.,
Second source, second plate basket 4-4 and the 3rd collection pit 4-221 collectively form another electrolysis loop.And when reaction member 4 after
Continue after rotating 180, the anode conducting post 4-5 on the first sheet metal 5 and second plate basket 4-4 being connected with the positive pole of the first power supply
Contact, the second sheet metal 6 being connected with the negative pole of the first power supply connect with the negative electrode conductive pole being plugged on the 4th collection pit 4-222
Touch, i.e. the first power supply, second plate basket 4-4 and the 4th collection pit 4-222 collectively form an electrolysis loop；At the same time, with
First sheet metal 5 of the positive pole connection of second source is contacted with the anode conducting post 4-5 on first anode basket 4-3 and the second electricity
Second sheet metal 6 of the negative pole connection in source contacts with the negative electrode conductive pole being plugged on the second collection pit 4-212, i.e., the second electricity
Source, first anode basket 4-3 and the second collection pit 4-212 collectively form another electrolysis loop.
Specifically, during use：
First, material, i.e. zinc granule, hard alloy scraps and NaF-KF fused salts are put into storage compartment 1；
Secondly, after being vacuumized by the first vacuum orifice 1-1 to storage compartment 1, discharging opening is opened, material can pass through charging
Unit 3 is fallen directly in first anode basket 4-3；
Then, driver element is started, so that reaction member 4 rotates 180 °, the now outlet of dosage unit 3 is located exactly at the
Two anode basket 4-4 top, after being again turned on discharging opening, material can fall directly on second plate by dosage unit 3
In basket 4-4；
Then, reative cell 2 is vacuumized by the second vacuum orifice 2-3, while starts heater, until in reative cell 2
After temperature reaches 300 DEG C, argon gas is filled with into reative cell 2 by air inlet 2-1, when the pressure in reative cell 2 reaches 105Pa
Afterwards, gas outlet 2-2 is opened, while is again started up heater, until the temperature in reative cell 2 reaches 750 DEG C, is now contained in the
One anode basket 4-3 and NaF-KF fused salts in second plate basket 4-4 and zinc granule are completely melt that NaF-KF fused salts just flow into the first stone
In ink tank 4-21 and the second graphite cuvette 4-22, because the density of zinc is larger, therefore liquid Zn can be deposited on the first collection pit 4-
211st, in the second collection pit 4-212, the 3rd collection pit 4-221 and the 4th collection pit 4-222；
Next, applying 0.6V voltages by the first power supply, while 2V voltages are applied by second source.Now, with
First sheet metal 5 of the positive pole connection of one power supply contact with the anode conducting post 4-5 on first anode basket 4-3 just, and first
Second sheet metal 6 of the negative pole connection of power supply contacts with the negative electrode conductive pole being plugged on the first collection pit 4-211, i.e., the first electricity
Source, first anode basket 4-3 and the first collection pit 4-211 collectively form an electrolysis loop；And it is connected with the positive pole of second source
The first sheet metal 5 contact, be connected with the negative pole of second source with the anode conducting post 4-5 on second plate basket 4-4 second
Sheet metal 6 contacts with the negative electrode conductive pole being plugged on the 3rd collection pit 4-221, i.e. second source, second plate basket 4-4 and
Three collection pit 4-221 collectively form another electrolysis loop.Because tungsten is different with the deposition potential of cobalt, i.e., when applied voltage is small
When 0.8V, cobalt is easy to separate out, and when applied voltage is more than 0.8V, tungsten is easy to separate out.Therefore, in first anode basket 4-3
After hard alloy scraps are gradually ionized in NaF-KF fused salts, cobalt ions can be reduced into simple substance, be deposited on the first collection pit
In 4-211, and after the hard alloy scraps in second plate basket 4-4 are gradually ionized in NaF-KF fused salts, tungsten ion can quilt
Simple substance is reduced into, is deposited in the 3rd collection pit 4-221；
Finally, after 1 hour, starting driver element makes reaction member 4 rotate 180 °.Due to the first collection pit 4-211
With the 4th collection pit 4-222 and the second collection pit 4-212 and the 3rd collection pit 4-221 on the Central Symmetry of reaction member 4,
Therefore after reaction member 4 rotates 180 °, on the first sheet metal 5 and second plate basket 4-4 that be connecteds with the positive pole of the first power supply
Anode conducting post 4-5 contacts, the second sheet metal 6 being connected with the negative pole of the first power supply are with being plugged on the 4th collection pit 4-222
Negative electrode conductive pole contact, i.e. the first power supply, second plate basket 4-4 and the 4th collection pit 4-222 collectively form one and are electrolysed back
Road；And contacted with the first sheet metal 5 that the positive pole of second source connects with the anode conducting post 4-5 on first anode basket 4-3 and
Second sheet metal 6 of the negative pole connection of second source contacts with the negative electrode conductive pole being plugged on the second collection pit 4-212, i.e., and the
Two power supplys, first anode basket 4-3 and the second collection pit 4-212 collectively form another electrolysis loop.So as to second plate basket 4-4
In hard alloy scraps be gradually ionized in NaF-KF fused salts after, cobalt ions can be reduced into simple substance, be deposited on the 4th receipts
In the 4-222 of collection hole, and after the hard alloy scraps in first anode basket 4-3 are gradually ionized in NaF-KF fused salts, tungsten ion
Simple substance can be reduced into, is deposited in the second collection pit 4-212.
Thus, every 1 hour, primary first-order equation unit 4 is rotated, cobalt will be received constantly in the first collection pit 4-211 and the 4th
Deposited in the 4-222 of collection hole, at the same time, tungsten can be deposited constantly in the second collection pit 4-212 and the 3rd collection pit 4-221.By
It is different from the density of tungsten and cobalt in zinc, therefore after the completion of preparing, directly can suction out liquid Zn, and then just can obtain pure tungsten and pure
Cobalt.
Preferably, the first corundum plate 4-11 for suspending first anode basket 4-3 is covered with the first graphite cuvette 4-21, the
The second corundum plate 4-12 for suspending second plate basket 4-4, specifically, the first corundum plate 4- are covered with two graphite cuvette 4-22
11 middle part offers the first mounting hole, and the first stone is stretched into first anode basket 4-3 top with the first mounting hole clamping, the second end
In ink tank 4-21；The second mounting hole, second plate basket 4-4 top and the second installation are offered in the middle part of second corundum plate 4-12
The second graphite cuvette 4-22 is stretched into hole clamping, the second end.
Further, the first siphon port 4-13 is offered on the first corundum plate 4-11 and the second corundum plate 4-12, reacted
The the second siphon port 2-4 for closing on the first siphon port 4-13 is offered on room 2.Thus, after the completion of preparation, led to using siphoning installation
Cross the second siphon port 2-4 and corresponding first siphon port 4-13, so that it may by the first collection pit 4-211, the second collection pit 4-212,
Liquid Zn in 3rd collection pit 4-221 or the 4th collection pit 4-222 suctions out, and then just can obtain pure tungsten and pure cobalt.
Preferably, reaction member 4 include being embedded with the first corundum plate 4-11 and the second corundum plate 4-12 upper groove body 4-1 with
And the lower groove 4-2 provided with the first graphite cuvette 4-21 and the second graphite cuvette 4-22.It is highly preferred that upper groove body 4-1 and lower groove 4-2
It is detachably connected, for example, upper groove body 4-1 is connected with lower groove 4-2 by pin.
Further, corundum 4- is filled between lower groove 4-2 and the first graphite cuvette 4-21 and the second graphite cuvette 4-22
23。
Preferably, the import of dosage unit 3 is in infundibulate, and the size of import be more than discharging opening size, with ensure from
The material that discharging opening is fallen is fully entered in dosage unit 3.
Further, since negative electrode conductive pole easily corrodes, update and replace for the ease of the later stage, the first collection pit 4-211, second
Collection pit 4-212, the 3rd collection pit 4-221 and the 4th collection pit 4-222 respectively with the corresponding pluggable connection of negative electrode conductive pole.
Specifically, the first collection pit 4-211, the second collection pit 4-212, the 3rd collection pit 4-221 and the 4th collection pit 4-222 bottom
Center offer negative electrode mounting hole 4-6 for plugging negative electrode conductive pole.Wherein, negative electrode conductive pole include nickel rod 4-71 and
The corundum 4-23 sets being arranged on nickel rod 4-71.
Wherein, driver element includes being plugged in the drive link 7 of the bottom centre of reaction member 4 and electrically connected with drive link 7
Motor, i.e. one end of drive link 7 is plugged in center, the other end and the motor connection of the bottom of reaction member 4.Thus, electricity is worked as
While machine driving drive link 7 rotates, reaction member 4 can rotate therewith under the drive of drive link 7.
Preferably, first anode basket 4-3 and second plate basket 4-4 forms by platinum filament braiding.
Embodiment 2
Based on the above-mentioned continuous device for preparing tungsten powder and cobalt powder, present invention also offers one kind continuously to prepare tungsten powder and cobalt powder
Method, this method comprises the following steps：
S1, material added into storage compartment 1 by charging aperture, and redirect and perform step S2；Wherein, material include zinc granule,
Hard alloy scraps and NaF-KF fused salts；Wherein, NaF-KF mol ratio is preferably 4:6.
S2, charging aperture is closed, storage compartment 1 is vacuumized by the first vacuum orifice 1-1, until the pressure in storage compartment 1
Reach the first specified pressure, and redirect and perform step S3；
S3, discharging opening is opened, because the outlet of now dosage unit 3 is located exactly at first anode basket 4-3 top, so that
After opening discharging opening, material can be fallen directly in first anode basket 4-3 by dosage unit 3, after the first specified time
After adding the material of specified amount i.e. into first anode basket 4-3, discharging opening is closed, and redirects and performs step S4；
S4, driving reaction member 4 rotate 180 °, and redirect and perform step S5；
S5, discharging opening is opened, because first anode basket 4-3 and second plate basket 4-4 is on the Central Symmetry of reaction member 4,
Therefore after reaction member 4 rotates 180 °, the outlet of dosage unit 3 is located exactly at second plate basket 4-4 top, so as to beat again
After outputing material mouth, material can be fallen directly in second plate basket 4-4 by dosage unit 3, after the first specified time i.e.
After adding the material of specified amount into second plate basket 4-4, discharging opening is closed, and redirects and performs step S6；
S6, by the second vacuum orifice 2-3 reative cell 2 is vacuumized, specified until the pressure in reative cell 2 reaches second
Pressure, while start heater, until temperature reaches the first assigned temperature in reative cell 2, and redirect and perform step S7；Wherein,
First assigned temperature is preferably 300 DEG C.
S7, inert gas is passed through to reative cell 2 by air inlet 2-1, specified until the pressure in reative cell 2 reaches the 3rd
After pressure, gas outlet 2-2 is opened, and starts heater, until the temperature in reative cell 2 reaches the second assigned temperature, and is redirected
Perform step S8；Wherein, inert gas is preferably that argon gas, the 3rd specified pressure are preferably 105Pa, the second assigned temperature are preferably
750℃。
S8, start the first power supply to first anode basket 4-3 and the first collection pit 4-211 application 0.6V voltages, start simultaneously
Second source applies 2V voltages to second plate basket 4-4 and the 3rd collection pit 4-221, and redirects and perform step S9；Due to now
The first sheet metal 5 connected with the positive pole of the first power supply contact just with the anode conducting post 4-5 on first anode basket 4-3 and
Second sheet metal 6 of the negative pole connection of the first power supply contacts with the negative electrode conductive pole being plugged on the first collection pit 4-211, i.e., and the
One power supply, first anode basket 4-3 and the first collection pit 4-211 collectively form an electrolysis loop；And with the positive pole of second source
First sheet metal 5 of connection is contacted with the anode conducting post 4-5 on second plate basket 4-4, is connected with the negative pole of second source
Second sheet metal 6 contacts with the negative electrode conductive pole being plugged on the 3rd collection pit 4-221, i.e. second source, second plate basket 4-4
Another electrolysis loop is collectively formed with the 3rd collection pit 4-221；Therefore, the hard alloy scraps in first anode basket 4-3 exist
After being gradually ionized in NaF-KF fused salts, cobalt ions can be reduced into simple substance, be deposited in the first collection pit 4-211, and the
After hard alloy scraps are gradually ionized in NaF-KF fused salts in two anode basket 4-4, tungsten ion can be reduced into simple substance, deposition
In the 3rd collection pit 4-221；
S9, after the second specified time, driving reaction member 4 rotate 180 ° so that the first power supply is to second plate basket
4-4 and the 4th collection pit 4-222 applies 0.6V voltages, second source applies to first anode basket 4-3 and the second collection pit 4-212
2V voltages, and redirect and perform step S10；Wherein, the second specified time was preferably 1 hour.Due to, the first collection pit 4-211 with
4th collection pit 4-222 and the second collection pit 4-212 and the 3rd collection pit 4-221 on the Central Symmetry of reaction member 4, because
This, after reaction member 4 rotates 180 °, the sun on the first sheet metal 5 and second plate basket 4-4 that be connected with the positive pole of the first power supply
Pole conductive pole 4-5 contacts, the second sheet metal 6 being connected with the negative pole of the first power supply are with being plugged on the 4th collection pit 4-222
Negative electrode conductive pole contacts, i.e. the first power supply, second plate basket 4-4 and the 4th collection pit 4-222 collectively form an electrolysis loop；
And contacted with the first sheet metal 5 that the positive pole of second source connects with the anode conducting post 4-5 on first anode basket 4-3 and the
Second sheet metal 6 of the negative pole connection of two power supplys contacts with the negative electrode conductive pole being plugged on the second collection pit 4-212, i.e., and second
Power supply, first anode basket 4-3 and the second collection pit 4-212 collectively form another electrolysis loop.So as in second plate basket 4-4
Hard alloy scraps be gradually ionized in NaF-KF fused salts after, cobalt ions can be reduced into simple substance, be deposited on the 4th collection
Cheat in 4-222, and after the hard alloy scraps in first anode basket 4-3 are gradually ionized in NaF-KF fused salts, tungsten ion meeting
Simple substance is reduced into, is deposited in the second collection pit 4-212.
S10, after the second specified time, driving reaction member 4 rotates 180 °, and redirects and perform step S8.
Thus, every 1 hour, primary first-order equation unit 4 is rotated, cobalt will be received constantly in the first collection pit 4-211 and the 4th
Deposited in the 4-222 of collection hole, at the same time, tungsten can be deposited constantly in the second collection pit 4-212 and the 3rd collection pit 4-221.By
It is different from the density of tungsten and cobalt in zinc, therefore after the completion of preparing, pass through the second siphon port 2-4 and corresponding the using siphoning installation
One siphon port 4-13, so that it may collect the first collection pit 4-211, the second collection pit 4-212, the 3rd collection pit 4-221 or the 4th
The liquid Zn cheated in 4-222 suctions out, and then just can obtain pure tungsten and pure cobalt.As shown in Figure 6 and Figure 7, the tungsten powder that finally prepares and
The particle of cobalt powder is uniform, composition is single.
It should be noted that the voltage that the first power supply applies is not limited to 0.6V, the voltage that second source applies is also not necessarily limited to
2V, as long as the voltage that the first power supply applies is less than 0.8V, the voltage that second source applies is more than 0.8V.
Finally it should be noted that：Above example is only to illustrate the technical scheme of invention, rather than its limitations；Although ginseng
Invention is described in detail according to previous embodiment, it will be understood by those within the art that：It still can be right
Technical scheme described in foregoing embodiments is modified, or carries out equivalent substitution to which part technical characteristic；And this
A little modifications are replaced, and the essence of appropriate technical solution is departed from the spirit and scope for inventing each embodiment technical scheme.
Claims (10)
- A kind of 1. continuous device for preparing tungsten powder and cobalt powder, it is characterised in that including：Storage compartment, the storage compartment are provided with the first vacuum orifice and the charging aperture and discharging opening that can open and close；Reative cell, the reative cell be located at the storage compartment lower section, the reative cell be provided with the second vacuum orifice, air inlet, Gas outlet and heater；Reaction member, for the reaction member in the reative cell, the both ends of the reaction member are respectively equipped with the first graphite Groove and the second graphite cuvette；Suspension has first anode basket and second plate respectively in first graphite cuvette and second graphite cuvette The top of basket, the first anode basket and the second plate basket is respectively connected with anode conducting post；The bottom of first graphite cuvette The both ends in portion offer the first collection pit and the second collection pit respectively, and the both ends of the bottom of second graphite cuvette offer respectively 3rd collection pit and the 4th collection pit, first collection pit, second collection pit, the 3rd collection pit and the described 4th The bottom of collection pit is inserted with negative electrode conductive pole；The first anode basket and the second plate basket, first collection pit With the 4th collection pit and second collection pit with the 3rd collection pit on the reaction member Central Symmetry；Dosage unit, the import of the dosage unit located at the lower section of the discharging opening, outlet located at the first anode basket and The top of circumference where the second plate basket；First power supply and second source, first power supply and the second source are respectively arranged on the both sides of the reative cell, institute The positive pole for stating the first power supply and the second source is connected with the first sheet metal by wire, and first sheet metal is located at institute State on the circumference where the top of anode conducting post；First power supply is connected with the negative pole of the second source by wire There is the second sheet metal, second sheet metal is on the circumference where the bottom of the negative electrode conductive pole；AndDriver element, the driver element are used to driving the reaction member using its center to be that the center of circle rotates, so that described in each First sheet metal and second sheet metal electrically connect with the corresponding anode conducting post and the negative electrode conductive pole respectively.
- 2. the continuous device for preparing tungsten powder and cobalt powder according to claim 1, it is characterised in that on first graphite cuvette The first corundum plate for suspending the first anode basket is covered with, is covered with second graphite cuvette for suspending described the Second corundum plate of two anode baskets.
- 3. the continuous device for preparing tungsten powder and cobalt powder according to claim 2, it is characterised in that the first corundum plate and The first siphon port is offered on the second corundum plate, is offered on the reative cell and closes on the second of first siphon port Siphon port.
- 4. the continuous device for preparing tungsten powder and cobalt powder according to claim 2, it is characterised in that the reaction member includes It is embedded with the upper groove body of the first corundum plate and the second corundum plate and provided with first graphite cuvette and described second The lower groove of graphite cuvette.
- 5. the continuous device for preparing tungsten powder and cobalt powder according to claim 4, it is characterised in that the lower groove with it is described Corundum is filled between first graphite cuvette and second graphite cuvette.
- 6. the continuous device for preparing tungsten powder and cobalt powder according to claim 1, it is characterised in that the dosage unit is entered Mouth is in infundibulate, and the size of the import is more than the size of the discharging opening.
- 7. the continuous device for preparing tungsten powder and cobalt powder according to claim 1, it is characterised in that first collection pit, Second collection pit, the 3rd collection pit and the 4th collection pit respectively with the corresponding pluggable company of negative electrode conductive pole Connect.
- 8. the continuous device for preparing tungsten powder and cobalt powder according to claim 7, it is characterised in that the negative electrode conductive pole bag Include nickel rod and the corundum set being arranged on the nickel rod.
- 9. the continuous device for preparing tungsten powder and cobalt powder according to any one of claim 1 to 8, it is characterised in that the drive Moving cell includes the motor for being plugged in the drive link of the reaction member bottom centre and being electrically connected with the drive link.
- A kind of 10. continuous method for preparing tungsten powder and cobalt powder, it is characterised in that comprise the following steps：S1, material is added into storage compartment by charging aperture, and redirect and perform step S2；Wherein, the material includes zinc granule, given up Hard alloy and NaF-KF fused salts；S2, charging aperture is closed, storage compartment is vacuumized by the first vacuum orifice, until the pressure in storage compartment reaches the first finger Constant-pressure, and redirect and perform step S3；S3, discharging opening is opened to first anode basket addition material, after the first specified time, close discharging opening, and redirect and hold Row step S4；S4, driving reaction member rotate 180 °, and redirect and perform step S5；S5, discharging opening is opened to second plate basket addition material, after the first specified time, close discharging opening, and redirect and hold Row step S6；S6, by the second vacuum orifice reative cell is vacuumized, until the pressure in reative cell reaches the second specified pressure, simultaneously Start heater, until reaction indoor temperature reaches the first assigned temperature, and redirect and perform step S7；S7, inert gas is passed through to reative cell by air inlet, until after the pressure in reative cell reaches the 3rd specified pressure, beaten Gas port is outputed, and starts heater, until the temperature in reative cell reaches the second assigned temperature, and redirects and performs step S8；S8, start the first power supply 0.6V voltages are applied to first anode basket and the first collection pit, while start second source to the Two anode baskets and the 3rd collection pit apply 2V voltages, and redirect and perform step S9；S9, after the second specified time, driving reaction member rotate 180 ° so that the first power supply is to second plate basket and the 4th Collection pit applies 0.6V voltages, second source applies 2V voltages to first anode basket and the second collection pit, and redirects execution step S10；S10, after the second specified time, close the first power supply and second source, driving reaction member rotates 180 °, and redirects Perform step S8.
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| CN107858709A (en) * | 2017-12-14 | 2018-03-30 | 东莞理工学院 | A kind of fused salt electrolysis apparatus for preparing metal mixed powder |
| CN110656357A (en) * | 2019-08-22 | 2020-01-07 | 北京工业大学 | Device and method for removing carbon and recovering cobalt and tungsten in waste WC-Co alloy |
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| CN107513730B (en) | 2019-06-14 |
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