CN107513730B - Continuously prepare the device and method of tungsten powder and cobalt powder - Google Patents
Continuously prepare the device and method of tungsten powder and cobalt powder Download PDFInfo
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- CN107513730B CN107513730B CN201710772262.3A CN201710772262A CN107513730B CN 107513730 B CN107513730 B CN 107513730B CN 201710772262 A CN201710772262 A CN 201710772262A CN 107513730 B CN107513730 B CN 107513730B
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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 fields, provide a kind of device and method for continuously preparing tungsten powder and cobalt powder, which includes storage compartment, reaction chamber, reaction member, dosage unit, driving unit, 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 third collection pit and the 4th collection pit respectively；First power supply and second source are respectively arranged on the two sides of reaction chamber；Driving unit is rotated for drive response unit by the center of circle of its center.The present invention not only can continuously be obtained cobalt in the first collection pit and the 4th collection pit using this method, obtain tungsten in the second collection pit and third collection pit, but also significantly improved the rate of recovery and separative efficiency, avoided electrode conversion.
Description
Technical field
The present invention relates to electrochemical technology fields, more particularly to a kind of device and side for continuously preparing tungsten powder and cobalt powder
Method.
Background technique
Refractory metals tungsten and rare metal cobalt are particularly important strategic elements generally acknowledged in the world, are passed through to country is improved
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, to further cause the shortage of tungsten resource.In addition to this, 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 is carbide and binding metal refractory metals tungsten through having height hard made of powder metallurgy process
The material of degree, high-flexural strength, obtains in fields such as machine-building, mining, communications and transportation, energy exploration, building decorations
To being widely applied.Currently, the tungsten resource that the whole world is more than 50% is used to manufacture hard alloy, and the tungsten in hard alloy scraps contains
Amount just has reached 74%~91%.Therefore, recycling hard alloy scraps are a kind of very effective approach for recycling tungsten, cobalt.
The method of existing recycling 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 recovery efficiency of the molten method of zinc, and it is easy to bring some impurity elements into；Electrification
Method, oxidation-reduction method can not be recycled continuously, and recovery efficiency is relatively low；Acid leaching process can generate some exhaust gas such as SO2、
NO2。
Summary of the invention
The present invention is to solve tungsten, the rate of recovery of cobalt are low in the prior art, the technical issues of can not continuously recycling.
To solve the above problems, the present invention provides a kind of device for continuously preparing tungsten powder and cobalt powder, which includes:
Storage compartment, the inlet port and outlet port that the storage compartment is equipped with the first vacuum orifice and can open and close；
Reaction chamber, the reaction chamber are set to the lower section of the storage compartment, and the reaction chamber is equipped with the second vacuum orifice, air inlet
Mouth, gas outlet and heater；
Reaction member, the reaction member are set in the reaction chamber, and 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 column；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
Equipped with third collection pit and the 4th collection pit, first collection pit, second collection pit, the third collection pit and described
The bottom of 4th collection pit is inserted with cathode conductive column；The first anode basket and the second plate basket, first receipts
Ji Keng and the 4th collection pit and second collection pit and the third collection pit are about the reaction member center
Symmetrically；
Dosage unit, the import of the dosage unit is set to the lower section of the discharge port, outlet is set to the first anode
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 reaction chamber
The anode of side, first power supply and the second source is connected with the first sheet metal, first sheet metal by conducting wire
On the circumference where the top of the anode conducting column；The cathode of first power supply and the second source, which passes through, leads
Line is connected with the second sheet metal, and second sheet metal is on the circumference where the bottom end of the cathode conductive column；And
Driving unit, the driving unit are used to that the reaction member to be driven to rotate using its center as the center of circle, so that each
First sheet metal and second sheet metal are electrically connected with the corresponding anode conducting column and the cathode conductive column respectively
It connects.
Wherein, the first graphite groove upper cap is equipped with the first corundum plate for suspending the first anode basket, and described the
Two graphite groove upper caps are equipped with the second corundum plate for suspending the second plate basket.
Wherein, the first siphon port is offered on the first corundum plate and the second corundum plate, on the reaction chamber
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 equipped 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 greater than the size of the discharge port.
Wherein, first collection pit, second collection pit, the third collection pit and the 4th collection pit difference
With the corresponding pluggable connection of cathode conductive column.
Wherein, the cathode conductive column includes nickel stick and the corundum set that is arranged on the nickel stick.
Wherein, the driving unit include be plugged in the reaction member bottom centre drive rod and with the transmission
The motor of bar electrical connection.
To solve the above problems, the present invention also provides a kind of method for continuously preparing tungsten powder and cobalt powder, this method includes
Following steps:
S1, material is added into storage compartment by feed inlet, and jumps and executes step S2；Wherein, the material includes zinc
Grain, hard alloy scraps and NaF-KF fused salt；
S2, feed inlet is closed, storage compartment is vacuumized by the first vacuum orifice, until the indoor pressure of storing reaches the
One specified pressure, and jump and execute step S3；
Material is added to first anode basket in S3, opening discharge port, after the first specified time, closes discharge port, and jump
Turn to execute step S4；
180 ° of S4, drive response unit rotational, and jump and execute step S5；
Material is added to second plate basket in S5, opening discharge port, after the first specified time, closes discharge port, and jump
Turn to execute step S6；
S6, reaction chamber is vacuumized by the second vacuum orifice, until reacting indoor pressure reaches the second specified pressure,
Start heater simultaneously, until reaction room temperature reaches the first assigned temperature, and jumps and execute step S7；
S7, inert gas is passed through to reaction chamber by air inlet, until reacting indoor pressure reaches third specified pressure
Afterwards, gas outlet is opened, and starts heater, until reacting indoor temperature reaches the second assigned temperature, and jumps execution step
S8；
S8, the first power supply of starting apply 0.6V voltage to first anode basket and the first collection pit, while starting second source
2V voltage is applied to second plate basket and third collection pit, and jumps and executes step S9；
S9, after the second specified time, 180 ° of drive response unit rotational so that the first power supply to second plate basket and
4th collection pit applies 0.6V voltage, second source and applies 2V voltage to first anode basket and the second collection pit, and jumps execution
Step S10；
S10, after the second specified time, 180 ° of drive response unit rotational, and jump execute 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
With third collection pit about reaction member central symmetry the characteristics of, by driving unit drive response unit rotational, make to react
When unit rotational is to designated position, the first power supply applies 0.6V voltage, second source applies 2V voltage, so that the first power supply, the
One anode basket and the first collection pit collectively form an electrolysis circuit, while collect second source, second plate basket and third
Hole collectively forms another electrolysis circuit；After reaction member continues to rotate 180 °, and a power supply, second plate basket and can be made
Four collection pits collectively form an electrolysis circuit, while collectively form second source, first anode basket and the second collection pit separately
One electrolysis circuit, thus different with the precipitation coefficient of cobalt using tungsten, so that it may continuously in the first collection pit and the 4th collection pit
It obtains cobalt, obtain tungsten in the second collection pit and third collection pit, so that the rate of recovery and separative efficiency are not only significantly improved, and
And electrode conversion is also avoided, extend the service life of the device.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram for the device for continuously preparing tungsten powder and cobalt powder in the embodiment of the present invention 1；
Fig. 2 is the structural schematic diagram of reaction member in the embodiment of the present invention 1；
Fig. 3 is the structural schematic diagram of cathode conductive column in the embodiment of the present invention 1；
Fig. 4 is the structural schematic diagram of lower groove in the embodiment of the present invention 1；
Fig. 5 is the structural schematic diagram of upper groove body in the embodiment of the present invention 1；
Fig. 6 is the cobalt powder prepared in the embodiment of the present invention 2 and the XRD diagram of tungsten powder, wherein Fig. 6 (a) is the XRD diagram of cobalt powder；
6 (b) be the XRD diagram of tungsten powder；
Fig. 7 is the SEM figure 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) scheme for the SEM of tungsten powder.
Appended drawing reference:
1, storage compartment；1-1, the first vacuum orifice；2, reaction chamber；2-1, air inlet；
2-2, gas outlet；2-3, the second vacuum orifice；2-4, the second siphon port；
3, dosage unit；4, 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, third 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 column；4-6, cathode mounting hole；4-71, nickel stick；
4-72, corundum set；5, the first sheet metal；6, the second sheet metal；7, drive rod.
Specific embodiment
To keep the purposes, technical schemes and advantages of invention clearer, below in conjunction with the attached drawing in invention, in invention
Technical solution be explicitly described, it is clear that described embodiment is invention a part of the embodiment, rather than whole realities
Apply example.It is obtained by those of ordinary skill in the art without making creative efforts based on the embodiment in invention
Every other embodiment belongs to the range of invention protection.
In the description of the present invention, unless otherwise indicated, the orientation or position of the instructions such as term " on ", "lower", "top", "bottom"
Setting relationship is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description of the present invention and simplification of the description, rather than
The device or element of indication or suggestion meaning must have a particular orientation, be constructed and operated in a specific orientation, therefore cannot
It is interpreted as limitation of the present invention.
It should be noted that unless otherwise clearly defined and limited, term " connection " shall be understood in a broad sense, for example, can
To be to be fixedly connected, may be a detachable connection, or be integrally connected；It can be directly connected, intermediate 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 meaning.
Embodiment 1
In conjunction with shown in Fig. 1 to Fig. 5, the present invention provides a kind of device for continuously preparing tungsten powder and cobalt powder, which includes:
Storage compartment 1, the side wall of storage compartment 1 are equipped with that the first vacuum orifice 1-1, top and bottom offer respectively to open and close
Inlet port and outlet port；
Reaction chamber 2, reaction chamber 2 are set to the lower section of storage compartment 1, and reaction chamber 2 is equipped with the second vacuum orifice 2-3, air inlet 2-
1, gas outlet 2-2 and heater；Wherein, air inlet 2-1 and gas outlet 2-2 is separately positioned on the two sides of reaction chamber 2, and air inlet
2-1 is located at the top of gas outlet 2-2；Heater is preferably the heater strip for being wrapped in the outer wall of reaction chamber 2.
Reaction member 4, reaction member 4 are set in reaction chamber 2, and 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
The top of second plate basket 4-4, first anode basket 4-3 and second plate basket 4-4 are respectively connected with anode conducting column 4-5；First stone
The both ends of the bottom of ink tank 4-21 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 third collection pit 4-221 and the 4th collection pit 4-222 respectively, the first collection pit 4-211, second are received
The bottom of collection hole 4-212, third collection pit 4-221 and the 4th collection pit 4-222 are inserted with cathode conductive column；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 third
Collection pit 4-221 is about 4 central symmetry of reaction member；
Dosage unit 3, the import of dosage unit 3 is set to the lower section of discharge port, outlet is set to first anode basket 4-3 and second
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 two sides of reaction chamber 2, the first power supply and
The anode of second source is connected with the first sheet metal 5 by conducting wire, and the first sheet metal 5 is set to the top of anode conducting column 4-5
On the circumference at place；The cathode of first power supply and second source passes through conducting wire and is connected with the second sheet metal 6, the second sheet metal 6
On the circumference where the bottom end of cathode conductive column；And
Driving unit, driving unit is for drive response unit 4 using its center as center of circle rotation, so that each first metal
Piece 5 and the second sheet metal 6 are electrically connected with corresponding anode conducting column 4-5 and cathode conductive column respectively, that is to say, that when reaction is single
When member 4 turns to designated position, with the anode on positive the first sheet metal 5 and first anode basket 4-3 connecting of the first power supply
Conductive column 4-5 contact, second connect with the cathode of the first power supply sheet metals 6 and the yin that is plugged on the first collection pit 4-211
The contact of pole conductive column, i.e. the first power supply, first anode basket 4-3 and the first collection pit 4-211 collectively form an electrolysis circuit；With
This simultaneously, with second source anode connection the first sheet metal 5 contacted with the anode conducting column 4-5 on second plate basket 4-4,
The second sheet metal 6 connected with the cathode of second source is contacted with the cathode conductive column being plugged on third collection pit 4-221, i.e.,
Second source, second plate basket 4-4 and third collection pit 4-221 collectively form another electrolysis circuit.And when reaction member 4 after
After continuous rotation 180, with the anode conducting column 4-5 on positive the first sheet metal 5 and second plate basket 4-4 connecting of the first power supply
Contact, the second sheet metal 6 connecting with the cathode of the first power supply connect with the cathode conductive column being plugged on the 4th collection pit 4-222
Touching, i.e. the first power supply, second plate basket 4-4 and the 4th collection pit 4-222 collectively form an electrolysis circuit；At the same time, with
First sheet metal 5 of the anode connection of second source is contacted with the anode conducting column 4-5 on first anode basket 4-3 and the second electricity
Second sheet metal 6 of the cathode connection in source is contacted with the cathode conductive column 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 circuit.
Specifically, when use:
Firstly, be put into material in storage compartment 1, i.e. zinc granule, hard alloy scraps and NaF-KF fused salt；
Secondly, opening discharge port after vacuumizing by the first vacuum orifice 1-1 to storage compartment 1, material can pass through charging
Unit 3 is fallen directly in first anode basket 4-3；
Then, start driving unit, so that reaction member 4 rotates 180 °, the outlet of dosage unit 3 at this time is located exactly at the
The top of two anode basket 4-4, so that material can fall directly on second plate by dosage unit 3 after being again turned on discharge port
In basket 4-4；
Then, reaction chamber 2 is vacuumized by the second vacuum orifice 2-3, while starts heater, until in reaction chamber 2
After temperature reaches 300 DEG C, argon gas is filled with into reaction chamber 2 by air inlet 2-1, when the pressure in reaction chamber 2 reaches 105Pa
Afterwards, gas outlet 2-2 is opened, while being again started up heater, until the temperature in reaction chamber 2 reaches 750 DEG C, is contained in the at this time
One anode basket 4-3 and NaF-KF fused salt in second plate basket 4-4 and zinc granule are completely melt that NaF-KF fused salt just flows into the first stone
In ink tank 4-21 and the second graphite cuvette 4-22, since the density of zinc is larger, liquid Zn can be deposited on the first collection pit 4-
211, in the second collection pit 4-212, third collection pit 4-221 and the 4th collection pit 4-222；
Next, applying 0.6V voltage by the first power supply, while 2V voltage is applied by second source.At this point, with
First sheet metal 5 of the anode connection of one power supply contact with the anode conducting column 4-5 on first anode basket 4-3 just, and first
Second sheet metal 6 of the cathode connection of power supply is contacted with the cathode conductive column 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 circuit；And it is connect with the anode of second source
The first sheet metal 5 contact, connect with the cathode of second source with the anode conducting column 4-5 on second plate basket 4-4 second
Sheet metal 6 is contacted with the cathode conductive column being plugged on third collection pit 4-221, i.e. second source, second plate basket 4-4 and
Three collection pit 4-221 collectively form another electrolysis circuit.Since tungsten is different with the deposition potential of cobalt, i.e., when applied voltage is small
When 0.8V, cobalt is easy to be precipitated, and when applied voltage is greater than 0.8V, tungsten is easy to be precipitated.Therefore, in first anode basket 4-3
After hard alloy scraps are gradually ionized in NaF-KF fused salt, 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 salt, tungsten ion can quilt
It is reduced into simple substance, is deposited in third collection pit 4-221；
Finally, starting driving unit makes reaction member 4 rotate 180 ° after 1 hour.Due to the first collection pit 4-211
With the 4th collection pit 4-222 and the second collection pit 4-212 and third collection pit 4-221 about 4 central symmetry of reaction member,
Therefore after reaction member 4 rotates 180 °, on positive the first sheet metal 5 and second plate basket 4-4 connecting of the first power supply
It anode conducting column 4-5 contact, the second sheet metal 6 being connect with the cathode of the first power supply and is plugged on the 4th collection pit 4-222
Cathode conductive column 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 with second source anode connection the first sheet metal 5 contacted with the anode conducting column 4-5 on first anode basket 4-3, and
Second sheet metal 6 of the cathode connection of second source is contacted with the cathode conductive column 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 circuit.To second plate basket 4-4
In hard alloy scraps be gradually ionized in NaF-KF fused salt 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 salt, tungsten ion
It can be reduced into simple substance, be deposited in the second collection pit 4-212.
As a result, 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
It is 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 third collection pit 4-221.By
The density of Yu Xinyu tungsten and cobalt is different, therefore after the completion of preparing, directly liquid Zn can be sucked out, and then pure tungsten and pure just can be obtained
Cobalt.
Preferably, the first graphite cuvette 4-21 upper cover is equipped with the first corundum plate 4-11 for suspending first anode basket 4-3, the
Two graphite cuvette 4-22 upper covers are equipped with the second corundum plate 4-12 for suspending second plate basket 4-4, specifically, the first corundum plate 4-
11 middle part offers the first mounting hole, and the top of first anode basket 4-3 and the clamping of the first mounting hole, second end protrude into the first stone
In ink tank 4-21；The second mounting hole, the top of second plate basket 4-4 and the second installation are offered in the middle part of second corundum plate 4-12
Hole clamping, second end protrude into the second graphite cuvette 4-22.
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.It is logical using siphoning installation as a result, after the completion of preparation
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 third collection pit 4-221 or the 4th collection pit 4-222 is sucked out, and then pure tungsten and pure cobalt just can be obtained.
Preferably, reaction member 4 include be embedded with the upper groove body 4-1 of the first corundum plate 4-11 and the second corundum plate 4-12 with
And the lower groove 4-2 equipped 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 be in infundibulate, and the size of import be greater than discharge port size, with guarantee from
The material that discharge port is fallen fully enters in dosage unit 3.
In addition, update and replace for the ease of the later period since cathode conductive column easily corrodes, the first collection pit 4-211, second
Collection pit 4-212, third collection pit 4-221 and the 4th collection pit 4-222 respectively with the corresponding pluggable connection of cathode conductive column.
Specifically, the bottom of the first collection pit 4-211, the second collection pit 4-212, third collection pit 4-221 and the 4th collection pit 4-222
Center offer the cathode mounting hole 4-6 for plugging cathode conductive column.Wherein, cathode conductive column include nickel stick 4-71 and
The corundum set 4-72 being arranged on nickel stick 4-71.
Wherein, driving unit includes being plugged in the drive rod 7 of 4 bottom centre of reaction member and being electrically connected with drive rod 7
Motor, i.e. one end of drive rod 7 is plugged in the center of the bottom of reaction member 4, the other end is connected to motor.Work as electricity as a result,
While machine drives drive rod 7 to rotate, reaction member 4 can rotate therewith under the drive of drive rod 7.
Preferably, first anode basket 4-3 and second plate basket 4-4 are woven by platinum filament.
Embodiment 2
Based on the above-mentioned device for continuously preparing tungsten powder and cobalt powder, tungsten powder and cobalt powder are continuously prepared the present invention also provides a kind of
Method, method includes the following steps:
S1, material is added into storage compartment 1 by feed inlet, and jumps and executes step S2；Wherein, material include zinc granule,
Hard alloy scraps and NaF-KF fused salt；Wherein, the molar ratio of NaF-KF is preferably 4:6.
S2, feed inlet 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 jumps and execute step S3；
S3, discharge port is opened, since the outlet of dosage unit 3 at this time is located exactly at the top of first anode basket 4-3, thus
After opening discharge port, material can be fallen directly in first anode basket 4-3 by dosage unit 3, after the first specified time
After the material of specified amount is added i.e. into first anode basket 4-3, discharge port is closed, and jumps and executes step S4；
S4, drive response unit 4 rotate 180 °, and jump and execute step S5；
S5, discharge port is opened, since first anode basket 4-3 and second plate basket 4-4 is about 4 central symmetry of reaction member,
Therefore after reaction member 4 rotates 180 °, the outlet of dosage unit 3 is located exactly at the top of second plate basket 4-4, 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 the material of specified amount is added into second plate basket 4-4, discharge port is closed, and jumps and executes step S6；
S6, reaction chamber 2 is vacuumized by the second vacuum orifice 2-3, is specified until the pressure in reaction chamber 2 reaches second
Pressure, while starting heater, until temperature reaches the first assigned temperature in reaction chamber 2, and jumps and execute step S7；Wherein,
First assigned temperature is preferably 300 DEG C.
S7, inert gas is passed through to reaction chamber 2 by air inlet 2-1, until the pressure in reaction chamber 2 reaches third and specifies
After pressure, gas outlet 2-2 is opened, and start heater, until the temperature in reaction chamber 2 reaches the second assigned temperature, and jumped
Execute step S8；Wherein, it is preferably 10 that inert gas, which is preferably argon gas, third specified pressure,5Pa, the second assigned temperature are preferably
750℃。
S8, the first power supply of starting apply 0.6V voltage to first anode basket 4-3 and the first collection pit 4-211, start simultaneously
Second source applies 2V voltage to second plate basket 4-4 and third collection pit 4-221, and jumps and execute step S9；Due at this time
With the first power supply anode connection the first sheet metal 5 contact just with the anode conducting column 4-5 on first anode basket 4-3, and
Second sheet metal 6 of the cathode connection of the first power supply is contacted with the cathode conductive column 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 circuit；And the anode with second source
First sheet metal 5 of connection is contacted with the anode conducting column 4-5 on second plate basket 4-4, is connect with the cathode of second source
Second sheet metal 6 is contacted with the cathode conductive column being plugged on third collection pit 4-221, i.e. second source, second plate basket 4-4
Another electrolysis circuit is collectively formed with third collection pit 4-221；Therefore, the hard alloy scraps in first anode basket 4-3 exist
After being gradually ionized in NaF-KF fused salt, 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 salt in two anode basket 4-4, tungsten ion can be reduced into simple substance, deposition
In third collection pit 4-221；
S9, after the second specified time, drive response unit 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 voltage, second source applies first anode basket 4-3 and the second collection pit 4-212
2V voltage, and jump and execute 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 third collection pit 4-221 about 4 central symmetry of reaction member, because
This, after reaction member 4 rotates 180 °, with the sun on positive the first sheet metal 5 and second plate basket 4-4 connecting of the first power supply
It pole conductive column 4-5 contact, the second sheet metal 6 being connect with the cathode of the first power supply and is plugged on the 4th collection pit 4-222
The contact of cathode conductive column, i.e. the first power supply, second plate basket 4-4 and the 4th collection pit 4-222 collectively form an electrolysis circuit；
And it is contacted with the first sheet metal 5 of the anode connection of second source with the anode conducting column 4-5 on first anode basket 4-3 and the
Second sheet metal 6 of the cathode connection of two power supplys is contacted with the cathode conductive column 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 circuit.To in second plate basket 4-4
Hard alloy scraps be gradually ionized in NaF-KF fused salt after, cobalt ions can be reduced into simple substance, be deposited on the 4th collection
It cheats in 4-222, and after the hard alloy scraps in first anode basket 4-3 are gradually ionized in NaF-KF fused salt, tungsten ion meeting
It is reduced into simple substance, is deposited in the second collection pit 4-212.
S10, after the second specified time, drive response unit 4 rotate 180 °, and jump execute step S8.
As a result, 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
It is 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 third collection pit 4-221.By
The density of Yu Xinyu tungsten and cobalt is different, therefore after the completion of preparing, and passes 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, third collection pit 4-221 or the 4th
The liquid Zn cheated in 4-222 is sucked out, and then pure tungsten and pure cobalt just can be obtained.As shown in Figure 6 and Figure 7, the tungsten powder that finally prepares and
The particle of cobalt powder is uniform, ingredient 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 greater than 0.8V.
Finally, it should be noted that above embodiments are only to illustrate the technical solution of invention, rather than its limitations；Although ginseng
Invention is described in detail according to previous embodiment, those skilled in the art should understand that: it still can be right
Technical solution documented by foregoing embodiments is modified or equivalent replacement of some of the technical features；And this
It modifies or replaces, the spirit and scope for each embodiment technical solution of invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of device for continuously preparing tungsten powder and cobalt powder characterized by comprising
Storage compartment, the inlet port and outlet port that the storage compartment is equipped with the first vacuum orifice and can open and close；
Reaction chamber, the reaction chamber be set to the storage compartment lower section, the reaction chamber be equipped with the second vacuum orifice, air inlet,
Gas outlet and heater；
Reaction member, the reaction member are set in the reaction chamber, and the both ends of the reaction member are respectively equipped with the first graphite
Slot 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 column；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
Third collection pit and the 4th collection pit, first collection pit, second collection pit, the third collection pit and the described 4th
The bottom of collection pit is inserted with cathode conductive column；The first anode basket and the second plate basket, first collection pit
With the 4th collection pit and second collection pit and the third collection pit about the reaction member central symmetry；
Dosage unit, the import of the dosage unit is set to the lower section of the discharge port, outlet is set to 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 two sides of the reaction chamber, institute
The anode for stating the first power supply and the second source is connected with the first sheet metal by conducting wire, and first sheet metal is set to institute
It states on the circumference where the top of anode conducting column；First power supply passes through conducting wire with the cathode of the second source and connects
There is the second sheet metal, second sheet metal is on the circumference where the bottom end of the cathode conductive column；And
Driving unit, the driving unit are used to that the reaction member to be driven to rotate using its center as the center of circle, so that each described
First sheet metal and second sheet metal are electrically connected with the corresponding anode conducting column and the cathode conductive column respectively.
2. the device according to claim 1 for continuously preparing tungsten powder and cobalt powder, which is characterized in that on first graphite cuvette
It is covered with the first corundum plate for suspending the first anode basket, the second graphite groove upper cap is equipped with for suspending described the
Second corundum plate of two anode baskets.
3. according to claim 2 continuously prepare the device of tungsten powder and cobalt powder, which is characterized in that the first corundum plate and
The first siphon port is offered on the second corundum plate, is offered on the reaction chamber and is closed on the second of first siphon port
Siphon port.
4. according to claim 2 continuously prepare the device of tungsten powder and cobalt powder, which is characterized 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 is equipped with first graphite cuvette and described second
The lower groove of graphite cuvette.
5. according to claim 4 continuously prepare the device of tungsten powder and cobalt powder, which is characterized in that the lower groove with it is described
Corundum is filled between first graphite cuvette and second graphite cuvette.
6. according to claim 1 continuously prepare the device of tungsten powder and cobalt powder, which is characterized in that the dosage unit into
Mouth is in infundibulate, and the size of the import is greater than the size of the discharge port.
7. the device according to claim 1 for continuously preparing tungsten powder and cobalt powder, which is characterized in that first collection pit,
Second collection pit, the third collection pit and the 4th collection pit respectively with the corresponding pluggable company of cathode conductive column
It connects.
8. the device according to claim 7 for continuously preparing tungsten powder and cobalt powder, which is characterized in that the cathode conductive column packet
The corundum set for including nickel stick and being arranged on the nickel stick.
9. the device according to any one of claims 1 to 8 for continuously preparing tungsten powder and cobalt powder, which is characterized in that the drive
Moving cell includes the motor for being plugged in the drive rod of the reaction member bottom centre and being electrically connected with the drive rod.
10. a kind of method for continuously preparing tungsten powder and cobalt powder, which comprises the following steps:
S1, material is added into storage compartment by feed inlet, and jumps and executes step S2；Wherein, the material includes zinc granule, gives up
Hard alloy and NaF-KF fused salt；
S2, feed inlet is closed, storage compartment is vacuumized by the first vacuum orifice, until the indoor pressure of storing reaches the first finger
Constant-pressure, and jump and execute step S3；
Material is added to first anode basket in S3, opening discharge port, after the first specified time, closes discharge port, and jump and hold
Row step S4；
180 ° of S4, drive response unit rotational, and jump and execute step S5；
Material is added to second plate basket in S5, opening discharge port, after the first specified time, closes discharge port, and jump and hold
Row step S6；
S6, reaction chamber is vacuumized by the second vacuum orifice, until reacting indoor pressure reaches the second specified pressure, simultaneously
Start heater, until reaction room temperature reaches the first assigned temperature, and jumps and execute step S7；
S7, inert gas is passed through to reaction chamber by air inlet, until beating after the indoor pressure of reaction reaches third specified pressure
Port is outputed, and starts heater, until reacting indoor temperature reaches the second assigned temperature, and jumps and executes step S8；
S8, the first power supply of starting apply 0.6V voltage to first anode basket and the first collection pit, while starting second source to the
Two anode baskets and third collection pit apply 2V voltage, and jump and execute step S9；
S9, after the second specified time, 180 ° of drive response unit rotational so that the first power supply is to second plate basket and the 4th
Collection pit applies 0.6V voltage, second source and applies 2V voltage to first anode basket and the second collection pit, and jumps execution step
S10；
S10, after the second specified time, close the first power supply and second source, 180 ° of drive response unit rotational, and jump
Execute step S8.
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| CN107858709B (en) * | 2017-12-14 | 2019-08-06 | 东莞理工学院 | A kind of fused salt electrolysis apparatus preparing metal mixed powder |
| CN110656357B (en) * | 2019-08-22 | 2020-12-18 | 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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