CN105177635A - System and method for continuously preparing tungsten powder - Google Patents
System and method for continuously preparing tungsten powder Download PDFInfo
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- CN105177635A CN105177635A CN201510580529.XA CN201510580529A CN105177635A CN 105177635 A CN105177635 A CN 105177635A CN 201510580529 A CN201510580529 A CN 201510580529A CN 105177635 A CN105177635 A CN 105177635A
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Abstract
The invention discloses a system and method for continuously preparing tungsten powder. The system comprises an electrolytic cell, a perforated graphite anode basket, an anode charging port, a cathode charging port, a liquid phase cathode conducting disc, a liquid zinc cathode, a sliding turnover plate, an electrolytic cell supporting rod, a ball valve collecting opening, a collecting crucible, vacuumizing openings, air inlets, exhaust outlets, an oxygen blowing opening and an openable discharging door. A product and anode mud are effectively separated by using liquid zinc as the cathode, and continuous recovery of waste hard alloy can be achieved by updating an electrolytic anode, an electrolytic cathode and fused salt through the cathode charging port, the anode charging port, the sliding turnover plate and the oxygen blowing opening. The system and method have the characteristics that the obtained product is high in purity, the craft process is continuous, and repeated heating and cooling are avoided.
Description
Technical field:
The present invention relates to a kind of system and method for continuous production tungsten powder.The present invention can realize utilizing molten salt electrochemistry method continuous production tungsten powder, supplements raw material at the working temperature, collects product, belong to molten salt electrochemistry field.
Background technology:
Wimet is the material with high rigidity, high-flexural strength be made up through powder metallurgy process of the carbide of refractory metals tungsten and matrix metal, and it is widely used in fields such as machinofacture, mining, communications and transportation, energy exploration, building decorations.But refractory metals tungsten and rare metal cobalt are the very important strategic elements of generally acknowledging in the world, on raising national economy, military competition power, there is very important impact.Though China is tungsten resource big country, due to long-term excessively coyoting, managerial confusion, the tungsten ore resource of China is on the verge of exhaustion.More alarming is that China's cobalt resource is very short, and a large amount of import will be leaned on every year to maintain needs, and these have threatened the Sustainable development of Cemented Carbide Industry all largely.At present, the tungsten resource of the whole world more than 50% is for the manufacture of Wimet, and the W content in scrap hard alloy just reaches 74%-91%, China annual consumption tungsten metal about 2.7 ten thousand t, if the rate of recovery can reach 40%, for setting up Resources Guarantee System and promoting that recycling economy development is significant.
Be applied to industrialized Wimet renovation process and have tens kinds, long flow process and short route can be divided into by complex process degree.Long flow and method mainly comprises nitre method, method for smelting sodium sulfate, chlorination process, mineral acid lixiviation process etc., and these methods mostly comprise hydrometallurgy and complicated chemical process, make its process comparatively numerous and diverse, and economic benefit is poor.Current people more favor and reclaim Wimet in use abbreviated system, are wherein applied to that abbreviated system both domestic and external mainly comprises pyroprocessing method, mechanical crushing method, zinc melt method, electrochemical process and oxidation reduction process.
The advantage that pyroprocessing method has that technical process is short, coordinative composition of equipments is simple, carbide alloy mixture that is that reclaim is cleaner, little to the pollution level of environment, but also exist that energy consumption is high, inferior position that the loss through volatilization of hot stage cobalt, reclaimed materials are only suitable for doing macrocrystalline tungstenalloy.And utilize mechanical crushing method to reclaim high-quality Wimet, except needing abundant recovery experience, skill and good fragmentation and abrasive blast equipment, also need accurately analytical technology, Cemented Carbide Properties test set and compound sintering time to the strict control of its carbon balance and the clear understanding etc. to shrinking percentage, WC crystalline perfection.Although electrochemical process solves the problem of anode passivation by improving electrolyzer, but there is significant limitation in electrochemical process, cannot process the waste hand alloy material of cobalt contents less than 8%, and this method can consume a large amount of chemical feedstocks, produce the pollution that a series of objectionable impurities easily causes environment.
Fused salt electrolysis process is by electrochemical method in the ionogen of melting salt, restores pure metal tungsten on the working electrode (s or obtains alloy product.Under metallurgical industry demand for development short route, low cost, eco-friendly megatrend, fused salt electrolysis process takies few owing to having device resource preparing in metal and alloy thereof, technological operation is simple, receives much concern to unique advantages such as the side effect of environment are little simultaneously.Chinese invention patent CN104018190A (day for announcing 2014.9.03) proposes a kind of method that molten salt electrochemistry method reclaims hard alloy scraps, it achieves the preparation of the dissolving of hard alloy scraps and tungsten, cobalt dust, but have ignored the process of anode sludge C, and continuous print electrolysis production can not be realized due to the limitation of device.
Summary of the invention:
The object of the invention is to avoid the problems referred to above, a kind of system and method for continuous production tungsten powder is provided.Realize the convenient separation of the reasonable process of antianode mud, the recycling of fused salt and resultant.
A system for continuous production tungsten powder, is characterized in that comprising:
Electrolyzer, graphite anode basket with holes, anode charging opening, negative electrode charging opening, liquid cathode conductive plate, liquid Zn negative electrode, slip turnover panel, electrolyzer support bar, ball valve are collected mouth, are collected crucible, lower vacuum orifice, lower inlet mouth, lower venting port, oxygen blast mouth, can folding discharge door, upper vacuum orifice, enterprising gas port, upper venting port;
Upper vacuum orifice, enterprising gas port, upper venting port are arranged on the top of feed compartment; Anode charging opening is arranged on the top of graphite anode basket with holes, and is provided with slip turnover panel between the two, and negative electrode charging opening is arranged on above electrolyzer, and is provided with another block slip turnover panel between the two; Two pieces of slip turnover panel symmetric designs, are respectively used to control the connected sum of anode charging opening between graphite anode basket with holes and close; Close for the connected sum between negative electrode charging opening and electrolyzer; Have liquid Zn negative electrode, liquid cathode conductive plate and ball valve to collect mouth in electrolyzer, ball valve is collected below mouth and is placed with collection crucible; The below of electrolyzer also includes lower vacuum orifice, lower inlet mouth, lower venting port, oxygen blast mouth;
Wherein, graphite anode basket with holes, anode charging opening and the wire extended to outside stove form electrolytic anode, liquid cathode conductive plate, liquid cathode and the wire extended to outside stove form electrolysis cathode, and ball valve is collected mouth, collects crucible, can be formed product collecting device by folding discharge door.
Further, described slip turnover panel comprises fixed rotating shaft, slide link and slide block; Fixed rotating shaft rotating band movable slider slides, and slip turnover panel is opened or closed.
Further, the liquid cathode guide electroplax of described system is made up of nickel plate.
Apply the method for described system, it is characterized in that: supplement anode scrap hard alloy and liquid cathode by slip reprint; Collect mouth by ball valve to process in liquid cathode and product collection to collection crucible in order to further; By reacting remaining carbon to fused salt oxygen blast process to remove, complete the renewal to fused salt; Continuous electrolysis is completed by supplementary anode scrap hard alloy, zinc negative electrode and fused salt.
5, application rights requires the method for system described in 1, it is characterized in that step comprises:
1) scrap hard alloy waste material drops in graphite anode basket with holes, and zinc drops in fused salt as liquid cathode;
2) utilize 750 DEG C of NaCl-KCl fused salt 3V constant voltages to carry out electrolysis to scrap hard alloy, and make tungsten, cobalt dust deposits in liquid cathode;
3) utilize leakage fluid dram liquid Zn and product to be discharged, and collect product;
4) carbon remaining in fused salt is purified by oxygen blown mode; In oxygen blast operation steps, when venting port gas detection is oxycarbide, proved response is completely, need continue oxygen blast; When venting port gas detection is pure oxygen, proved response is complete, and carbon has been removed totally.
5) by adding scrap hard alloy and zinc, the repetition of said process is completed.
Can realize continuous electrolysis scrap hard alloy by said system, its detailed process is as follows:
1, NaCl-KCl heats up after down to 750 degrees Celsius in argon shield; vacuum drying giving up will be carried out in advance and add anode charging opening 103 with regard to Wimet; the zinc granule carrying out vacuum drying treatment is in advance added negative electrode charging opening 104; and by 107 slip turnover panels, scrap hard alloy being dropped in graphite anode basket 102 with holes, zinc granule drops in electrolyzer 101.Because zinc fusing point is low and than great, melt after entering electrolyzer 101 and be sunken to bottom by liquid cathode conductive plate formation liquid cathode.
2, apply 3.0V bath voltage at anode and cathode two ends and carry out potentiostatic deposition, tungsten in scrap hard alloy under electrochemical action in the form of an ion stripping and in liquid cathode deposition become tungsten powder, because tungsten proportion is greater than zinc, therefore tungsten powder is sunken to bottom liquid cathode.The anode peat participated in scrap hard alloy, because proportion is little, is suspended in fused salt or on liquid cathode and does not enter liquid Zn inside.
3, after electrolysis completes, slowly open ball valve collection mouth 109 and liquid cathode and tungsten powder product are discharged in collection crucible 110, cathode product can be taken out by folding discharge door 115 by side, and collects tungsten powder by steaming zinc method.
4, by oxygen blast mouth 114 to the inner oxygen blast of electrolyzer 101, the carbon of consumption reaction remnants.After oxygen blast completes, fused salt restPoses, and continues to add scrap hard alloy, zinc granule and NaCl-KCl powder and supplements fused salt amount, will carry out in atmosphere furnace vacuumizing and changing protection of inert gas afterwards, to complete circulation continuous electrolysis.
Advantage of the present invention is mainly reflected in:
1, the present invention adopts liquid cathode, and availability difference makes the anode sludge separate with product.When avoiding the existing of the anode sludge, product purity is low, affects the equal defect of product thing.Present system, by feed in raw material reprint, liquid cathode discharge of folding collecting mouth and the oxygen blast carbon removal treatment to fused salt, completes the continuous electrolysis to scrap hard alloy.At high temperature, by renewal anode waste material, renewal liquid cathode, renewal fused salt, the circulation that product completes whole technological process can be collected.Solve Electrolytic need heat up cooling wait repeat troublesome operation, prepared the high purity tungsten that mean particle size is 200nm.
Accompanying drawing illustrates:
Fig. 1 is the main TV structure schematic diagram of the present invention.
Number in the figure: 101 electrolyzers, 102 graphite anode baskets with holes, 103 anode charging openings, 104 negative electrode charging openings, 105 liquid cathode conductive plates, 106 liquid Zn negative electrodes, 107 slip turnover panels, 108 electrolyzer support bars, 109 ball valves collect that mouths, 110 collect crucibles, 111 times vacuum orifices, 112 times inlet mouths, 113 times venting ports, 114 oxygen blast mouths, 115 can folding discharge door, upper vacuum orifice 116, enterprising gas port 117, upper venting port 118.
Fig. 2 is feed compartment structural representation.
Number in the figure: 201 feed compartments, anode charging opening 103, negative electrode charging opening 104, slip turnover panel 107, fixed rotating shaft 202, slide link 203, slide block 204, upper vacuum orifice 116, enterprising gas port 117, upper venting port 118.
Be the open mode of slip turnover panel on the left of Fig. 2, right side is the closing condition of slip turnover panel.Two turnover panel synchronous workings during operation.For left side turnover panel: when opening, fixed rotating shaft 202 rotates clockwise band movable slider 204 and moves to the left, and slip turnover panel 107 is opened; During closedown, fixed rotating shaft 202 rotates counterclockwise, and band movable slider 204 moves to the right, and slip turnover panel 107 is closed.
Fig. 3 is the product X RD and SEM photo that adopt conventional cathode to obtain, can find out in product to there is carbon impurity and tungsten carbon compound.
Fig. 4 is the product X RD and SEM photo that adopt liquid cathode to obtain, can find out that product is single tungsten, and pattern is even.
Embodiment:
According to accompanying drawing, the present invention will be described below.
A system for continuous production tungsten powder, it comprises: electrolyzer 101, graphite anode basket with holes 102, anode charging opening 103, negative electrode charging opening 104, liquid cathode conductive plate 105, liquid Zn negative electrode 106, slip turnover panel 107, electrolyzer support bar 108, ball valve collect mouth 109, collect crucible 110, lower vacuum orifice 111, lower inlet mouth 112, lower venting port 113, oxygen blast mouth 114, can folding discharge door 115, upper vacuum orifice 116, enterprising gas port 117, upper venting port 118.
Wherein feed compartment comprises: feed compartment 201, anode charging opening 103, negative electrode charging opening 104, slip turnover panel 107, fixed rotating shaft 202, slide link 203, slide block 204, upper vacuum orifice 116, enterprising gas port 117, upper venting port 118.
By in atmosphere heating furnace, slidably turnover panel 107 and the electrolyzer 101 with ball valve collection mouth 109, bottom belt oxygen blast mouth 114 are formed described system.Wherein, graphite anode basket 102 with holes, anode charging opening 103 and the wire extended to outside stove form electrolytic anode; liquid cathode conductive plate 105, liquid cathode 106 and the wire extended to outside stove form electrolysis cathode; ball valve is collected mouth 109, collects crucible 110, can be formed product collecting device by folding discharge door 115, and lower vacuum orifice 111, lower inlet mouth 112, lower venting port 113, oxygen blast mouth 114 complete the operating process of vacuum in atmospheric resistance furnace, protection of inert gas, oxidizing atmosphere de-carbon jointly.Wherein oxygen blast mouth stove the inner is connected with bottom of electrolytic tank gas permeable brick, can directly to electrolyte bath oxygen blast.
Fig. 1 is whole system structural front view, atmospheric resistance furnace temperature rise rate used 10 DEG C/min, maximum heating temperature 1600 DEG C.NaCl, KCl 500g altogether that the mol ratio of carrying out combination drying is in advance 1:1 will be loaded in electrolyzer.Be evacuated in stove by lower vacuum orifice 111; and be warming up to 300 DEG C of insulations and make it to take off planar water for 2 hours; pass into argon gas by lower inlet mouth 112 and open lower venting port 113 and make to be full of protection of inert gas in stove, and be warming up to 850 DEG C of insulations and make NaCl, KCl melting and fully mix for 1 hour.Be cooled to 750 DEG C of preparations and carry out electrolysis.
Fig. 2 is feed compartment structural representation; open feed compartment upper cover; the scrap hard alloy carrying out processed is in advance added in anode charging opening 103, the zinc granule carrying out processed is in advance added in negative electrode charging opening; close feed compartment upper cover; by upper vacuum orifice 116 by the state that is evacuated in feed compartment; and add protection of inert gas by enterprising gas port 117, open venting port 118.Open slip turnover panel 107, make scrap hard alloy fall into graphite anode basket 102 with holes, zinc granule falls into electrolyzer 101 and forms liquid cathode.
Utilize D.C. regulated power supply between anode and cathode, apply 3.0V bath voltage electrolysis 10 hours, tungsten stripping become tungsten simple substance at liquid Zn negative electrode 106 surface deposition in the form of an ion in anode under electrochemical action, and owing to sinking to further bottom liquid cathode than great.The anode peat produced in electrolytic process, because proportion is little, is suspended in that fused salt is inner and liquid cathode is surperficial, can not enters liquid Zn cathode internal.
To be electrolysed complete after, repeat addition step, continue to add scrap hard alloy in anode basket.
Said process circulates after 3 times, slowly opens ball valve and collects mouth 109, the liquid Zn containing tungsten product is flowed in collection crucible 110, and opens and can be taken out by folding discharge door 115.And then by steaming zinc process, obtaining product tungsten and reclaiming zinc.
By oxygen blast mouth 114 to the oxygen 30 minutes of the electrolyte bath amount of blowing up with the carbon except dereaction remnants, vacuumize by lower vacuum orifice 111 and pass into argon gas by lower inlet mouth 112 and complete protection of inert gas.And mistake input zinc granule supplements liquid cathode all, supplements fused salt by the NaCl-KCl dropping into 1:1 mol ratio, the circulation completing negative electrode and fused salt upgrades.
Claims (5)
1. a system for continuous production tungsten powder, is characterized in that comprising:
Electrolyzer, graphite anode basket with holes, anode charging opening, negative electrode charging opening, liquid cathode conductive plate, liquid Zn negative electrode, slip turnover panel, electrolyzer support bar, ball valve are collected mouth, are collected crucible, lower vacuum orifice, lower inlet mouth, lower venting port, oxygen blast mouth, can folding discharge door, upper vacuum orifice, enterprising gas port, upper venting port;
Upper vacuum orifice, enterprising gas port, upper venting port are arranged on the top of feed compartment; Anode charging opening is arranged on the top of graphite anode basket with holes, and is provided with slip turnover panel between the two, and negative electrode charging opening is arranged on above electrolyzer, and is provided with another block slip turnover panel between the two; Two pieces of slip turnover panel symmetric designs, are respectively used to control the connected sum of anode charging opening between graphite anode basket with holes and close; Close for the connected sum between negative electrode charging opening and electrolyzer; Have liquid Zn negative electrode, liquid cathode conductive plate and ball valve to collect mouth in electrolyzer, ball valve is collected below mouth and is placed with collection crucible; The below of electrolyzer also includes lower vacuum orifice, lower inlet mouth, lower venting port, oxygen blast mouth;
Wherein, graphite anode basket with holes, anode charging opening and the wire extended to outside stove form electrolytic anode, liquid cathode conductive plate, liquid cathode and the wire extended to outside stove form electrolysis cathode, and ball valve is collected mouth, collects crucible, can be formed product collecting device by folding discharge door.
2. the system of a kind of continuous production tungsten powder according to claim 1, is characterized in that: described slip turnover panel comprises fixed rotating shaft, slide link and slide block; Fixed rotating shaft rotating band movable slider slides, and slip turnover panel is opened or closed.
3. the system of a kind of continuous production tungsten powder according to claim 1, is characterized in that: the liquid cathode guide electroplax of described system is made up of nickel plate.
4. application rights requires the method for system described in 1, it is characterized in that: supplement anode scrap hard alloy and liquid cathode by slip reprint; Collect mouth by ball valve to process in liquid cathode and product collection to collection crucible in order to further; By reacting remaining carbon to fused salt oxygen blast process to remove, complete the renewal to fused salt; Continuous electrolysis is completed by supplementary anode scrap hard alloy, zinc negative electrode and fused salt.
5. application rights requires the method for system described in 1, it is characterized in that step comprises:
1) scrap hard alloy waste material drops in graphite anode basket with holes, and zinc drops in fused salt as liquid cathode;
2) utilize 750 DEG C of NaCl-KCl fused salt 3V constant voltages to carry out electrolysis to scrap hard alloy, and make tungsten, cobalt dust deposits in liquid cathode;
3) utilize leakage fluid dram liquid Zn and product to be discharged, and collect product;
4) carbon remaining in fused salt is purified by oxygen blown mode;
5) add scrap hard alloy and zinc, repeat said process.
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| CN107513730A (en) * | 2017-08-31 | 2017-12-26 | 北京工业大学 | The continuous device and method for preparing tungsten powder and cobalt powder |
| CN108048879A (en) * | 2017-12-14 | 2018-05-18 | 东莞理工学院 | A kind of electrolytic preparation device for the metal powder for being capable of separation of solid and liquid |
| 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 |
| CN112281190A (en) * | 2020-10-12 | 2021-01-29 | 郑州大学 | Electrochemical method for preparing molybdenum metal by utilizing molybdenum disulfide |
| CN114059103A (en) * | 2021-11-15 | 2022-02-18 | 中南大学 | Method for recovering tungsten carbide and cobalt from waste hard alloy |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108048879A (en) * | 2017-12-14 | 2018-05-18 | 东莞理工学院 | A kind of electrolytic preparation device for the metal powder for being capable of separation of solid and liquid |
| 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 |
| CN112281190A (en) * | 2020-10-12 | 2021-01-29 | 郑州大学 | Electrochemical method for preparing molybdenum metal by utilizing molybdenum disulfide |
| CN112281190B (en) * | 2020-10-12 | 2021-11-05 | 郑州大学 | Electrochemical method for preparing molybdenum metal by utilizing molybdenum disulfide |
| CN114059103A (en) * | 2021-11-15 | 2022-02-18 | 中南大学 | Method for recovering tungsten carbide and cobalt from waste hard alloy |
| CN114059103B (en) * | 2021-11-15 | 2023-08-15 | 中南大学 | Method for recovering tungsten carbide and cobalt from waste hard alloy |
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