CN108977664B - The method for recycling tungsten carbide and cobalt in scrap hard alloy - Google Patents
The method for recycling tungsten carbide and cobalt in scrap hard alloy Download PDFInfo
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- CN108977664B CN108977664B CN201810819409.4A CN201810819409A CN108977664B CN 108977664 B CN108977664 B CN 108977664B CN 201810819409 A CN201810819409 A CN 201810819409A CN 108977664 B CN108977664 B CN 108977664B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum carbides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
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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
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
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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
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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
- C25C7/06—Operating or servicing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a kind of methods of tungsten carbide and cobalt in recycling scrap hard alloy, comprising steps of melting and is cooled to bulk alloy to being completely melt after scrap hard alloy is mixed with graphite and metallic cobalt；Using the bulk alloy as anode, graphite plate or conductive metal sheet as cathode, Electrochemical Stripping is carried out in acidic electrolysis bath, obtains tungsten carbide in anode later, obtains cobalt in cathode.This method is less prone to anodic passivity in electrolytic process, and realizes the recycling of tungsten carbide and cobalt.
Description
Technical field
The present invention relates to the recovery technology fields of scrap hard alloy, more particularly in a kind of recycling scrap hard alloy
The method of tungsten carbide and cobalt.
Background technique
Hard alloy is widely used in cutter material due to the advantages that its hardness is high, intensity is good, heat-and corrosion-resistant, such as bores
Head, lathe tool, milling cutter are also used for cutting cast iron, non-ferrous metal, plastics, and are applied to shield machine bit tool.By compositional classification
The smooth niobium series hard alloy (YW) of tungsten-cobalt series hard alloy (YG), kennametal (YT), tungsten titanium can be divided into.According to shape
Classification can be divided into spherical, rodlike, plate.Binding metal therein may have one or more of cobalt, nickel, iron, and content is from nothing
0% content of bonding hard alloy is differed to 20%, has nanocrystalline, Ultra-fine Grained, sub-micro brilliant, thin again according to grain size
Several different hard alloy such as brilliant, middle crystalline substance, coarse-grain, super coarse-grain.Also by the methods of chemical vapor deposition (CVD) in hard
Alloy surface covers wear-resisting or antioxidant coating (TiC/Al2O3) hard alloy cutter.Common Hard alloy has tens
Kind, and the trade mark of different manufacturers production is unified not to the utmost, type reaches several hundred thousands of kinds.Due to scrap hard alloy structure and element
Multifarious, this brings certain difficulty to recycling scrap hard alloy.
There are mainly two types of the methods of common recycling scrap hard alloy, will one is element therein is all aoxidized
Tungsten becomes tungstenic solution, such as nitre method, vulcanized sodium smelting process, high-temperature air oxidation method, is recycled back into the life of former tungsten carbide
APT is extracted in production. art, removal of impurities, is carried out reduction and carbonization and is produced tungsten carbide；Another kind is to dissolve Binder Phase, directly obtains carbonization
Tungsten powder, such as molten lixiviation process of acid, zinc melt the methods of method, electrochemical dissolution.Second class method flow is short, and especially electrochemistry selects
Property dissolution be a kind of effective ways for recycling scrap hard alloy, but with the dissolution of Binder Phase in course of dissolution, surface holds
Carbide layers are easily formed, so that anodic passivity, the metals such as internal cobalt, nickel are difficult to further dissolve out, and leaching process is difficult to continue, low
The hard alloy of Binder Phase content is more difficult.To solve the problems, such as to remove hard alloy scraps surface carbonation tungsten layer, people in time
Mechanical ball mill etc. outside several electrolysis installations, including titanium/tantalum rotary drum anode, slot is devised, principle is essentially continued with Mechanical Method
Surface carbonation tungsten layer is destroyed, new carbide surface is exposed, carries out course of dissolution constantly.Such method can be to a certain degree
It is upper to solve the problems, such as anodic passivity, but that there are still anodes is easy to wear, device structure is complicated, and be still difficult to handle low Binder Phase useless
The problem of old hard alloy.
In addition to complicated and diversified hard alloy type, the problems such as anodic passivity, the impurity brought into tungsten carbide use process
Also certain difficulty is brought to recycling scrap hard alloy.In intermetallic composite coating, in addition to bring iron, there are also be brazed what cutter head introduced
Copper；Geology cutter head but will introduce mineralogical composition, such as aluminium oxide/calcium.No matter which kind of recovery method is used, it is miscellaneous how to remove these
Matter should be all taken into account.
Summary of the invention
In order to solve the technical issues of above-mentioned electrolysis processing scrap hard alloy is easy to produce anodic passivity in the process, this hair
It is bright to propose a kind of method for recycling tungsten carbide and cobalt in scrap hard alloy.
Technical problem of the invention is resolved by technical solution below:
A kind of method of tungsten carbide and cobalt in recycling scrap hard alloy, comprising steps of by scrap hard alloy and graphite
With melting after metallic cobalt mixing to being completely melt, and it is cooled to bulk alloy；
Using the bulk alloy as anode, graphite plate or conductive metal sheet as cathode, carried out in acidic electrolysis bath
Electrochemical Stripping obtains tungsten carbide in anode later, obtains cobalt in cathode.
Preferably, the graphite is powdered graphite；And/or the metallic cobalt includes cobalt powder and/or blocky cobalt.
Preferably, the temperature of the melting is 1200-1700 DEG C.
Preferably, the time of the melting is 10-50 minutes.
Preferably, the acidic electrolysis bath is acidity CoCl2Electrolyte.
It is highly preferred that the acidity CoCl2The concentration of electrolyte is 0.5-2mol/L, pH value 0-6.
It preferably, further include mixing the tungsten carbide of anode with graphite after carrying out Electrochemical Stripping in acidic electrolysis bath
Object is closed to be separated.
It is highly preferred that the tungsten carbide of anode is separated in a manner of flotation with graphite mixture.
Preferably, the scrap hard alloy includes WC-Co series hard alloy；WC-Co series hard alloy is preferably YG8 hard
Matter alloy.
Preferably, the mass ratio of the scrap hard alloy and the graphite and the metallic cobalt is 1:0.01-0.05:
0.5-1。
In a preferred embodiment, a kind of method for recycling tungsten carbide and cobalt in scrap hard alloy is proposed, comprising steps of
Melting is to completely molten after WC-Co series hard alloy is mixed with graphite and metallic cobalt according to mass ratio 1:0.01-0.05:0.5-1
Change, and is cooled to bulk alloy.Wherein, the graphite is powdered graphite；The metallic cobalt is cobalt powder and/or blocky cobalt；It is described
The temperature of melting is 1200-1700 DEG C；The time of the melting is 10-50 minutes.
Using the bulk alloy as anode, graphite plate or conductive metal sheet as cathode, carried out in acidic electrolysis bath
Electrochemical Stripping, obtains tungsten carbide in anode, obtains cobalt in cathode.Wherein, the acidic electrolysis bath is acidity CoCl2Electrolysis
Liquid；The acidity CoCl2The concentration of electrolyte is 0.5-2mol/L, pH value 0-6；It is molten that electrochemistry is carried out in acidic electrolysis bath
It further include separating the tungsten carbide of anode with graphite mixture after out；The tungsten carbide of anode and graphite mixture is excellent
Choosing is separated in a manner of flotation.
The beneficial effect of the present invention compared with the prior art includes: after mixing scrap hard alloy with graphite and metallic cobalt
Melting is to being completely melt, graphite can ensure carbon saturation to prevent the oxidation of tungsten carbide, while tungsten carbide during melting
From melting to that can crystallize during being cooled to bulk alloy, interval ensures tungsten carbide crystalline substance between the addition of cobalt expands tungsten carbide crystal grain
Body can independent growths so that other metal impurities are not carbonized tungsten and are coated, bulk alloy carries out electrification as anode later
When learning dissolution, the metal impurities not being wrapped by can be dissolved out into acidic electrolysis bath, and the process of dissolution will not be because of tungsten carbide
Cladding generates anodic passivity phenomenon, so that anode can remove the remaining tungsten carbide for being mixed with graphite of metal impurities, graphite plate or
Conductive metal sheet obtains cobalt as cathode, in cathode, and therefore, this method is less prone to anodic passivity in electrolytic process, and real
The recycling of tungsten carbide and cobalt is showed.
Detailed description of the invention
Fig. 1 is the method flow schematic diagram of tungsten carbide and cobalt in present invention recycling scrap hard alloy.
Fig. 2 is the micro- electron microscope of alloy after melting in embodiment 1.
Fig. 3 is the micro- electron microscope of anode slime after being electrolysed in embodiment 1.
Fig. 4 is the micro- electron microscope of the tungsten-carbide powder obtained in embodiment 1.
Fig. 5 is the heavy cobalt figure of cathode after being electrolysed in embodiment 1.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing 1-5 to this hair
Bright specific embodiment is described in detail.Many details are explained in the following description in order to fully understand this
Invention.But the invention can be embodied in many other ways as described herein, those skilled in the art can be
Without prejudice to doing similar improvement in the case where intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Embodiment 1
The present embodiment proposes a kind of method for recycling tungsten carbide and cobalt in scrap hard alloy, comprising steps of
Waste and old YG8 hard alloy is mixed with graphite, metallic cobalt block according to the mass ratio of 28:1:28, corundum earthenware is put into
In crucible, the melting in intermediate frequency vacuum induction furnace, heating power 10kW, temperature is 1600~1700 DEG C, continuous heating 30min
Natural cooling afterwards obtains and takes out molten alloy block (i.e. bulk alloy).As shown in Fig. 2, the alloy after melting is irregular shape
Shape.
Use conventional DC power supply as electrolysis power, tank voltage 1.0V, electrolyte is the CoCl of 2mol/L2Solution, electricity
The pH value for solving liquid is 0.2, and above-mentioned alloy block is electrolysed as anode, titanium sheet as cathode.It is obtained largely after electrolysis from anode
Anode slime is deposited with cobalt on cathode.As shown in figure 3, anode slime there is also other in addition to there is a particle of triangular prism shape not
The little particle of rule.As shown in figure 5, the cobalt of 8cm or so length is deposited on cathode, these cobalt recoverables, as melting
Preceding metal cobalt raw material is added.
Anode slime is the mixture of graphite and tungsten carbide, is separated graphite with tungsten carbide by way of flotation, is dried
Pure macrocrystalline tungsten carbide powder is obtained afterwards.As shown in figure 4, the tungsten carbide particle structural integrity in the tungsten-carbide powder, has
Triangular prism shape crystal morphology is adapted as the raw materials for production of coarse-grain hard alloy without obvious microscopic defect.In conjunction with Fig. 3, it is known that
Irregular little particle in Fig. 3 is by isolated graphite.
Embodiment 2
The present embodiment proposes a kind of method for recycling tungsten carbide and cobalt in scrap hard alloy, comprising steps of
Waste and old YG8 hard alloy is mixed with graphite, metallic cobalt block according to the mass ratio of 42:1:27, corundum is transferred to
In crucible, the melting in intermediate frequency vacuum induction furnace, heating power 10kW, temperature is 1600~1700 DEG C, continuous heating
Natural cooling after 30min obtains and takes out molten alloy block.
Use conventional DC power supply as electrolysis power, tank voltage 1.0V, electrolyte is the CoCl of 2mol/L2Solution, electricity
The pH value for solving liquid is 0.2, and above-mentioned alloy block is as anode, and titanium sheet is as cathode.A large amount of anode slimes are obtained from anode after electrolysis,
It deposited metallic cobalt on cathode.
Anode slime is the mixture of graphite and tungsten carbide (WC), is separated graphite with tungsten carbide by way of flotation,
Pure macrocrystalline tungsten carbide powder is obtained after drying.Tungsten carbide particle structural integrity in the tungsten-carbide powder has triangular prism
Shape crystal morphology is adapted as the raw materials for production of coarse-grain hard alloy without obvious microscopic defect.
Can be used as general tungsten carbide powder after the pure macrocrystalline tungsten carbide powder crushing and screening that above-described embodiment obtains makes
With.
It should be noted that relative to standard hydrogen electrode current potential, Co2+Standard electrode EMF are as follows: -0.28V similarly may be used
It is respectively as follows: Ni to find other metal ions relative to the standard electrode EMF of standard hydrogen electrode current potential2+For -0.257V, Cr2+
For -0.913V, Cu2+For 0.342V, Fe2+For -0.447V, Zn2+For -0.7618V.If ion concentration is identical, in same electrolysis
In liquid, then cathode sedimentary sequence are as follows: Cu > Ni > Co > Fe > Zn > Cr.And in the present invention, the major metal cation of electrolyte is
Co2+, wherein Cu2+With Ni2+Concentration it is very low, therefore Co can be precipitated first, to obtain cobalt in cathode.Certainly, with impurity
It accumulates, the concentration impurity ion in solution can increase, especially Cu2+And Ni2+, electrolyte removal of impurities processing must be just carried out at this time.
The mode of electrolyte removal of impurities has the cobalt electrolysis process that can much use for reference maturation in the prior art.
In recycling scrap hard alloy proposed by the present invention in the method for tungsten carbide and cobalt, whole flow process need to only be added on a small quantity
Graphite, and cobalt and part graphite can be recycled；The foreign metals such as iron/titanium/aluminium/copper/nickel in hard alloy can be
It is enriched in electrolyte；Anodic passivity phenomenon is less prone in electrolytic process；The advantages that product is the tungsten carbide and cobalt of high value.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Each technical characteristic of embodiment described above can carry out arbitrarily
Combination, for simplicity of description, it is not all possible to each technical characteristic in above-described embodiment combination be all described, so
And as long as there is no contradiction in the combination of these technical features, it all should be considered as described in this specification.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those skilled in the art to which the present invention belongs, it is not taking off
Under the premise of from present inventive concept, several equivalent substitute or obvious modifications can also be made, and performance or use is identical, all answered
When being considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of method of tungsten carbide and cobalt in recycling scrap hard alloy, which is characterized in that comprising steps of waste and old hard is closed
Melting is to being completely melt after gold is mixed with graphite and metallic cobalt, and is cooled to bulk alloy；Using the bulk alloy as anode,
Graphite plate or conductive metal sheet carry out Electrochemical Stripping as cathode in acidic electrolysis bath, obtain tungsten carbide in anode later,
Cobalt is obtained in cathode.
2. the method as described in claim 1, which is characterized in that the graphite is powdered graphite；And/or the metallic cobalt is
Cobalt powder and/or blocky cobalt.
3. the method as described in claim 1, which is characterized in that the temperature of the melting is 1200-1700 DEG C.
4. the method as described in claim 1, which is characterized in that the time of the melting is 10-50 minutes.
5. the method as described in claim 1, which is characterized in that the acidic electrolysis bath is acidity CoCl2Electrolyte.
6. method as claimed in claim 5, which is characterized in that the acidity CoCl2The concentration of electrolyte is 0.5-2mol/L,
PH value is 0-6.
7. the method as described in claim 1, which is characterized in that after carrying out Electrochemical Stripping in acidic electrolysis bath, also wrap
It includes and separates the tungsten carbide of anode with graphite mixture.
8. the method as described in claim 1, which is characterized in that by the tungsten carbide of anode and graphite mixture in a manner of flotation
It is separated.
9. the method as described in claim 1, which is characterized in that the scrap hard alloy includes WC-Co series hard alloy.
10. the method as described in claim 1, which is characterized in that the scrap hard alloy and the graphite and the metal
The mass ratio of cobalt is 1:0.01-0.05:0.5-1.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111575567B (en) * | 2020-04-09 | 2021-07-20 | 江西理工大学 | Regeneration method of waste high-cobalt coarse-grain hard alloy |
| CN111500829B (en) * | 2020-04-27 | 2021-10-29 | 厦门钨业股份有限公司 | Method for quenching and recycling 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 |
| CN114645296A (en) * | 2022-04-21 | 2022-06-21 | 湖北绿钨资源循环有限公司 | Method for recycling tungsten carbide by electrolyzing waste hard alloy under assistance of ultrasonic waves |
| CN114934296A (en) * | 2022-04-21 | 2022-08-23 | 湖北绿钨资源循环有限公司 | Method for recycling tungsten carbide by electrolyzing waste hard alloy under assistance of aeration |
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