CN105586491A - Comprehensive recycling method for waste hard alloy - Google Patents
Comprehensive recycling method for waste hard alloy Download PDFInfo
- Publication number
- CN105586491A CN105586491A CN201610030639.3A CN201610030639A CN105586491A CN 105586491 A CN105586491 A CN 105586491A CN 201610030639 A CN201610030639 A CN 201610030639A CN 105586491 A CN105586491 A CN 105586491A
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- Prior art keywords
- hard alloy
- alloy
- scrap hard
- comprehensive recovering
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Classifications
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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
-
- 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
- C22B23/023—Obtaining nickel or cobalt by dry processes with formation of ferro-nickel or ferro-cobalt
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
-
- 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
Abstract
The invention provides a comprehensive recycling method for waste hard alloy. The method comprises the steps that pure iron blocks and the waste hard alloy are evenly mixed according to the mass ratio of (0.01-2):1; the evenly-mixed pure iron blocks and waste hard alloy are placed in a smelting furnace to be heated and molten, and alloy melt is formed; the alloy melt is atomized into fine liquid drops through an atomization device, and the liquid drops are condensed to form hard alloy powder; alkaline matter is added to the hard alloy powder for calcination, and a calcined material is formed; water is added to the calcined material for leaching, and a tungsten containing solution and iron and cobalt containing filter residues are obtained through filtering; the tungsten containing solution is purified and enriched, and a pure tungstate solution is obtained; and the iron and cobalt containing filter residues are dried and reduced, and iron-cobalt alloy is obtained. According to the method, the waste hard alloy can be effectively smashed, the aim of preparing powder is achieved, the process is simple, operation is convenient, and recycling cost is low.
Description
Technical field
The present invention relates to secondary resource and recycle and raw material crushing technology field, more specifically, relate toA kind of comprehensive recovering process of scrap hard alloy.
Background technology
Along with carbide alloy is in the growth of traditional field application and the expansion of new application, waste and old hard closesThe output of gold increases year by year, thereby effective recovery of scrap hard alloy becomes the focus of domestic and international research,Also be the important leverage that realizes hard carbide industry sustainable development.
At present, the main method that hard alloy scraps reclaims comprise the molten method of nitre method, zinc, mechanical crushing method,Electrochemical process, acid-soluble method and chloridising etc. But due to characteristics such as hardness is high, density large, good toughness,Carbide alloy is difficult to fragmentation and grinding. The methods such as nitre method, electrochemical process, acid-soluble method and chloridising reclaimCarbide alloy generally directly reacts alloy after preliminary fragmentation with chemical reagent, owing to not passing through and grindingMill, the specific area of carbide alloy is limited, and chemical reaction rate is very slow, and production efficiency is very low; Machinery is brokenBroken method has very high requirement to broken and milling apparatus, and crushing efficiency is low, milling time long (500h left and right),Energy consumption is very high, and is difficult to meet the requirements of granularity; The molten method of zinc is equivalent to add before Mechanical Crushing onePreprocessing process, obtain being easy to broken loose shape cemented carbide body, but it does not solve carbide alloy at allBe difficult to the problem of grinding, therefore production cost and energy consumption are higher, and removal process exists zinc pollution.
As can be seen here, how effectively the difficult point that scrap hard alloy reclaims and key point are fragmentation and grindMill obtains easy-to-handle cemented carbide powder, and conventional method is all difficult to reach this purpose at present.Therefore, need to provide a kind of new recovery method.
Summary of the invention
In view of the above problems, the object of this invention is to provide a kind of comprehensive recovering process of scrap hard alloy,Effectively broken worn-out carbide alloy, reaches the object of powder process, and technique is simple, easy to operate,Cost recovery is low.
The comprehensive recovering process that the invention provides a kind of scrap hard alloy, comprising:
By pure iron piece and scrap hard alloy in mass ratio 0.01～2:1 mix;
The pure iron piece mixing and scrap hard alloy are placed on to heat fused in smelting furnace, and formation is closedGold melt;
Described alloy melt is formed to tiny drop by atomising device atomization, shape after described Drop CondensationBecome cemented carbide powder;
In described cemented carbide powder, add alkaline matter roasting, form roasting material;
To the leaching that adds water in described roasting material, filter and obtain tungstenic solution and iron content, cobalt filter residue;
By described tungstenic solution purification, enrichment, obtain pure tungstate solution;
By described iron content, cobalt filter residue and drying, reduction, obtain ferrocobalt.
In addition, preferred scheme is that the pure iron piece mixing and scrap hard alloy are being placed on moltenIn furnace, in the process of heat fused, wherein, the temperature of described smelting furnace is 1450 DEG C～1700 DEG C, heatingTime is 0.5h～4h.
In addition, preferred scheme is that described atomising device comprises middle bottom pour ladle, nozzle and atomizing cup; ItsIn, described alloy melt enters described middle bottom pour ladle and enters into described nozzle by bottom discharge spout and is atomizedFor tiny drop, the condensation in described atomizing cup of described drop forms described cemented carbide powder.
In addition, preferred scheme is that atomization method comprises high pressure draught ballistic method, high pressure liquid stream ballistic methodAnd centrifugal process.
In addition, preferred scheme is, in the process that adds alkaline matter roasting in described cemented carbide powderIn, by described alkaline matter and cemented carbide powder in mass ratio 0.005～3:1 mix, at 400 DEG CRoasting 0.5～10h at～1000 DEG C, makes the metal in described carbide alloy be converted into corresponding oxide.
In addition, preferred scheme is that described alkaline matter comprises NaOH, magnesium hydroxide and hydroxideA kind of alkali in potassium or sodium carbonate, sodium acid carbonate, potash, saleratus, magnesium carbonate, magnesium bicarbonateIn a kind of basic salt.
In addition, preferred scheme is, in the process of leaching that adds water in described roasting material; Wherein,
Described roasting material evenly mixes by liquid-solid ratio 0.5～20:1 with described water, at 5 DEG C～95 DEG C, stirs and soaksGo out 0.1h～10h.
In addition, preferred scheme is, by described tungstenic solution purification, enrichment, to obtain pure wolframic acidIn the process of salting liquid, described tungstenic solution, by chemical method, ion-exchange and extraction, is removed itIn objectionable impurities and make the tungsten in solution be converted into ammonium salt form.
In addition, preferred scheme is, by described iron content, cobalt filter residue and drying, reduction, to obtain iron cobalt and closeIn the process of gold, add carbon dust to mix dry filter residue, at 400 DEG C～1000 DEG C reduction 15h～48h,Obtain described ferrocobalt.
From technical scheme above, the comprehensive recovering process of scrap hard alloy provided by the invention,There is following beneficial effect:
1) can with carbide alloy in tungsten form the pure iron piece of low-melting compound and add waste and old hard to and closeJin Zhong, significantly reduces the fusing point of mixture, improves the fusing effect of carbide alloy;
2) carbide alloy after fusing obtains cemented carbide powder through powder by atomization, can solve waste and old at presentThe broken difficult problem with grinding of carbide alloy, the more traditional fragmentation of the energy consumption of pulverizing process and cost, Ginding processObviously reduce;
3) the cemented carbide powder sodium carbonate roasting the water logging that obtain, make tungsten enter solution and with slag in cobalt andIron separates. Because carbide alloy is crushed into thinner powder, the reaction rate of roasting and leaching process addsHurry up, production efficiency improves greatly;
4) leach tungsten in the solution obtaining and exist with tungstate radicle anion, can be easily by purification enrichmentObtain pure tungstate solution. In leached mud, cobalt and iron mainly exist with the form of oxide, by going backFormer melting can directly obtain ferrocobalt.
5) invented technology method is simple, easy to operate, can be cost-effectively by carbide alloy powder process separationReclaim tungsten and cobalt wherein, the comprehensive cost recovery of tungsten cobalt is low, is suitable for industrial applications.
In order to realize above-mentioned and relevant object, one or more aspects of the present invention comprise below will be in detailThe feature that illustrates and particularly point out in the claims. Explanation and accompanying drawing below describe this in detailSome bright illustrative aspects. But what indicated these aspects only can use principle of the present inventionSome modes in variety of way. In addition, the present invention be intended to comprise all these aspects and they etc.Jljl.
Brief description of the drawings
By reference to the content below in conjunction with the description of the drawings and claims, and along with to the present inventionUnderstanding more comprehensively, other object of the present invention and result will more be understood and should be readily appreciated that. In the accompanying drawings:
Fig. 1 is the comprehensive recovering process schematic flow sheet according to the scrap hard alloy of the embodiment of the present invention.
In institute's drawings attached, identical label is indicated similar or corresponding feature or function.
Detailed description of the invention
In the following description, for purposes of illustration, for complete to one or more embodiment is providedFoliation solution, has set forth many details. But, clearly, can there is no these details yetSituation under realize these embodiment.
Below with reference to accompanying drawing, specific embodiments of the invention are described in detail.
For the comprehensive recovering process of scrap hard alloy provided by the invention is described, Fig. 1 shows basisThe comprehensive recovering process flow process of the scrap hard alloy of the embodiment of the present invention.
As shown in Figure 1, the comprehensive recovering process of scrap hard alloy provided by the invention comprises:
S110: by pure iron piece and scrap hard alloy in mass ratio 0.01～2:1 mix;
S120: the pure iron piece mixing and scrap hard alloy are placed on to heat fused in smelting furnace,Form alloy melt;
S130: described alloy melt is formed to tiny drop by atomising device atomization, and described drop is coldAfter solidifying, form cemented carbide powder;
S140: add alkaline matter roasting in described cemented carbide powder, form roasting material;
S150: to the leaching that adds water in described roasting material, filter and obtain tungstenic solution and iron content, cobalt filter residue;
S160: by described tungstenic solution purification, enrichment, obtain pure tungstate solution;
S170: by described iron content, cobalt filter residue and drying, reduction, obtain ferrocobalt.
The detailed process of the above-mentioned comprehensive recovering process for scrap hard alloy of the present invention, wherein, in stepIn S120, the pure iron piece mixing and scrap hard alloy being placed on to heat fused in smelting furnaceIn process, the temperature of smelting furnace is 1450 DEG C～1700 DEG C, and the heat time is 0.5h～4h.
In step S130, bottom pour ladle, nozzle and atomizing cup in the middle of atomising device comprises; Wherein, alloy is moltenBody enters middle bottom pour ladle and enters into nozzle by bottom discharge spout and is atomized as tiny drop, and drop is at mistChange condensation in cylinder and form described cemented carbide powder.
In step S130, it should be noted that, atomization method comprises high pressure draught ballistic method, high pressure liquidStream ballistic method and centrifugal process.
In step S140, adding in the process of alkaline matter roasting, by alkalescence in cemented carbide powderMaterial and cemented carbide powder in mass ratio 0.005～3:1 mix, roasting at 400 DEG C～1000 DEG C0.5～10h, makes the metal in carbide alloy be converted into corresponding oxide.
Wherein, alkaline matter comprises a kind of alkali or the carbonic acid in NaOH, magnesium hydroxide and potassium hydroxideA kind of basic salt in sodium, sodium acid carbonate, potash, saleratus, magnesium carbonate, magnesium bicarbonate.
In step S150, in the process of leaching that adds water in roasting material; Wherein, roasting material with described inWater evenly mixes by liquid-solid ratio 0.5～20:1, leaching 0.1h～10h at 5 DEG C～95 DEG C.
In step S160, by tungstenic solution purification, enrichment, obtain the mistake of pure tungstate solutionCheng Zhong, tungstenic solution is by chemical method, ion-exchange and extraction, removes objectionable impurities wherein alsoMake the tungsten in solution be converted into ammonium salt form.
In step S170, by iron content, cobalt filter residue and drying, reduction, obtain in the process of ferrocobalt,Add carbon dust to mix dry filter residue, at 400 DEG C～1000 DEG C reduction 15h～48h, obtain iron cobaltAlloy.
According to the comprehensive recovering process of above-mentioned scrap hard alloy in conjunction with real below specifically execute example, to thisBright being further described, following examples are intended to illustrate the present invention instead of limitation of the invention further.
Embodiment 1
Get useless WC-Co carbide alloy 500g, add Fe piece 100g, obtain at 1600 DEG C of heating 2hAlloy melt, the hard that alloy melt obtains average grain diameter < 0.06mm through high pressure liquid stream impact atomization method closesBronze end; The alloy powder obtaining is after 1:2.5 adds sodium carbonate to mix in mass ratio, roasting at 850 DEG CBurn 2h, the roasting material obtaining, roasting material and water mix by liquid-solid ratio 4:1 and leach at 90 DEG C1.5h, obtains after washing and filtering containing WO3Be less than 1.5% containing cobalt filter residue and sodium tungstate solution; Sodium tungstate is moltenLiquid is through chemical subtraction, Pro-concentration with ion exchange process and after transition, obtain pure ammonium tungstate solution; Dry containing cobalt filter residueAfter dry, 1:10 adds carbon dust at 850 DEG C of reduction 30h in mass ratio, obtains closing containing the Fe-Co of cobalt 40.3%Gold.
Embodiment 2
1:4 adds after Fe piece in useless WC-Co carbide alloy in mass ratio, at 1650 DEG C of heating 1.5h,The carbide alloy melt obtaining, then adopts high pressure liquid stream impact atomization method to obtain average grain diameter < 0.06mmCemented carbide powder; Get 200g cemented carbide powder, add 40g NaOH, roasting at 800 DEG CBurn 3h, obtain roasting material, roasting material and water mix by liquid-solid ratio 5:1, and leach 2.5h at 80 DEG C,After washing and filtering, obtain containing WO3Be less than 1.0% containing cobalt filter residue and sodium tungstate solution; Sodium tungstate solution is through changingAfter learning removal of impurities, solvent extraction and back extraction, obtain pure ammonium tungstate solution; Containing after cobalt filter residue and drying, by matterAmount adds carbon dust at 900 DEG C of reduction melting 24h than 1:8, obtains the Fe-Co alloy containing cobalt 37.5%.
Embodiment 3
Get useless WC-Co carbide alloy 500g, add Fe piece 80g, what obtain at 1550 DEG C of heating 2h is hardMatter alloy melt, alloy melt obtains the hard of average grain diameter < 0.074mm through high pressure draught impact atomization methodAlloy powder; Get 200g cemented carbide powder, add 125g sodium acid carbonate, roasting 3h at 800 DEG C,Obtain roasting material, roasting material and water mix by liquid-solid ratio 5:1, and leach 2h at 95 DEG C, washingAfter filtration, obtain containing WO3Be less than 0.95% containing cobalt filter residue and sodium tungstate solution; Sodium tungstate solution is through chemistryAfter removal of impurities, solvent extraction and back extraction, obtain pure ammonium tungstate solution; Containing after cobalt filter residue and drying, by qualityAdd coke at 800 DEG C of reduction melting 36h than 1:12, obtain the Fe-Co alloy containing cobalt 42.4%.
Can find out the comprehensive recovery side of scrap hard alloy provided by the invention by above-mentioned embodimentMethod, not only effective broken worn-out carbide alloy, reaches the object of powder process and recovery of the present inventionMethod is simple, easy to operate, and the comprehensive cost recovery of tungsten cobalt is low.
Combining of the scrap hard alloy that proposes according to the present invention described in the mode of example above with reference to accompanying drawingClose recovery method. But, it will be appreciated by those skilled in the art that propose for the invention described above uselessThe comprehensive recovering process of old carbide alloy can also be made various on the basis that does not depart from content of the present inventionImprove. Therefore, protection scope of the present invention should be determined by the content of appending claims.
Claims (9)
1. a comprehensive recovering process for scrap hard alloy, comprising:
By pure iron piece and scrap hard alloy in mass ratio 0.01～2:1 mix;
The pure iron piece mixing and scrap hard alloy are placed on to heat fused in smelting furnace, and formation is closedGold melt;
Described alloy melt is formed to tiny drop by atomising device atomization, shape after described Drop CondensationBecome cemented carbide powder;
In described cemented carbide powder, add alkaline matter roasting, form roasting material;
To the leaching that adds water in described roasting material, filter and obtain tungstenic solution and iron content, cobalt filter residue;
By described tungstenic solution purification, enrichment, obtain pure tungstate solution;
By described iron content, cobalt filter residue and drying, reduction, obtain ferrocobalt.
2. the comprehensive recovering process of scrap hard alloy as claimed in claim 1, wherein,
In the process that the pure iron piece mixing and scrap hard alloy is placed on to heat fused in smelting furnaceIn, wherein,
The temperature of described smelting furnace is 1450 DEG C～1700 DEG C, and the heat time is 0.5h～4h.
3. the comprehensive recovering process of scrap hard alloy as claimed in claim 1, wherein,
Bottom pour ladle, nozzle and atomizing cup in the middle of described atomising device comprises; Wherein,
Described alloy melt enters described middle bottom pour ladle and enters into described nozzle by bottom discharge spout and is atomizedFor tiny drop, the condensation in described atomizing cup of described drop forms described cemented carbide powder.
4. the comprehensive recovering process of the scrap hard alloy as described in claim 1 or 3, wherein,
Atomization method comprises high pressure draught ballistic method, high pressure liquid stream ballistic method and centrifugal process.
5. the comprehensive recovering process of scrap hard alloy as claimed in claim 1, wherein,
Adding in the process of alkaline matter roasting in described cemented carbide powder,
By described alkaline matter and cemented carbide powder in mass ratio 0.005～3:1 mix, at 400 DEG CRoasting 0.5～10h at～1000 DEG C, makes the metal in described carbide alloy be converted into corresponding oxide.
6. the comprehensive recovering process of the scrap hard alloy as described in claim 1 or 5, wherein,
Described alkaline matter comprise a kind of alkali in NaOH, magnesium hydroxide and potassium hydroxide or sodium carbonate,A kind of basic salt in sodium acid carbonate, potash, saleratus, magnesium carbonate, magnesium bicarbonate.
7. the comprehensive recovering process of scrap hard alloy as claimed in claim 1, wherein,
In the process of leaching that adds water in described roasting material; Wherein,
Described roasting material evenly mixes by liquid-solid ratio 0.5～20:1 with described water, at 5 DEG C～95 DEG C, stirs and soaksGo out 0.1h～10h.
8. the comprehensive recovering process of scrap hard alloy as claimed in claim 1, wherein,
By described tungstenic solution purification, enrichment, obtain in the process of pure tungstate solution,
Described tungstenic solution, by chemical method, ion-exchange and extraction, is removed objectionable impurities whereinAnd make the tungsten in solution be converted into ammonium salt form.
9. the comprehensive recovering process of scrap hard alloy as claimed in claim 1, wherein,
By described iron content, cobalt filter residue and drying, reduction, obtain in the process of ferrocobalt, by what be driedFilter residue adds carbon dust to mix, and at 400 DEG C～1000 DEG C reduction 15h～48h, obtains described ferrocobalt.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106435224A (en) * | 2016-08-17 | 2017-02-22 | 湖南金源新材料股份有限公司 | Method for preparing ammonium paratungstate from waste containing tungsten |
| CN108796226A (en) * | 2018-07-04 | 2018-11-13 | 赣州有色冶金研究所 | A method of it recycling alkali and soaks tungsten slag |
| CN111041208A (en) * | 2019-11-30 | 2020-04-21 | 福达合金材料股份有限公司 | Method for efficiently recycling copper and tungsten in copper-tungsten alloy waste |
| CN111575567A (en) * | 2020-04-09 | 2020-08-25 | 江西理工大学 | Regeneration method of waste high-cobalt coarse-grain hard alloy |
| CN117206531A (en) * | 2023-11-07 | 2023-12-12 | 崇义章源钨业股份有限公司 | Crushing method of waste solid hard alloy |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435224A (en) * | 2016-08-17 | 2017-02-22 | 湖南金源新材料股份有限公司 | Method for preparing ammonium paratungstate from waste containing tungsten |
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| CN111041208B (en) * | 2019-11-30 | 2021-06-22 | 福达合金材料股份有限公司 | Method for efficiently recycling copper and tungsten in copper-tungsten alloy waste |
| CN111575567A (en) * | 2020-04-09 | 2020-08-25 | 江西理工大学 | Regeneration method of waste high-cobalt coarse-grain hard alloy |
| CN117206531A (en) * | 2023-11-07 | 2023-12-12 | 崇义章源钨业股份有限公司 | Crushing method of waste solid hard alloy |
| CN117206531B (en) * | 2023-11-07 | 2024-02-27 | 崇义章源钨业股份有限公司 | Crushing method of waste solid hard alloy |
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