CN102719681B - Decarbonization method of nickel or nickel alloy recovery smelting - Google Patents
Decarbonization method of nickel or nickel alloy recovery smelting Download PDFInfo
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- CN102719681B CN102719681B CN2012102463812A CN201210246381A CN102719681B CN 102719681 B CN102719681 B CN 102719681B CN 2012102463812 A CN2012102463812 A CN 2012102463812A CN 201210246381 A CN201210246381 A CN 201210246381A CN 102719681 B CN102719681 B CN 102719681B
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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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- 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
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Abstract
The invention discloses a decarbonization method of nickel or nickel alloy recovery smelting, which solves the problems that secondary pollution is easily caused, other alloy elements in nickel ingot are oxidized and can not be removed and the like in the recovery smelting of nickel and nickel alloy waste in the prior art. The method includes the recovered nickel or nickel alloy waste and a vacuum induction furnace and is technically characterized by comprising the following steps of: putting the waste into the crucible of the vacuum induction furnace; after the waste is completely molten, measuring the carbon content in the nickel or nickel alloy melt; adding the calcined foam nickel of the required mass to remove redundant carbon in the nickel or nickel alloy melt; refining to remove impurities by electromagnetic stirring, and discharging the generated CO by vacuum degassing; and casting after the carbon content in the nickel or nickel alloy melt reaches the standard value so as to form a cast ingot of which the carbon content reaches the standard. The method disclosed by the invention has reasonable flow design, is simple to operate, and prevents secondary pollution; the decarbonization raw materials are easily available; and the standard requirements of other element chemical components are completely met while obviously improving the melt decarbonization effect.
Description
Technical field
The present invention relates to the production method of the old material recycling of a kind of nickel and nickelalloy, particularly a kind of main employing nickel foam reclaims to nickel or the nickelalloy of nickel and the old material of nickelalloy (comprising waste material, reclaimed materials, tailing etc.) recycling the decarbonization method of smelting, and belongs to refining of metal removal of impurities field.
Background technology
In the prior art, nickel foam is a kind of novel metallic substance.It has tridimensional network, the characteristics such as namely its porosity is high, specific surface area is large, the easy filling of active substance; Compare with common nickel plate, because its specific surface area is large, not only the oxygen of surface adsorption is many with the material of volume, and the oxide compound that forms after calcination is also many.Nickel foam is mainly used in battery electrode material, fuel cell, catalystic material etc., specifically applies as follows:
1. battery electrode material
Nickel foam is mainly used in battery electrode material, is used in particular for the NiMH battery, and this rechargeable cell is widely used in laptop computer, mobile phone, Electric Scooter, electric bicycle, hybrid vehicle etc.
2. fuel cell
The common working temperature of molten carbonate fuel cell is between 550-700 ℃, and nickel foam can become the eelctro-catalyst of molten carbonate fuel cell.Nickel foam can be used for that the two poles of the earth pole plate in proton exchange membrane electrogenesis pond (PEMFC) is material modified, the electrode interconnecting feeder of Solid Oxide Fuel Cell (SOFC), electrolysis electrode materials (as in water electrolysis agent environment).
3. catalystic material
Nickel foam has unique tridimensional network characteristics, makes it become the support of the catalyst of automobile catalyst transmodulator, catalyticcombustion, diesel vehicle exhaust cleaner.During engine cold-start, carbon monoxide and hydrocarbon polymer transform, and due to heat conduction property, the foamed nickel catalyst agent carrier may be superior to ceramic catalyst carrier.On this meaning, nickel foam can be compared with the high temperaturesteel support of the catalyst or be more superior than high temperaturesteel support of the catalyst.
4. other application
Nickel foam also can be used for filter material, processes the magnetic current conductor of magnetic particle in fluid.Other application comprises and is applied to store up hydrogen medium, heat-exchange medium etc.
Have no nickel foam through retrieval and be used for the report of nickel and the old material processing of nickelalloy.
Nickel and nickelalloy, because having good machinery, the performance such as anticorrosion and anti-corrosion, have been widely used in space flight, military project and special dimension., because the nickel high price is expensive,, so often use aborning the old material of nickel and nickelalloy (comprising waste material, reclaimed materials, tailing) to carry out recycling,, to reduce production costs, increase economic efficiency.But,, because old material surface generally all is stained with greasy dirt or is subject to the impact of the factor such as environmental pollution,, therefore cause the carbon content severe overweight of old material,, if do not carry out the carbonization treatment smelting that directly feeds intake after reclaiming, can't produce qualified product.
The de-carbon method of existing nickel and the old material of nickelalloy mainly contains:
1, alkali cleaning facture
The machine oil, the turning liquid that add process due to nickel and the old material remained on surface of nickelalloy machine, raise carbon content, utilize the method for alkali cleaning can remove the oil on surface, turning liquid etc., but this kind method is easy to cause secondary pollution, and operation is also inconvenient.
2, oxide treatment method
Nickel and the old material of nickelalloy are put in electric furnace and are heated to more than 600 ℃, make the carbonizations such as machine oil, turning liquid, the CO of generation, CO
2Vapor away.Although this kind method can be removed most of unnecessary carbon, also there will be some other problems simultaneously, as the oxidized formation oxide compound slag inclusion likely of other alloying element in the nickel ingot, then during melting except not going still can't produce qualified product.
For this reason, the decarbonization method that must find the old material recovery of a kind of nickel and nickelalloy smelting solves this problem.
Summary of the invention
The purpose of this invention is to provide a kind of nickel or nickelalloy and reclaim the decarbonization method of smelting, solved nickel and nickelalloy old material in the prior art reclaim smelt exist easily cause secondary pollution, in the nickel ingot during the oxidized melting again of other alloying element except the problem such as not going.Process design of the present invention is reasonable, and is simple to operate, non-secondary pollution, and decarburization raw material used is easy to get, and when significantly improving melt de-carbon effect, meets the standard-required of other element chemistry composition fully.
The technical solution adopted in the present invention is: the crucible of described old material being put into vacuum induction furnace, after whole old material fusings, measure the carbon content in nickel or nickelalloy melt, according to detected carbon superscale,, adding the nickel foam after calcination is processed of requirement in containing the crucible of melt, with surface, with the nickel foam of oxide film, remove unnecessary carbon in nickel or nickelalloy melt; Described nickel foam after calcination is processed, through 800-1200 ℃ of calcination, makes the nickel foam surface form 1-3 μ m nickel oxide, and the nickel foam oxygen level after calcination is controlled at 2 wt %-10 wt %; The thickness of the described nickel foam after calcination is processed is 1-80mm, and aperture is 0.1-10mm, and porosity is 60-98%, through-hole rate is 〉=98%, volume density is 0.1-1.2g/cm3, absorption 1 wt %-8 wt % oxygen, and the hole count on per inch length is 5-130 PPI; In the de-carbon process, adopt induction stirring refining removal of impurities, the CO that produces to be discharged through vacuum stripping, reaction is carried out chemical composition and is detected online after finishing, and casts after the carbon content in nickel or nickelalloy melt reaches standard value, forms carbon content ingot casting up to standard; The method of calculation of required nickel foam after calcination is processed are: first determine the superscale of carbon in nickel or nickelalloy melt, according to the superscale of carbon, determine the oxygen level that needs, select afterwards oxygen level to meet the requirements of nickel foam and join in alloy melt.
Characteristics and positively effect that the present invention has are: because the present invention adopts vacuum induction furnace, first whole nickel or the old material of nickelalloy are melted in crucible in fusion process,, if carbon content exceeds standard, add the nickel foam after calcination is processed of requirement to carry out carbonization treatment in the crucible that contains melt immediately.The decarbonization process flow scheme design of its smelting is reasonable, adds surface to contain the nickel foam of nickel oxide simple to operate, and non-secondary pollution, thereby with low cost, has obtained nickel up to standard and Ni alloy ingot, and in ingot casting, carbon content can reach 0.01-0.30wt%.
In addition, the nickel foam of decarburization used only requires to meet national standard, and the producer of most of production nickel foam all can provide, and raw material is easy to get.The nickel foam calcination is processed also very simple, only need to be with nickel foam at 800-1200 ℃ of lower high-temperature calcination, can make the nickel foam surface form 1-3 μ m nickel oxide layer, general resistance furnace all can meet the calcination requirement, and the nickel foam oxygen level after calcination is controlled in 2 wt %-10 wt % scopes.
Due to after nickel or the old material of nickelalloy be fused into melt, carry out immediately carbonization treatment, this moment, melt did not also add other alloying element to carry out alloying, the main component of melt is the impurity of nickel and minute quantity, although other element chemistry composition in melt has some fluctuations in carbon rejection process, but fluctuation range is minimum, all in the scope that standard allows, does not affect the standard-required of other element chemistry composition.
Nickel foam is used for nickel in the present invention and decarburization is carried out in the old material recovery of nickelalloy smelting, realizes the old material of nickel and nickelalloy (comprising waste material, reclaimed materials, tailing) recycling.Therefore, the present invention compared with prior art, has significantly improved nickel and nickelalloy melt de-carbon effect.It solved nickel and the old material of nickelalloy in the prior art reclaim smelt exist easily cause in secondary pollution, nickel ingot other alloying element likely during oxidized melting again except the problem such as not going, thereby effectively reduce in nickel and nickelalloy melt carbon content and reach standard value, to meet the requirement that improves material purity.
Embodiment
Describe the specific embodiment of the invention method in detail below in conjunction with embodiment.This nickel or nickelalloy reclaim the decarbonization method of smelting and comprise nickel or the old material of nickelalloy and the vacuum induction furnace of recovery.Its concrete operation step is as follows:
The old material of the nickel that one, first will reclaim or nickelalloy is put into the crucible of vacuum induction furnace, after whole old material fusings, measure the carbon content in nickel or nickelalloy melt, according to detected carbon superscale, add in containing the crucible of melt the nickel foam after calcination is processed that needs quality remove nickel or nickelalloy melt in unnecessary carbon.
The operation steps of the nickel foam through the calcination processing used is: nickel foam is put into general resistance furnace,, through 800-1200 ℃ of calcination, make the nickel foam surface form 1-3 μ m nickel oxide, the nickel foam oxygen level after calcination is controlled in 2 wt %-10 wt % scopes.The thickness of the nickel foam of processing through calcination is 1-80mm, and aperture is 0.1-10mm, and porosity is 60-98%, and through-hole rate be 〉=98%, and volume density is 0.1-1.2g/cm3, adsorbs 1 wt %-8 wt % oxygen, and the hole count on per inch length is 5-130PPI.
Two, when nickel foam being used for nickel and nickelalloy melt smelting de-carbon, adopt induction stirring refining removal of impurities, the CO that produces is discharged through vacuum stripping.
Three, after the reaction of de-carbon, vacuum exhaust finishes, carry out chemical composition and detect online, cast after the carbon content in nickel or nickelalloy melt reaches standard value, form ingot casting up to standard.
With general nickel metallographic phase ratio, porosity and the specific surface area of nickel foam are large, thereby with the contact area of nickel or nickelalloy melt, greatly increase, and by the NiO of surface oxidation and the oxygen of absorption thereof and the carbon in nickel or nickelalloy melt, fully react, and reaction formula is as follows:
NiO+C→Ni+CO↑；
O
2+2C→2CO↑
When nickel or nickelalloy melt de-carbon, the method of calculation of required nickel foam after calcination is processed are: the superscale of first determining carbon in nickel or nickelalloy melt, determine the oxygen level that needs according to the superscale of carbon, select afterwards oxygen level to meet the requirements of nickel foam and join in alloy melt and go to get final product.Specifically can determine by following two kinds of methods:
Method one: computing method
A certain amount of nickel foam through the calcination aftertreatment is put into the material alloying chamber of vacuum induction furnace, until melt, all do not measured carbon component before alloying after fusing.If carbon content exceeds standard, calculate the quality of the nickel foam that need to add according to the data that detect, the nickel foam that will need after calculating is disposable to add in the vacuum induction furnace crucible that contains melt.Adopt induction stirring and vacuum stripping in the de-carbon process, carry out chemical composition after reaction finishes and detect online, the qualified rear casting of composition.
Method two: observation
A certain amount of nickel foam of processing through calcination is put into the material alloying chamber of vacuum induction furnace, until melt, all do not measured carbon component before alloying after fusing.If carbon content exceeds standard, with nickel foam adding in the vacuum induction furnace crucible that contains melt of a little several times.While just adding nickel foam, because the more chemical reaction of carbon content is strong, liquation seethes with excitement, magic flower.Along with constantly adding of nickel foam, carbon is consumed by reaction gradually, and the CO of generation also reduces gradually, and liquation boiling, phenomenon of turning over flower weaken gradually, until melt liquid level is tending towards tranquil.Bubbles volume stops adding nickel foam seldom the time,, so can judge according to the growing amount of bubble the de-carbon situation of melt, after online detection chemical composition is qualified, can stop adding nickel foam.
Embodiment 1
1 ton of Yin Kenaier 718 alloy cast ingot of melting, put into the Yin Kenaier 718 old material of alloy that reclaim in the crucible of vacuum induction furnace, smelts the concrete operation step of decarburization as mentioned above.Wherein
Chemical composition (massfraction %) required value and measured value are as follows:
Refining finishes to carry out the 1st chemical composition and detects online, and carbon content exceeds standard 0.012%.
In the present embodiment, the nickel foam specification is: thickness 1mm, and aperture 0.1mm, porosity 98%, through-hole rate 98%, volume density 0.176g/cm3, absorption 8Wt% oxygen, top layer contains the 3um nickel oxide.Wherein, the density of nickel oxide is 6.67g/cm
3The method of calculating required nickel foam is as follows:
1) carbon amount: the 1000 * 0.012%=0.12Kg that exceeds standard;
2) need NiO amount: 0.12/12 * (16+58)=0.74Kg; (wherein 12 is the nucleidic mass of carbon; 16 is the nucleidic mass of oxygen; 58 is the nucleidic mass of nickel)
3), if only with nickel oxide, carry out de-carbon, need nickel oxide area S
1:
S
1=m/ ρ h; (wherein m is nickel oxide quality 0.74Kg, and ρ is the density 6.67g/cm of nickel oxide
3, h is nickel oxide thickness 3um).
S as calculated
1=37m
2,, because sheet material is two sides, add 18.5m
2Porous nickel mesh can meet the demands.
4) the general absorption in the nickel foam of this kind specification surface 8Wt% oxygen, participate in the de-carbon reaction equally.As only with the oxygen of absorption, removing unnecessary carbon, the nickel foam area S that needs
2:
0.176 * 1 * 10
-1* S
2* 8% * 12/16=120, (this kind specification nickel foam volume density 0.176g/cm3 wherein; Thickness 1mm; Absorption 8Wt% oxygen; 12 is the nucleidic mass of carbon; 16 is the nucleidic mass of oxygen; 120g is the carbon amount that exceeds standard)
Try to achieve nickel foam area S
2=11.4m
2,, because porous nickel mesh is two sides, add 5.7m
2Nickel foam sheet material can meet the demands.
The oxygen of the nickel oxide on nickel foam surface and it self absorption participates in the de-carbon reaction simultaneously, considers the nickel foam 5m that drops into this kind specification
2Can meet the de-carbon requirement, with 5m
2Nickel foam is carried out de-carbon disposable adding in alloy melt, carries out the 2nd chemical composition after de-carbon finishes and detects online, and (massfraction %) is as follows for detected result:
Be detected as online a minute qualified laggard row casting.
Embodiment 2
1 ton of Monel K500 alloy cast ingot of melting, put into the old material of Monel K500 that reclaims in the crucible of vacuum induction furnace, smelts the concrete operation step of decarburization as mentioned above.Wherein
Chemical composition (massfraction %) required value and measured value are as follows:
Refining finishes not add Mn, Ti, Al carries out carrying out the 1st chemical composition on-line analysis before alloying, finds that carbon content exceeds standard 0.033%.
In the present embodiment, the nickel foam specification is: thickness 2mm, and aperture 0.1mm, porosity 90%, through-hole rate 98%, volume density 0.88g/cm3, absorption 5Wt% oxygen, top layer contains the 3um nickel oxide.Wherein, the density of nickel oxide is 6.67g/cm
3Calculate required interpolation nickel foam method as follows:
1) carbon amount: the 1000 * 0.033%=0.33Kg that exceeds standard
2) need NiO amount: 0.33/12 * (16+58)=2.035Kg; (wherein 12 is the nucleidic mass of carbon; 16 is the nucleidic mass of oxygen; 58 is the nucleidic mass of nickel)
3), if only with nickel oxide, carry out de-carbon, need nickel oxide area S
1:
S
1=m/ ρ h; (wherein m is nickel oxide quality 2.035Kg, and ρ is the density 6.67g/cm of nickel oxide
3, h is nickel oxide thickness 3um)
S=101.7m as calculated
2,, because sheet material is two sides, add 51m
2Nickel foam sheet material can meet the demands.
4) the nickel foam surface adsorption 5Wt% oxygen of this kind specification, participate in the de-carbon reaction equally.As only with the oxygen of absorption, removing unnecessary carbon, the nickel foam area S that needs
2:
0.88 * 2 * 10
-1* S
2* 5% * 12/16=330; (this kind specification nickel foam volume density 0.88g/cm3 wherein; Thickness 2mm; Absorption 5Wt% oxygen; 12 is the nucleidic mass of carbon; 16 is the nucleidic mass of oxygen; 330g is the carbon amount that exceeds standard)
Try to achieve nickel foam area S
2=5m
2,, because porous nickel mesh is two sides, add 2.5m
2Porous nickel mesh can meet the demands.
The oxygen of the nickel oxide film that nickel foam has and it self absorption participates in the de-carbon reaction simultaneously, considers the nickel foam 2.5m that drops into this kind specification
2Can meet the de-carbon requirement.With 2.5m
2Nickel foam is carried out refining disposable adding in alloy melt, and after refining finishes, interpolation Mn, Ti, Al carry out alloying, carry out 2 chemical compositions before casting after alloying and detect online.Detected result (massfraction %) is as following table:
After chemical composition is qualified, meet the casting requirement, can cast.
Embodiment 3
1 ton of Monel K400 ingot casting of melting, put into the old material of Monel K400 that reclaims in the crucible of vacuum induction furnace, smelts the concrete operation step of decarburization as mentioned above.Wherein
Chemical composition (massfraction %) required value and measured value are as follows:
In the present embodiment, the nickel foam specification is: thickness 5mm, and aperture 0.1mm, porosity 85%, through-hole rate 98%, volume density 1.32g/cm3, absorption 3Wt% oxygen, top layer contains the 2um nickel oxide.
When the 1st time chemical composition detected online, carbon content exceeded standard 0.086%, need to carry out de-carbon.The nickel foam fritter that material alloying is indoor adds in crucible several times.While just adding nickel foam, because carbon content is more, chemical reaction is strong, liquation boiling, magic flower.Along with constantly adding of nickel foam, carbon is consumed by reaction gradually, and the CO of generation also reduces gradually, and liquation boiling, phenomenon of turning over flower weaken gradually, until melt liquid level is tending towards tranquil bubbles volume, stops adding nickel foam seldom the time.Carry out subsequently the 2nd chemistry and become to learn online the detection, (massfraction %) is as follows for detected result:
Chemical composition is qualified, meets the casting requirement, can cast.Practice shows, this kind de-carbon method meets production requirement, and is easy and simple to handle.
Claims (1)
1. a nickel or nickelalloy reclaim the decarbonization method of smelting, the nickel or the old material of nickelalloy and the vacuum induction furnace that comprise recovery, it is characterized in that: the crucible of described old material being put into vacuum induction furnace, after whole old material fusings, measure the carbon content in nickel or nickelalloy melt,, according to detected carbon superscale,, adding the nickel foam after calcination is processed of requirement in containing the crucible of melt, with surface, with the nickel foam of oxide film, remove unnecessary carbon in nickel or nickelalloy melt; Described nickel foam after calcination is processed, through 800-1200 ℃ of calcination, makes the nickel foam surface form 1-3 μ m nickel oxide, and the nickel foam oxygen level after calcination is controlled at 2 wt %-10 wt %; The thickness of the described nickel foam after calcination is processed is 1-80mm, and aperture is 0.1-10mm, and porosity is 60-98%, through-hole rate is 〉=98%, volume density is 0.1-1.2g/cm3, absorption 1 wt %-8 wt % oxygen, and the hole count on per inch length is 5-130 PPI; In the de-carbon process, adopt induction stirring refining removal of impurities, the CO that produces to be discharged through vacuum stripping, reaction is carried out chemical composition and is detected online after finishing, and casts after the carbon content in nickel or nickelalloy melt reaches standard value, forms carbon content ingot casting up to standard; The method of calculation of required nickel foam after calcination is processed are: first determine the superscale of carbon in nickel or nickelalloy melt, according to the superscale of carbon, determine the oxygen level that needs, select afterwards oxygen level to meet the requirements of nickel foam and join in alloy melt.
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| CN108929934B (en) * | 2018-07-03 | 2020-05-26 | 北京北冶功能材料有限公司 | Decarburization smelting method of iron-nickel alloy reclaimed material |
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| JP4059118B2 (en) * | 2003-03-24 | 2008-03-12 | Ｊｆｅスチール株式会社 | Method for producing Fe-Ni alloy cold rolled sheet material for shadow mask with excellent etching perforation |
| RU2271398C1 (en) * | 2004-06-01 | 2006-03-10 | ОАО "Институт Гипроникель" | Method of thermochemical treatment of nickel-plated polymer articles |
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