CN104342560B - A kind of metallurgical composite slag one step reduction obtains molten iron and the technique of sulfonium phase - Google Patents
A kind of metallurgical composite slag one step reduction obtains molten iron and the technique of sulfonium phase Download PDFInfo
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- CN104342560B CN104342560B CN201410542165.1A CN201410542165A CN104342560B CN 104342560 B CN104342560 B CN 104342560B CN 201410542165 A CN201410542165 A CN 201410542165A CN 104342560 B CN104342560 B CN 104342560B
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- ferrum
- slag
- sulfonium
- molten iron
- copper
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000002893 slag Substances 0.000 title claims abstract description 30
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 24
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 230000009467 reduction Effects 0.000 title claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 20
- 238000011084 recovery Methods 0.000 claims abstract description 16
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005453 pelletization Methods 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 37
- 229910052802 copper Inorganic materials 0.000 claims description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 34
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 239000000571 coke Substances 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 238000004073 vulcanization Methods 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000005255 carburizing Methods 0.000 claims description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 2
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000013589 supplement Substances 0.000 claims description 2
- 239000000446 fuel Substances 0.000 claims 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009851 ferrous metallurgy Methods 0.000 abstract description 2
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 10
- 239000002956 ash Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 6
- 239000003245 coal Substances 0.000 description 3
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000006124 Pilkington process Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- 241000722270 Regulus Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical group 0.000 description 1
- 229910052784 alkaline earth metal Chemical group 0.000 description 1
- 150000001342 alkaline earth metals Chemical group 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
Classifications
-
- 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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- Manufacture And Refinement Of Metals (AREA)
Abstract
A kind of metallurgical composite slag one step reduction obtains molten iron and the technique of sulfonium phase, belongs to Ferrous Metallurgy and technical field of non-ferrous metallurgy.Relate to the separation and recovery that metallurgical composite slag is realized during molten point of reduction ferrum and non-ferrous metal.By allocating Calx into after levigate for metallurgy composite slag, carbonaceous reducing agent prepares carbonaceous pelletizing, realizes slag sulfonium ferrum three-phase layering, be separately recovered ferrum and non-ferrous metal after carbonaceous pelletizing direct-reduction in molten point of stove.This kind of technique can not only realize ferrum and separate with non-ferrous metal, moreover it is possible to non-ferrous metal is enriched in sulfonium mutually in, play the effect to multiple metallic element synthetical recovery.The stacking of metallurgical slag not only causes serious environmental problem, also creates the significant waste of resource, and this technique utilizes present situation by greatly change metallurgical slag, produces considerable economic benefit and social benefit, has broad application prospects.
Description
Technical field
The invention belongs to Ferrous Metallurgy and technical field of non-ferrous metallurgy, particularly relate to a kind of metallurgical composite slag one step also
The former technique obtaining molten iron and sulfonium phase, make in metallurgical composite slag the comprehensive reutilization of metallic element, particularly ferrum with
The reduction of non-ferrous metal copper, nickel etc. and separation and recovery.
Technical background
Pyrometallurgical smelting is topmost metallurgy of copper mode, and its copper yield accounts for the 80% of total copper yield, domestic even up to
97%, the copper ashes yield of ton copper is about 2.2t, and the quantity of slag is huge.Copper ashes ferrum, copper grade are respectively 30%～40% and
0.5%～2%, there is the highest recycling and be worth.The Iron grade of nickel slag is suitable with copper ashes, possibly together with 0.2%～0.7%
Nickel.
The Land use systems of copper ashes mainly includes pyrogenic process dilution and mill float glass process.The former reduces slag by reduction or sulfuration enrichment
In copper content, copper is recovered with the form of sulfide.Mill float glass process is a kind of physical treatment mode, can effectively return
Receive sulfide and the metal of copper, but invalid to oxide.Therefore, both the above method has selection to the recovery of copper
Property.Up to the present, the molten point mode of reduction is still that the process maximally effective means of copper ashes, but copper almost all enters
Molten iron forms copper-iron alloy, and both separate difficulty.Nickel is close with the character of copper, is easily formed ferronickel in reduction process
Alloy.There are some researches show, when carbon content forms the layering of molten iron and sulfonium in molten iron when reaching certain content, add
FeS-MS (M is alkali metal or alkaline-earth metal) flux can strengthen non-ferrous metal further between sulfonium with molten iron phase
Distribution ratio, promote non-ferrous metal separate with ferrum.
Summary of the invention
It is an object of the invention to provide a kind of metallurgical composite slag one step reduction and obtain molten iron and the technique of sulfonium phase, this work in skill, copper ashes, nickel slag is reduced with the form of carbonaceous pelletizing, molten point (molten point, be to complete after material melts completely Slag separates with melt) after obtain molten iron and sulfonium phase (copper matte regulus, nickel matte), and other trace non-ferrous metal element is rich Combine in sulfonium mutually in, it is achieved that the synthetical recovery of metal.
The present invention relates to during molten point of reduction, realize metallurgical composite slag the separation and recovery of ferrum and non-ferrous metal.Will
Allocate Calx into after metallurgical composite slag is levigate, carbonaceous reducing agent prepares carbonaceous pelletizing, molten after carbonaceous pelletizing direct-reduction
Realize slag-sulfonium-ferrum three-phase layering in dividing stove, be separately recovered ferrum and non-ferrous metal.This kind of technique can not only realize ferrum and have
The separation of non-ferrous metal, moreover it is possible to non-ferrous metal is enriched in sulfonium mutually in, play the effect to multiple metallic element synthetical recovery.
The stacking of metallurgical slag not only causes serious environmental problem, also creates the significant waste of resource, and this technique is by pole
Greatly change metallurgical slag utilizes present situation, produces considerable economic benefit and social benefit, before having wide application
Scape.
Metal-oxide and sulfide in composite slag are all reduced, and during molten point, molten iron is in the case of carbon is saturated
Realize the three-phase layering of slag-ferrum-sulfonium, and non-ferrous metal enrichment of element in sulfonium mutually in, reach metallic element is comprehensively returned
The purpose received.Concrete technology and the technical parameter controlled in process are as follows:
A carbonaceous pelletizing is reductase 12 0～30mins within the temperature range of 1250 DEG C～1300 DEG C, copper in composite slag, nickel,
The oxide of the elements such as ferrum and sulfide are reduced thoroughly:
Cu2S+CaO+C=2Cu+CO+CaS (1)
ΔGθ=116478-125T
Ni3S2+ 2CaO+2C=3Ni+2CO+2CaS (2)
ΔGθ=199376-250T
FeS+CaO+C=Fe+CO+CaS (3)
ΔGθ=141310-154T
Cu2O+C=2Cu+CO (4)
ΔGθ=57540-161T
NiO+C=Ni+CO (5)
ΔGθ=119062-171T
2FeO·SiO2+ 2CaO+2C=2Fe+2CO+2CaO SiO2 (6)
ΔGθ=209711-325T
B metallized pellet is molten within the temperature range of 1400 DEG C～1450 DEG C to be divided, it is achieved the separation that slag-ferrum is biphase；
C molten iron carburizing in the presence of having coke layer reaches saturated, and the sulfur in molten iron and carbon have alternative and formed
Fe-FeS two-phase, it is achieved ferrum, sulfonium separate；
The sulfide of the metals such as d copper, nickel is more higher than the sulfide stability of ferrum, and vulcanization reaction occurs
[FeS]+2 [Cu]=[Fe]+[Cu2S] (7)
2 [FeS]+3 [Ni]=2 [Fe]+[Ni3S2] (8)
The metal such as copper, nickel enters sulfonium phase, it is achieved non-ferrous metal separates with ferrum；
The raw material of the present invention reduces in the way of carbonaceous pelletizing, the existence of coke layer must be had to ensure in molten point of stove
The carbon content of molten iron, meanwhile, the sulfur part needed for vulcanization reaction comes from slag itself, and not enough part is by combustion
The sulfur that material strip enters supplements, and finally realizes the three-phase layering of slag-sulfonium-ferrum, reaches the purpose of comprehensive recovery of metallic elements.
Accompanying drawing explanation
Fig. 1 is copper ashes, the reduction of nickel slag one step, molten divisional processing flow chart.
Fig. 2 is the liquidus curve of FeS-MS binary system.
Fig. 3 is three-phase metallurgy principle schematic diagram.
Detailed description of the invention
Embodiment 1
Yunnan granulated copper slag, TFe content is 40.57%, and copper content is 0.75%, and natural alkalinity is 0.15.By copper
Slag is ground to granularity less than the powder of 0.125mm, and prepares basicity after adding a certain amount of Calx and coal blending and be
The carbonaceous pelletizing of 1.0.It is dried 4h in the carbonaceous pelletizing prepared is placed in 200 DEG C of baking ovens, puts into tubular electric resistance afterwards
In stove 1400 DEG C, graphite crucible inside holding 40mins carry out molten point.The granulated iron quality obtained after weighing molten point, really
Determine the recovery rate of ferrum, determined the copper content of sample by chemical titration analysis.Analysis result shows, when basicity is 1.0
The recovery rate of ferrum increases with the prolongation of temperature retention time, and reaching recovery rate during 40mins is 91%, granulated iron copper content with
The prolongation of temperature retention time and reduce, be reduced to 0.4% during 40mins, in molten iron, the removal efficiency of copper is close to 80%.
Embodiment 2
Jiangyin copper ashes, TFe content is 42.94%, and copper content is 0.69%, and natural alkalinity is 0.07.By river copper ashes
It is ground to granularity less than the powder of 0.125mm, and prepares carbonaceous pelletizing after adding a certain amount of Calx and coal blending.
The carbonaceous pelletizing prepared is placed in 200 DEG C of baking ovens and is dried 4h, put into afterwards tube type resistance furnace 1400 DEG C,
Graphite crucible inside holding 40mins carries out molten point.The granulated iron quality obtained after weighing molten point, determines the recovery rate of ferrum,
The copper content of sample is determined by chemical titration analysis.Analysis result shows, when basicity is 1.0, the recovery rate of ferrum is
92.3%, granulated iron copper content is reduced to 0.38%, and in molten iron, the removal efficiency of copper is more than 75%.
Embodiment 3
The nickelic slag in Jinchang, TFe content is 32.97%, and nickel content is 0.639%, and natural alkalinity is 0.59.By copper ashes
It is ground to granularity less than the powder of 0.125mm, and prepares carbonaceous pelletizing after adding a certain amount of Calx and coal blending.
The carbonaceous pelletizing prepared is placed in 200 DEG C of baking ovens and is dried 4h, put into afterwards tube type resistance furnace 1400 DEG C,
Graphite crucible inside holding 40mins carries out molten point.The granulated iron quality obtained after weighing molten point, determines the recovery rate of ferrum,
The nickel content of sample is determined by chemical titration analysis.Analysis result shows, when basicity is 1.0, the recovery rate of ferrum is
88%, granulated iron nickel content is reduced to 0.21%, and in molten iron, the removal efficiency of nickel is 85%.
Claims (2)
1. metallurgical composite slag one step reduction obtains molten iron and the technique of sulfonium phase, it is characterised in that technique and in work
The technical parameter controlled in skill is as follows:
A carbonaceous pelletizing is reductase 12 0～30mins within the temperature range of 1250 DEG C～1300 DEG C, copper in composite slag, nickel,
The oxide of ferrum element and sulfide are reduced thoroughly:
Cu2S+CaO+C=2Cu+CO+CaS (1)
ΔGθ=116478-125T
Ni3S2+ 2CaO+2C=3Ni+2CO+2CaS (2)
ΔGθ=199376-250T
FeS+CaO+C=Fe+CO+CaS (3)
ΔGθ=141310-154T
Cu2O+C=2Cu+CO (4)
ΔGθ=57540-161T
NiO+C=Ni+CO (5)
ΔGθ=119062-171T
2FeO·SiO2+ 2CaO+2C=2Fe+2CO+2CaO SiO2 (6)
ΔGθ=209711-325T
B metallized pellet is molten within the temperature range of 1400 DEG C～1450 DEG C to be divided, it is achieved the separation that slag-ferrum is biphase；
C molten iron carburizing in the presence of having coke layer reaches saturated, and the sulfur in molten iron and carbon have alternative and formed
Fe-FeS two-phase, it is achieved ferrum, sulfonium separate；
D copper, nickel metal sulfide more higher than the sulfide stability of ferrum, occur vulcanization reaction
[FeS]+2 [Cu]=[Fe]+[Cu2S] (7)
2 [FeS]+3 [Ni]=2 [Fe]+[Ni3S2] (8)
Copper, nickel metal enter sulfonium phase, it is achieved non-ferrous metal separates with ferrum.
Method the most according to claim 1, it is characterised in that raw material reduces in the way of carbonaceous pelletizing,
The existence of coke layer must be had in molten point of stove to ensure the carbon content of molten iron, meanwhile, the sulfur part needed for vulcanization reaction
Coming from slag itself, the sulfur that not enough part is brought into by fuel supplements, and finally realizes the three-phase layering of slag-sulfonium-ferrum,
Reach the purpose of comprehensive recovery of metallic elements.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107151743A (en) * | 2017-04-25 | 2017-09-12 | 昆明理工大学 | A kind of pyrite vulcanization corronil waste material makes copper matte regulus and the method for reclaiming dilval |
| CN107641718A (en) * | 2017-10-10 | 2018-01-30 | 东北大学 | A kind of method by the nickeliferous mixing slag production with iron |
| CN107699702A (en) * | 2017-10-10 | 2018-02-16 | 东北大学 | A kind of method that valuable component is reclaimed by cupric slag |
| CN109055720B (en) * | 2018-09-06 | 2019-10-25 | 钢研晟华科技股份有限公司 | A method of iron powder is prepared based on the modified copper ashes with cryogenic vulcanization reduction of alkaline process |
| CN110205432B (en) * | 2019-05-15 | 2020-12-25 | 昆明理工大学 | Method for producing iron-sulfur alloy |
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| CN103627835A (en) * | 2013-11-12 | 2014-03-12 | 金川集团股份有限公司 | Method for treating nickel smelting furnace slag |
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