CN102134655A - Method for separating zinc and indium and iron from indium-enriched high-iron high-zinc calcine through reduction-magnetic separation - Google Patents
Method for separating zinc and indium and iron from indium-enriched high-iron high-zinc calcine through reduction-magnetic separation Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 239000011701 zinc Substances 0.000 title claims abstract description 90
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 85
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 63
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 62
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 57
- 238000007885 magnetic separation Methods 0.000 title claims abstract description 25
- 230000009467 reduction Effects 0.000 claims abstract description 30
- 239000012141 concentrate Substances 0.000 claims abstract description 29
- 230000002829 reductive effect Effects 0.000 claims abstract description 23
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims abstract description 22
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 7
- 239000002918 waste heat Substances 0.000 claims abstract description 5
- 238000006722 reduction reaction Methods 0.000 claims description 35
- 239000004576 sand Substances 0.000 claims description 25
- 238000001354 calcination Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 18
- MVSVDCKYOGFCCK-UHFFFAOYSA-N [Fe].[In].[Zn] Chemical compound [Fe].[In].[Zn] MVSVDCKYOGFCCK-UHFFFAOYSA-N 0.000 claims description 14
- 239000003034 coal gas Substances 0.000 claims description 14
- 230000005291 magnetic effect Effects 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- NJWNEWQMQCGRDO-UHFFFAOYSA-N indium zinc Chemical compound [Zn].[In] NJWNEWQMQCGRDO-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000006148 magnetic separator Substances 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 32
- 238000002386 leaching Methods 0.000 abstract description 19
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000002184 metal Substances 0.000 abstract description 12
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 8
- 239000011707 mineral Substances 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 8
- 238000003723 Smelting Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 40
- 229910052935 jarosite Inorganic materials 0.000 description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 19
- 238000005516 engineering process Methods 0.000 description 16
- 239000011787 zinc oxide Substances 0.000 description 15
- 230000007935 neutral effect Effects 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- 229910052984 zinc sulfide Inorganic materials 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000005083 Zinc sulfide Substances 0.000 description 7
- 239000002893 slag Substances 0.000 description 7
- 235000011149 sulphuric acid Nutrition 0.000 description 7
- 239000001117 sulphuric acid Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- -1 iron ion Chemical class 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 235000010755 mineral Nutrition 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 5
- 229960001763 zinc sulfate Drugs 0.000 description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 150000004965 peroxy acids Chemical class 0.000 description 4
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical class [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000009854 hydrometallurgy Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 3
- 238000004137 mechanical activation Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052598 goethite Inorganic materials 0.000 description 2
- 229910052595 hematite Inorganic materials 0.000 description 2
- 239000011019 hematite Substances 0.000 description 2
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052569 sulfide mineral Inorganic materials 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- 229910001656 zinc mineral Inorganic materials 0.000 description 1
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Abstract
The invention relates to a method for separating zinc and indium and iron from indium-enriched high-iron high-zinc calcine through reduction-magnetic separation, belonging to the technical field of mineral processing. The invention is characterized in that the method adopts the technical means that mineral dressing is combined with smelting and performs smelting firstly and mineral dressing secondly; and the method is as follows: the waste heat of the indium-enriched high-iron zinc calcine obtained through fluidized roasting is utilized, the indium-enriched high-iron zinc calcine is introduced to perform low-temperature weak reduction treatment at below 570 DEG C and ensure that zinc ferrite is decomposed and reduced to ZnO, Fe3O4 and iron, the reduced calcine is levigated to prepare slurry, and zinc and indium and iron is separated through wet-type magnetic separation to obtain iron ore concentrates and indium-enriched zinc- enriched ore concentrates. The method has low energy consumption and low dosage of a reducing agent, is simple in operation, easy in control and high in metal recovery rate. Therefore, the indium embedded and distributed in zinc ferrite can be released, the loss caused by the high temperature volatilization of indium can be avoided, and the zinc and indium and iron of the indium-enriched high-iron high-zinc calcine can be separated in an ore dressing manner before leaching.
Description
Technical field
The present invention relates to a kind of method of rich indium high ferro zinc baking sand reduction magnetic separation separation of Zinc indium iron, belong to technical field of mineral processing.
Background technology
Rich indium high ferro zinc baking sand is a kind of zinc metallurgical material that is rich in indium and a large amount of impurity irons that zinc sulfides concentrate bearing high content of indium and iron obtains after calcination process.Along with the development of Zinc hydrometallurgy process, the utilization of the complicated zinc mineral resource of low zinc grade, high impurity content is more and more general, the most obvious with the utilization of high-iron zinc sulfide concentrate especially.
High-iron zinc sulfide concentrate typically refers to iron content greater than 7.5wt%, contains zinc less than 48wt%, and sulfur-bearing is generally at 25～35wt%, and association has the general name of a class zinc sulfide concentrates of the indium metal of high level.For handling this class high-iron zinc sulfide concentrate, the Technology flow process that adopts has two kinds usually, and first kind of Technology flow process is that zinc ore concentrate fluidized bed roasting-neutrality leaches-neutral leached mud rotary kiln high temperature reduction volatilization.In this Technology flow process, zinc ore concentrate fluidized bed roasting purpose is 870～1100 ℃ of controlled temperature, elementary sulfur in the zinc ore concentrate is removed, obtain the roasted ore of sulfur-bearing hardly, simultaneously, under this roasting condition, the oxidized generation oxide compound of iron sulphide and zinc sulphide, iron and zinc are inlayed coexistence in the high-iron zinc sulfide concentrate, chemical reaction will take place in the ferric oxide and the zinc oxide that generate, generate zinc ferrite, thereby, in roasting process, most iron generates the wustite that is insoluble in dilution heat of sulfuric acid inevitably, as materials such as zinc ferrites, form a series of wustite sosoloid, and zinc ferrite is a kind of wustite of being leached by dilute sulphuric acid of being difficult to.The neutral purpose that leaches is to be dissolved in the sulphuric acid soln the zinc in the zinc roasted ore is most with dilute sulphuric acid, realize that metallic zinc is transformed into the purpose of aqueous sulfuric acid from mineral, neutral leaching process obtains qualified solution of zinc sulfate, and this solution of zinc sulfate changes subsequent processing over to as the raw material that next step extracts metallic zinc; In neutral leaching process, also produce neutral leached mud; Because zinc ferrite etc. is not leached by dilute sulphuric acid, causes valuable elements such as zinc, indium to enter into leached mud, causes the loss of valuable elements such as metallic zinc, indium, nearly all iron also enters neutral leached mud.In order better to reclaim and to utilize this part not leached and enter into leached mud metallic zinc, indium etc., need special process and technology by dilute sulphuric acid; Neutral leached mud is according to the ferruginous difference of high-iron zinc sulfide concentrate, and it contains zinc about 18～24wt%, and iron content is about 25～35wt%, and sulfur-bearing is at 5～8wt%.The volatilization of neutral leached mud rotary kiln high temperature reduction is a kind of technical matters of handling neutral leached mud, and this process is the high temperature of 1250 ℃ of controls, adds coke as heat-generating agent and reductive agent, and the consumption of coke is the 50wt% that drops into the rotary kiln material amount.Neutral leached mud is carried out the high temperature reduction volatilization, and in the high temperature reduction volatilization process, zinc oxide and other zinc compound are reduced volatilization and gather dust and obtain oxide powder and zinc, and metallic zinc obtains enrichment in this oxide powder and zinc, and generally containing zinc is about 50wt%; In the rotary kiln high temperature reduction volatilization process, elementary sulfur in the neutral leached mud is oxidized, generates sulfurous gas and enters in the high-temperature smoke gas, because in rotary kiln high temperature reduction volatilization process, control high excess air coefficient, make that exhaust gas volumn is very big in this process, diluted the sulfurous gas that generates, it is very low to make flue gas contain sulfurous gas, be difficult to recycle, all be discharged in the atmosphere, cause sulfur dioxide pollution, and then produce acid rain; Metallic iron is reduced into suboxide or metallic iron enters into kiln slag, realizes the separation of iron zinc in this process.Oxide powder and zinc that this process is produced contains about the about 50wt% of zinc, needs independent special disposal to reclaim metallic zinc and valuable element such as indium wherein.Second kind of Technology flow process is that zinc ore concentrate fluidized bed roasting-neutrality leaching-neutral leached mud high temperature peracid leaching-jarosite process deironing-liquid-solid separation-jarosite slag (storing up)-zinc-containing solution returns main flow recovery zinc, in this technical matters flow process, zinc ore concentrate fluidized bed roasting and the neutral purpose that leaches are as previously mentioned.It is that the control extraction temperature is at 95 ℃ that neutral leached mud high temperature peracid leaches, sulfuric acid concentration reaches the technical qualification of 200～300g/l, whole acid concentration control 35～70g/l, neutral leached mud is leached, at this moment zinc ferrite etc. is not dissolved in the mineral of dilute sulphuric acid, can dissolve the sulphuric acid soln that enters into high density smoothly, obtain a kind of iron content height, contain the lower vitriol mixing solutions of zinc, iron and zinc separates in this zinc sulfate and the ferric sulfate mixing solutions, must adopt special method to carry out, the method of separation of Zinc and Iron from zinc sulfate and ferric sulfate mixing solutions has jarosite process in the method for industrial employing, goethite process and hematite process.In the zinc hydrometallurgy process, adopt jarosite process to remove iron in the high solution of zinc sulfate of iron ion content usually.Jarosite process is that controlled temperature is 90～95 ℃, and control pH value of solution value is smaller or equal to 1.5, adds a certain amount of monovalent ion, as potassium ion, and sodium ion, ammonium ions etc. add crystal seed simultaneously, make ferric sulfate generate AFe
3(SO
4)
2(H
2O)
6Such material, this material are a kind of crystallite precipitations, can separate from solution.The chemical reaction that generates jarosite is: 3Fe
2(SO
4)
3+ 2A (OH)+10H
2O=2AFe
3(SO
4)
2(H
2O)
6+ 5H
2SO
4, the chemical reaction that generates jarosite is a reversible reaction, that is to say, the process that generates precipitation as jarosite is one and discharges the vitriolic process that when sulfuric acid concentration reached a certain amount of, the jarosite crystallite of generation precipitation will be dissolved by acid again, generate iron ion, make iron ion return to solution.So, for jarosite is generated, must keep pH smaller or equal to or near 1.5, just can make jarosite keep the precipitation state like this.And the process that jarosite generates, to make sulfuric acid concentration rising in the reaction system, thereby the whole process that generates jarosite must be carried out acidity adjustment and control, generate and to adopt the method for adding the zinc roasted ore in the jarosite process, in and generating the sulfuric acid that the jarosite process produces; When iron all generates jarosite from solution after, just realized the separation of iron zinc.At this moment, obtain zinciferous solution and return main flow extraction metallic zinc.Obtain containing the jarosite slag of zinc 3～8wt% simultaneously, this jarosite slag is the finishing slag of zinc hydrometallurgy process, stores up, this jarosite slag contains contents of many kinds of heavy metal ion, in the process of storing up, there is the heavy-metal pollution problem, be a kind of typical source of heavy metal pollution.
In sum, in routine techniques and technology, no matter be that rotary kiln vaporization at high temperature method or high temperature peracid leaching method are handled neutral leached mud, reach the isolating purpose of iron zinc, all have the technical matters long flow path, the process control difficulty, metal recovery rate is low, and reagent consumption is big, and sulfurous gas is big for environment pollution in the high temperature reduction volatilization process, there are problems such as heavy-metal pollution in the jarosite slag muck, also limits simultaneously and has influenced zinc, the rate of recovery of indium and the utilization ratio of iron resources.
Chinese scholars is studied more to raising zinc, indium leaching yield, method for removing iron, hot acid extract technologies such as jarosite process, goethite process, hematite process have been researched and developed in succession, its basic ideas are to adopt leaching conditions such as high temperature, peracid to destroy zinc ferrite with common characteristics, remove with the form precipitation of jarosite, pyrrhosiderite or rhombohedral iron ore then, to reach the purpose that improves zinc, indium recovery.At the research that improves zinc, indium leaching yield in the zinc ferrite, Li Ximing etc. utilize mechanical activation to promote zinc ferrite to decompose and study, and promote the activation of calcining particle surface by mechanical activation, improve the leaching yield of zinc; Li Honggui etc. have studied the method for mechanical activation zinc leaching residue, improve zinc, the indium leaching yield of leached mud and the leaching that suppresses iron with this; Huang Wei, Liu Chen etc. utilize reducing roasting to handle zinc baking sand, decompose zinc ferrite, improve zinc leaching rate etc.
Though obtained effect preferably on the leaching yield of aforesaid method zinc, indium in improving calcining, but when decomposing zinc ferrite raising leaching yield, all inevitably a large amount of iron is leached in the solution, need through iron purification, and because leach liquor is rich in indium, in order effectively to reclaim indium metal, its purification process is comparatively complicated, in scavenging process, the zinc, the indium that leach are lost in the scum again in a large number, have reduced metal recovery rate.Causing the high basic reason of these processing method leach liquor iron content is the existence of zinc ferrite in the calcining.Because zinc sulfides concentrate bearing high content of indium and iron thing phase composite complexity, main metallic zinc, iron, indium are with the symbiosis of oxide morphology embedding cloth, and the indium overwhelming majority wherein with fine granularity embedding cloth in iron sulfide mineral, iron in the calcining of the fluidized bed roasting desulfurization gained overwhelming majority forms zinc ferrites, and the fine particle embedding cloth that is diameter and is 3-15 μ m is on the zno-based body; And the In in the calcining is close with the iron ion radius owing to ionic radius, and the overwhelming majority enters in the zinc ferrite lattice by the modes of displacement iron ion, forms wustite sosoloid.This characteristic has just determined just must take effective measures if will improve the leaching yield of zinc and indium in the calcining, decomposes zinc ferrite, and destruction zinc ferrite lattice discharges zinc and the indium of its parcel; Simultaneously for guarantee iron in the calcining the least possible enter leach liquor, just must before leaching, the ore dressing mode be crossed by most of Tie Tong and remove.
By thermomechanical analysis, zinc ferrite is easy to the reduction decomposition by CO as can be known, its component Fe
2O
3More than 570 ℃,, press Fe at reduction temperature with the raising of CO concentration in the furnace gas
2O
3→ Fe
3O
4→ FeO → Fe changes in proper order, presses Fe at reduction temperature below 570 ℃
2O
3→ Fe
3O
4→ Fe changes in proper order; And the In of embedding cloth wherein
2O
3Can directly be reduced to the less indium metal of vapour pressure below 500 ℃ at reduction temperature, and also exigent temperature of principle and the CO concentration of ZnO, be ZnO, Fe with the zinc ferrite reduction decomposition under low temperature weakly reducing atmosphere condition therefore
3O
4With metal In be easily, and reduction product Fe
3O
4Be strongly magnetic mineral, separate the iron that effectively to remove in the calcining by magnetic separation.
Summary of the invention
The present invention is directed to the deficiency of existing technology, a kind of processing method of rich indium high ferro zinc baking sand reduction magnetic separation separation of Zinc indium iron is provided, zinc indium iron in the calcining is separated in the ore dressing mode before leaching, a large amount of iron enter leach liquor when having avoided follow-up leaching, simplify purification process, can reach the purpose of comprehensive utilization of resources simultaneously.
Solve that the above-mentioned technical problem of the present invention taked technical scheme be: contain zinc 45wt%～55wt%, iron content 15wt%～30wt%, contain the rich indium high ferro zinc baking sand of indium 0.08wt%～0.25wt% what fluidized bed roasting obtained, utilize himself waste heat, feed coal gas and reduce processing a little less than carrying out low temperature below 570 ℃, making zinc ferrite decomposition-reduction wherein is ZnO, Fe
3O
4And part iron, again with the levigate slurrying of reduced calcine, carry out wet magnetic separation separation of Zinc indium iron, obtain iron ore concentrate and rich indium zinc ore concentrate.
Concrete processing method of the present invention also comprises following scheme:
1. the temperature of the rich indium high ferro zinc baking sand that obtains of fluidized bed roasting is 800～900 ℃; 2. the temperature that feeds the gas reduction processing is 450～550 ℃; 3. the mass concentration of the levigate slurrying of reduced calcine is 40wt%～60wt%, and is levigate to 100 orders; 4. the isolating magnetic induction density of magnetic separation is 30～100mT.
It is that rich indium high ferro zinc baking sand is directly sent into rotary kiln behind fluidized bed roasting that described reduction is handled, feed the coal gas of calcining quality 3wt%～8wt% at the revolution kilneye by the coal-gas producer of revolution kilneye, the control kiln temperature carries out the weak reducing roasting of low temperature for 450～550 ℃, and roasting time is 30～80min.
The feeding amount of coal gas is with reduction Fe in the described reduction reaction
2O
3Be Fe
3O
42～4 of the theoretical amount of required CO is extraordinarily gone into; Calcining after the reduction is to deliver to the levigate slurrying of wet-type ball mill behind naturally cooling, imports slurry pool then; The ore pulp that mill is good pumps into and carries out magnetic separation separation deironing in the adjustable permanent magnetic separator.
The principal reaction that takes place in the above-mentioned technology is:
3ZnFe
2O
4+CO＝3ZnO+2Fe
3O
4+CO
2
ZnFe
2O
4+CO＝ZnO+2FeO+CO
2
ZnFe
2O
4+FeO＝ZnO+Fe
3O
4
3(ZnO)
2·In
2O
3·Fe
2O
3+4CO＝6ZnO+2Fe
3O
4+2In+4CO
2
Fe
3O
4+4CO＝3Fe+4CO
2
Beneficial effect of the present invention is: present method adopts at rich indium high ferro zinc baking sand and selects the technique means of selecting after smelting combination, the first smelting, utilization reducing roasting---weak magnetic separation process separation of Zinc indium iron, obtain iron ore concentrate and rich indium zinc ore concentrate, compared with prior art have following beneficial effect:
(1) energy consumption is low, the reductive agent consumption is few.Making full use of boiling calcining self waste heat, after fluidized bed roasting is finished, zinc baking sand is contacted with a small amount of reductive agent, under the waste heat effect of self, carry out the weak reducing roasting of low temperature, is ZnO, Fe with the zinc ferrite decomposition-reduction
3O
4And small amounts of iron.
(2) metal recovery rate height.The weak reducing roasting of low temperature has avoided the strong reduction reaction of high temperature to generate a large amount of metallic zinc, metallic iron and iron protoxide, simultaneously because In
2O
3Can directly be reduced to the less indium metal of vapour pressure below 500 ℃, the weak reducing roasting of low temperature not only can make the indium metal of embedding cloth in the zinc ferrite be dissociated, the loss of having avoided the indium vaporization at high temperature to cause again.
(3) simple to operate, be easy to control, overcome in the calcining that mineral grain is meticulous, valuable element disperses to mix with foreign metal, embedding cloth coexists, be difficult to sort isolating problem.After reducing roasting, the lattice of zinc ferrite is destroyed, and the thing of iron partly changes ferromagnetic Fe mutually in the calcining
3O
4And metallic iron, significantly improve it and sort performance, be easy to magnetic separation and separate.
(4) realized that the zinc indium iron in the rich indium high ferro zinc baking sand is separated in the ore dressing mode before leaching.Adopt wet-milling wet separation easy to implement after the reducing roasting, but high efficiency separation zinc indium iron not only obtains rich indium zinc ore concentrate, can obtain a large amount of iron ore concentrates simultaneously, the iron in the calcining is recycled, comprehensive utilization of resources rate height.
(5) adopt gas reduction, do not have new impurity and introduce, fume amount is little, and the equipment corrosion degree is low.
Therefore, that the present invention has is simple to operate, be easy to control, production efficiency height, production cost is low, reagent consumption is few, energy consumption is low, the metal recovery rate advantages of higher, can efficiently handle rich indium high ferro zinc baking sand separation of Zinc indium iron.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Specific embodiment
Example one: from the rich indium high ferro zinc baking sand in somewhere, Yunnan, its main chemical compositions is:
| Component | Zn | Fe | In | Cu | Pb | Sn | Cd | Sb | S | As | SiO 2 | CaO |
| Content wt/% | 50.04 | 24.11 | 0.12 | 0.32 | 0.29 | 0.21 | 0.21 | 0.12 | 1.29 | 0.35 | 1.12 | 0.71 |
Main thing is mutually:
| The thing phase | ZnO | ZnFe 2O 4 | Fe 2O 3 | ZnS | SiO 2 | Other | Amount to |
| Ratio/wt% | 54.34 | 23.41 | 18.96 | 0.04 | 1.12 | 2.13 | 100 |
Reducing roasting---magnetic separation technology technology is:
(1) above-mentioned rich indium high ferro zinc baking sand is joined Φ 2.8 * 36m rotary kiln with the feed rate of 12.75t/h, in rotary kiln, feed the coal gas of calcining quality 5wt% by the coal-gas producer of revolution kilneye, 480～510 ℃ of control kiln temperatures, reducing roasting (material is at the revolution kiln residence time) 60min, the output reduced calcine.
The main thing of reduced calcine is mutually:
| The thing phase | Total zn | Total Fe | In | ZnO | ZnFe 2O 4 | Fe 3O 4 | Fe | ZnS | SiO 2 | Other | Amount to |
| Ratio/wt% | 50.41 | 24.84 | 0.122 | 61.43 | 7.48 | 23.55 | 4.12 | 0.04 | 1.14 | 2.24 | 100 |
(2) with the reduced calcine of rotary kiln output after naturally cooling is handled, be transported to wet-type ball mill with conveyor, the water of quality such as addings, the ore pulp of furnishing mass concentration 50wt%, levigate extremely-100 orders (0.15mm).It is pending that the fine grinding ore pulp of ball mill output imports slurry pool.
(3) above-mentioned slurry is pumped into adjustable permanent magnetic separator, under magnetic induction density 80mT, carries out low intensity magnetic separation and separate deironing, obtain the rich indium zinc ore concentrate of magnetic product iron ore concentrate and non magnetic product.
The technical matters index is:
Example two: from the rich indium high ferro zinc baking sand in somewhere, Yunnan, its main chemical compositions is:
| Component | Zn | Fe | In | Cu | Pb | Sn | Cd | Sb | S | As | SiO 2 | CaO |
| Content/wt% | 54.12 | 20.21 | 0.10 | 0.43 | 0.41 | 0.20 | 0.45 | 0.11 | 1.33 | 0.31 | 1.68 | 0.75 |
Main thing is mutually:
| The thing phase | ZnO | ZnFe 2O 4 | Fe 2O 3 | ZnS | SiO 2 | Other | Amount to |
| Ratio/wt% | 59.97 | 21.81 | 14.45 | 0.05 | 1.68 | 2.04 | 100 |
Reducing roasting---magnetic separation technology technology is:
(1) above-mentioned rich indium high ferro zinc baking sand is joined Φ 2.8 * 36m rotary kiln with the feed rate of 12.75t/h, in rotary kiln, feed the coal gas of calcining quality 3wt% by the coal-gas producer of revolution kilneye, 520～550 ℃ of control kiln temperatures, reducing roasting (material is at the revolution kiln residence time) 40min, the output reduced calcine.
The main thing of reduced calcine is mutually:
| The thing phase | Total Zn | Total Fe | In | ZnO | ZnFe 2O 4 | Fe 3O 4 | Fe | ZnS | SiO 2 | Other | Amount to |
| Ratio/wt% | 55.02 | 20.51 | 0.111 | 65.32 | 8.87 | 22.67 | 1.58 | 0.05 | 1.70 | 2.07 | 100 |
(2) with the reduced calcine of rotary kiln output after naturally cooling is handled, be transported to wet-type ball mill with conveyor, add the water of calcining quality 150wt%, the ore pulp of furnishing mass concentration 40wt%, levigate to-100 orders (0.15mm).It is pending that the fine grinding ore pulp of ball mill output imports slurry pool.
(3) above-mentioned slurry is pumped into adjustable permanent magnetic separator, under magnetic induction density 50mT, carries out low intensity magnetic separation and separate deironing, obtain the rich indium zinc ore concentrate of magnetic product iron ore concentrate and non magnetic product.
The technical matters index is:
Example three: from the rich indium high ferro zinc baking sand in somewhere, Guangxi, its main chemical compositions is:
| Component | Zn | Fe | In | Cu | Pb | Sn | Cd | Sb | S | As | SiO 2 | CaO |
| Content/wt% | 51.12 | 22.03 | 0.15 | 0.41 | 0.42 | 0.23 | 0.39 | 0.10 | 1.27 | 0.32 | 1.91 | 0.82 |
Main thing is mutually:
| The thing phase | ZnO | ZnFe 2O 4 | Fe 2O 3 | ZnS | SiO 2 | Other | Amount to |
| Ratio/wt% | 56.37 | 21.39 | 17.32 | 0.04 | 1.91 | 2.97 | 100 |
Reducing roasting---magnetic separation technology technology is:
(1) above-mentioned rich indium high ferro zinc baking sand is joined Φ 2.8 * 36m rotary kiln with the feed rate of 12.75t/h, in rotary kiln, feed the coal gas of calcining quality 8wt% by the coal-gas producer of revolution kilneye, 450～480 ℃ of control kiln temperatures, reducing roasting (material is at the revolution kiln residence time) 80min, the output reduced calcine.
The main thing of reduced calcine is mutually:
| The thing phase | Total Zn | Total Fe | In | ZnO | ZnFe 2O 4 | Fe 3O 4 | Fe | ZnS | SiO 2 | Other | Amount to |
| Ratio/wt% | 52.20 | 22.73 | 0.155 | 65.56 | 0.98 | 21.64 | 6.69 | 0.04 | 1.98 | 3.08 | 100 |
(2) with the reduced calcine of rotary kiln output after naturally cooling is handled, be transported to wet-type ball mill with conveyor, the water of quality such as addings, the ore pulp of furnishing mass concentration 50wt%, levigate extremely-200 orders (0.074mm).It is pending that the fine grinding ore pulp of ball mill output imports slurry pool.
(3) above-mentioned slurry is pumped into adjustable permanent magnetic separator, under magnetic induction density 100mT, carries out low intensity magnetic separation and separate deironing, obtain the rich indium zinc ore concentrate of magnetic product iron ore concentrate and non magnetic product.
The technical matters index is:
Claims (4)
1. the method for a rich indium high ferro zinc baking sand reduction magnetic separation separation of Zinc indium iron, it is characterized in that: contain zinc 45wt%～55wt%, iron content 15wt%～30wt%, contain the rich indium high ferro zinc baking sand of indium 0.08wt%～0.25wt% what fluidized bed roasting obtained, utilize himself waste heat, feed coal gas and reduce processing a little less than carrying out low temperature below 570 ℃, making zinc ferrite decomposition-reduction wherein is ZnO, Fe
3O
4And part iron, again with the levigate slurrying of reduced calcine, carry out wet magnetic separation separation of Zinc indium iron, obtain iron ore concentrate and rich indium zinc ore concentrate.
2. the method for rich indium high ferro zinc baking sand reduction magnetic separation separation of Zinc indium iron according to claim 1 is characterized in that: 1. the temperature of the rich indium high ferro zinc baking sand that obtains of fluidized bed roasting is 800～900 ℃; 2. the temperature that feeds the gas reduction processing is 450～550 ℃; 3. the mass concentration of the levigate slurrying of reduced calcine is 40wt%～60wt%, and is levigate to 100 orders; 4. the isolating magnetic induction density of magnetic separation is 30～100mT.
3. the method for rich indium high ferro zinc baking sand reduction magnetic separation separation of Zinc indium iron according to claim 2, it is characterized in that: it is that rich indium high ferro zinc baking sand is directly sent into rotary kiln behind fluidized bed roasting that described reduction is handled, feed the coal gas of calcining quality 3wt%～8wt% at the revolution kilneye by the coal-gas producer of revolution kilneye, the control kiln temperature carries out the weak reducing roasting of low temperature for 450～550 ℃, and roasting time is 30～80min.
4. the method for rich indium high ferro zinc baking sand reduction magnetic separation separation of Zinc indium iron according to claim 3, it is characterized in that: the feeding amount of coal gas is with reduction Fe in the reduction reaction
2O
3Be Fe
3O
42～4 of the theoretical amount of required CO is extraordinarily gone into; Calcining after the reduction is to deliver to the levigate slurrying of wet-type ball mill behind naturally cooling, imports slurry pool then; The ore pulp that mill is good pumps into and carries out magnetic separation separation deironing in the adjustable permanent magnetic separator.
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| CN102312083A (en) * | 2011-09-23 | 2012-01-11 | 来宾华锡冶炼有限公司 | Method for extracting zinc indium and recovering iron from high-iron high indium zinc concentrate |
| CN102399997A (en) * | 2011-10-28 | 2012-04-04 | 中南大学 | Method for refining zinc through combination of dressing and smelting |
| CN102643978A (en) * | 2012-04-24 | 2012-08-22 | 中南大学 | Method for inhibiting generation of ferrous oxide in high iron zinc calcine reduction roasting process by utilizing partial pressure of CO2 |
| CN103276197A (en) * | 2013-05-17 | 2013-09-04 | 中南大学 | Method for performing flash reducing and roasting on zinc calcine |
| CN103602806A (en) * | 2013-11-15 | 2014-02-26 | 吴鋆 | Smelting method of high-indium high-iron zinc concentrate |
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