CN107012328A - A kind of high ferro zinc leaching residue clean utilization method - Google Patents
A kind of high ferro zinc leaching residue clean utilization method Download PDFInfo
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- CN107012328A CN107012328A CN201710139793.9A CN201710139793A CN107012328A CN 107012328 A CN107012328 A CN 107012328A CN 201710139793 A CN201710139793 A CN 201710139793A CN 107012328 A CN107012328 A CN 107012328A
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- China
- Prior art keywords
- zinc
- high ferro
- leaching residue
- zinc leaching
- utilization method
- Prior art date
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- 239000011701 zinc Substances 0.000 title claims abstract description 108
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 103
- 238000002386 leaching Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 39
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 38
- 239000012141 concentrate Substances 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 29
- 238000005188 flotation Methods 0.000 claims abstract description 26
- 229910052742 iron Inorganic materials 0.000 claims abstract description 22
- 238000010791 quenching Methods 0.000 claims abstract description 21
- 230000000171 quenching effect Effects 0.000 claims abstract description 21
- 239000002893 slag Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052738 indium Inorganic materials 0.000 claims abstract description 18
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 11
- HASDHSVWTCCGIM-UHFFFAOYSA-N zinc iron(2+) oxygen(2-) Chemical class [O-2].[O-2].[Fe+2].[Zn+2] HASDHSVWTCCGIM-UHFFFAOYSA-N 0.000 claims abstract description 11
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 10
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000006148 magnetic separator Substances 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 238000010583 slow cooling Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 239000005864 Sulphur Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000003245 coal Substances 0.000 claims description 6
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052683 pyrite Inorganic materials 0.000 claims description 4
- 238000004073 vulcanization Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000000571 coke Substances 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 239000011028 pyrite Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 238000007885 magnetic separation Methods 0.000 claims description 2
- 229960004424 carbon dioxide Drugs 0.000 claims 1
- 229910002090 carbon oxide Inorganic materials 0.000 claims 1
- 239000003610 charcoal Substances 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 18
- 239000010949 copper Substances 0.000 abstract description 18
- 229910052802 copper Inorganic materials 0.000 abstract description 17
- 238000003723 Smelting Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052709 silver Inorganic materials 0.000 abstract description 6
- 239000004332 silver Substances 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 description 24
- 238000011084 recovery Methods 0.000 description 19
- 239000011133 lead Substances 0.000 description 17
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 14
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 13
- 229910052797 bismuth Inorganic materials 0.000 description 13
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 13
- 229910000368 zinc sulfate Inorganic materials 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulfur dioxide Inorganic materials O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 229910052924 anglesite Inorganic materials 0.000 description 6
- 229960001763 zinc sulfate Drugs 0.000 description 6
- 239000011686 zinc sulphate Substances 0.000 description 6
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 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
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 description 3
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical group [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 206010048259 Zinc deficiency Diseases 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- LWUVWAREOOAHDW-UHFFFAOYSA-N lead silver Chemical compound [Ag].[Pb] LWUVWAREOOAHDW-UHFFFAOYSA-N 0.000 description 1
- 229910052960 marcasite Inorganic materials 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/26—Cooling of roasted, sintered, or agglomerated ores
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
-
- 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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
-
- 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
- C22B58/00—Obtaining gallium or indium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
-
- 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 present invention relates to a kind of high ferro zinc leaching residue clean utilization method, belong to selecting and smelting technology field.First by high ferro zinc leaching residue drying and dehydrating; then reducing agent and vulcanizing agent are added simultaneously; carbon sulphur mixed atmosphere, which is carried out, under the conditions of temperature is 400 DEG C ~ 900 DEG C is calcined anti-0.5h ~ 3.5h; after roasting terminates; it is passed through nitrogen or argon gas makees protective gas; Slow cooling is carried out with 150 DEG C/h ~ 300 DEG C/h speed, water quenching obtains Water Quenching Slag after temperature is down to below 200 DEG C；Obtained Water Quenching Slag is carried out to conventional flotation processing, artificial sulphide concentrate and flotation tailing is obtained；Obtained flotation tailing is subjected to conventional magnetic separator and obtains zinc-iron oxides concentrate, zinc-iron oxides concentrate is passed through gaseous reducing agent and is 950 DEG C ~ 1300 DEG C reduction volatilization reaction 1.0h ~ 4.0h in temperature, after reduction volatilization terminates, the zinc product containing indium is obtained after the gas evaporated is reclaimed, iron product is obtained after remaining solid cooling of volatilizing.The valuable metal such as copper of the present invention, lead, zinc, indium and silver element can high efficiente callback and high-valued, cleaning new technology without scum generation.
Description
Technical field
The present invention relates to a kind of high ferro zinc leaching residue clean utilization method, belong to selecting and smelting technology field.
Background technology
High ferro zinc leaching residue is that high-iron zinc sulfide concentrate leaches a kind of intermediate obtained after flow for-two sections by fluidized bed roasting
Material, it is always the problem that domestic and international metallurgy industry needs to be broken through that high-valued and clean utilization is carried out to it.
In zinc metallurgical process, because zinc concentrate is often associated with 10% or so ferro element, in order to reach in roasting process
Zinc amount in zinc ferrite, zinc ferrite accounts for total zinc amount 8% ~ 10% is inevitably generated in preferable desulfurization degree, zinc calcine.When zinc essence
Ore deposit is the high iron charge that China is largely present（≥10%）Or during marmatite, ferrous acid Zn content can be higher in calcining.Zinc ferrite category is difficult
Zinc species are soaked, neutrality is leached and Weak-acid leaching link is difficult to be leached, and substantial amounts of leached mud can be produced in leaching process.Hot acid
Leach successfully solve zinc leaching rate improve and valuable metal lead silver recovery problem, but also generate two it is big new the problem of：Remove
Iron is burdensome, complex operation, production cost high；A large amount of iron dross removings are produced, valuable element loses big with scum, and iron resource can not
It is utilized effectively, there are a large amount of unstable heavy metal contaminants in scum, the process leaching ability of heavy metal of storing up easily causes secondary dirt
Dye etc., country has prohibited the outdoor of heavy scum and stored up.After fire metallurgy process processing the high ferro acid leaching residue quantity of slag is few, scum is dirty
Dye is small, is the new direction that zinc cleans smelting technique.However, nowadays rotary kiln technology Jiao amount consumption is up to the 50% of the quantity of slag, cause big
Measure CO2 emission and need to increase low concentration SO2Smoke processing system.In addition, iron, rare precious metal and gangue content have been given birth to
Into composite solid solution, rare precious metal and iron resource is caused to be difficult to reclaim.
Appoint as the continuous reinforcement of people's environmental consciousness, especially country attach most importance in the formulation energy-saving and emission-reduction of 12 periods
Since business, the thinking of development low-carbon green economy, and lead zinc deficiency and excess price is depressed, and Some Enterprises start to stop to such smelting
The pyrogenic attack of slag is refined, causes a large amount of zinc smelting slags to have to handle in the way of storing up or direct out sale, causes serious ring
Border pollution and the waste of valuable resource.Therefore, exploitation zinc smelting dreg cleaning treatment new technology to alleviate resource supply and demand contradiction with
And reduction environmental pollution has great importance.
Selecting smelting combination technology is zinc smelting dreg cleaning treatment research new trend in recent years.Chinese patent
The method that reduction roasting is used in CN201110332253.5, CN201110096566.5 and CN201210122328.1, leads to
Being precisely controlled for different reducing conditions is crossed, zinc ferrite selectivity zinc oxide and ferroso-ferric oxide is reduced to, then using magnetic
Choosing and the method for weak-acid leaching, realize efficiently separating for zinc-iron, but still there is the reduction of crossing of iron, and a large amount of iron enter after zinc leaching
Enter to leach the problems such as the recovering effect such as night and other metals such as lead, silver and indium is undesirable.In addition, primarily directed to zinc in patent
The zinc calcine that concentrate is obtained after fluidized bed furnace is handled, and the high ferro zinc leaching residue containing copper, silver and lead zinc sulfate is paid close attention to
It is less.For the slag charge of leaded zinc sulfate, the research team where applicants is once by introducing reducing atmosphere, by lead
The autovulcanization of zinc sulfate selectivity then uses flotation, the certain conversion of acquirement and flotation recovering effect for artificial sulphide ore
（CN201310065266.X）, but do not proposed for the high-valued and clean utilization of the high ferro zinc leaching residue containing various ingredients
The method of effect.
The content of the invention
The environmental pollution brought for a large amount of high ferro zinc leaching residues produced in Zinc Hydrometallurgy Process, wet method or pyrogenic process are recycled into
This height, conventional beneficiation method reclaims a series of problems, such as valuable metal difficulty is big, the present invention is intended to provide a kind of high ferro zinc leaching residue
High-valued, clean utilization method, material is dehydrated by this method first, after drying process, by slag under carbon-sulphur mixed atmosphere
In material lead zinc sulfate selectivity be converted into artificial sulphide ore, while realize copper, bismuth and silver vulcanization and zinc ferrite magnetic
Change conversion, artificial sulphide ore and high-purity ferrous acid zinc concentrate are then respectively obtained using floating-magnetic combined process flow, the former can be used as zinc
Concentrate sells, and the latter is by obtaining zinc product and high-grade ironmaking material containing indium after reduction volatilization.The present invention is by following
Technical scheme is realized.
A kind of high ferro zinc leaching residue clean utilization method, it is comprised the following steps that：
（1）First by high ferro zinc leaching residue drying and dehydrating, reducing agent and vulcanizing agent are then added simultaneously, are 400 DEG C ~ 900 in temperature
Carbon-sulphur mixed atmosphere is carried out under the conditions of DEG C and is calcined anti-0.5h ~ 3.5h, after roasting terminates, nitrogen is passed through or argon gas makees protective gas,
Slow cooling is carried out with 150 DEG C/h ~ 300 DEG C/h speed, water quenching obtains Water Quenching Slag after temperature is down to below 200 DEG C；
Specifically reaction equation is：
PbSO4+ 4C = PbS + 4CO(g) （1）
ZnSO4+ 4C = ZnS + 4CO(g) （2）
PbSO4 + 4CO(g) = PbS + 4CO2(g) （3）
ZnSO4 + 4CO(g) = ZnS + 4CO2(g) （4）
3ZnFe2O4(s) + C(s) = 3ZnO(s) + 2Fe3O4(s) + CO(g) （5）
3ZnFe2O4(s) + CO(g) = 3ZnO(s) + 2Fe3O4(s) + CO2(g) （6）
Fe2O3(s) + C(s) =2Fe3O4(s) + CO(g) （7）
Fe2O3(s) + CO(g) = 2Fe3O4(s) + CO2(g) （8）
FeS2= FeS+1/2S2(g) （9）
S→S2(g) （10）
2CuO+3/2S2(g)=2CuS+SO2(g) （11）
2CuO+ C+S2 (g)=2CuS+CO2 (g) （12）
2BiO+3/2S2(g)=2BiS+SO2(g) （13）
2BiO+ C+S2 (g)=2BiS+CO2 (g) （14）
4Ag2O+5S2(g)=8AgS+2SO2(g) （15）
2Ag2O+ C+2S2 (g)=4AgS+CO2 (g) （16）
Wherein react（1）~（4）The autovulcanization for being lead zinc sulfate under reducing atmosphere reaction,（5）~（8）For zinc ferrite and three
Aoxidize the magnetization decomposition reaction of two iron；（9）~（16）For the vulcanization reaction of copper, bismuth and silver oxide；
（2）By step（1）Obtained Water Quenching Slag carries out conventional flotation processing, obtains artificial sulphide concentrate and flotation tailing；
Vulcanization ore deposit floating agent system is used, flotation flowsheet is bulk flotation or diffeential floatation, and wherein bulk flotation is obtained
Be bulk concentrate, what diffeential floatation was obtained is single copper, lead and zinc concentrate；
（3）By step（2）Obtained flotation tailing carries out conventional magnetic separator and obtains zinc-iron oxides concentrate, zinc-iron oxides
Concentrate is passed through gaseous reducing agent and is 950 DEG C ~ 1300 DEG C reduction volatilization reaction 1.0h ~ 4.0h in temperature, after reduction volatilization terminates,
The zinc product containing indium is obtained after the gas evaporated is reclaimed（Zinc product containing indium is metal zinc or oxide powder and zinc, metal
The composition of zinc powder is：Zn90% ~ 95%, In0.5 ~ 2%, other 3% ~ 9.5%, the composition of oxide powder and zinc for Zn50% ~ 75%, In0.5 ~
3% other 23% ~ 49.5%）, iron product is obtained after remaining solid cooling of volatilizing（Composition is Fe85 ~ 97%, other 3 ~ 15%）, wave
Sending out reaction equation specific is：
ZnFe2O4(s) + 4H2(g)= Zn(g) + 2Fe(s) + 4H2O(g) （17）
ZnFe2O4(s) + 4CO(g) = Zn(g) + 2Fe(s) + 4CO2(g) （18）
ZnO(s) + H2(g) = Zn(g) + H2O(g) （19）
ZnO(s) + CO(g) = Zn (g) + CO2(g) （20）
In2O3+ 3CO(g) =2In(g) + 3CO2(g) （21）
In2O3 + 3H2(g) = 2In(g) + 3H2O(g) （22）
FeO(s) + H2(g) = Fe(s) + H2O(g) （23）
FeO(s) + CO(g) = Fe(s) + CO2(g) （24）.
The high ferro zinc leaching residue includes following mass percent component：Pb2~5%、Zn10~20%、Fe15~25%、Ag200~
400g/t and In150 ~ 450g/t.
The step（1）Middle reducing agent and vulcanizing agent be in sulphur coal, sulphur coal carbon content be 70wt% ~ 85wt%, sulphur
Content 3wt% ~ 6wt%, addition is high ferro zinc leaching residue quality 6% ~ 15%.
The step（1）Middle reducing agent is solid reductant or gaseous reducing agent.
The solid reductant is one or more of arbitrary proportion mixtures in activated carbon, coke, carbon dust, and addition is
High ferro zinc leaching residue quality 5% ~ 12%.
The gaseous reducing agent is carbon monoxide, hydrogen, producer gas, one or more of arbitrary proportions of coke-stove gas
Mixture；Gaseous reducing agent volumetric concentration containing CO 10% ~ 50%, the H2Volumetric concentration 1% ~ 12%, remaining component is N2。
The step（1）Middle vulcanizing agent is vulcanized sodium, pyrite or sulphur, and addition is high ferro zinc leaching residue quality 1% ~ 4%.
The step（3）Middle magnetic separator magnetic field intensity is 0.5 ~ 1T.
The step（3）CO volumetric concentrations are 30% ~ 90%, H in middle gaseous reducing agent2Volumetric concentration is 8% ~ 60%, remaining
Component is N2。
The beneficial effects of the invention are as follows：
（1）In carbon-sulphur mixed atmosphere, realize in slag charge the oxide curative such as lead zinc sulfate autovulcanization, copper, bismuth and silver and
The magnetized height coupling of zinc ferrite, has decreased or even eliminated the problem of environmental pollution brought of sulfur dioxide, simultaneously from source
Technique of preparing for low cost, low stain creates condition；
（2）Zinc-iron oxides after magnetization do not need ore grinding, directly carry out the magnetic separation in moderate strength magnetic field, improve the comprehensive of zinc-iron
Close grade and the rate of recovery.After the zinc-iron oxides reduction volatilization of purifying, obtained zinc, indium is obtained in the form of zinc powder or secondary zinc oxide
To reclaim, residue is high-grade iron granule, directly as iron-smelting raw material；
（3）Lead, zinc, indium and silver-colored comprehensive recovery improve 3 ~ 8%, and copper and bismuth comprehensive recovery improve 10% ~ 40%, and iron is integrated back
Yield improves 20 ~ 50%；
（4）The present invention is that one kind is produced without SO 2 tail gas, and the valuable metal element such as copper, lead, zinc, indium and silver can high efficiente callback
And high-valued, the cleaning new technology generated without scum.
Brief description of the drawings
Fig. 1 is present invention process flow chart.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in figure 1, the high ferro zinc leaching residue clean utilization method, it is comprised the following steps that：
（1）First by high ferro zinc leaching residue（The content of copper and bismuth is very low in the high ferro zinc leaching residue, and its chemical composition is：Pb3.4%、
Zn16.5%, Fe21.5%, Ag272.3g/t, In278.5g/t, the chemical and physical phase of lead is PbSO476%th, PbS8%, other 16%, zinc
Chemical and physical phase be：ZnSO438.6%、ZnFe2O458.3%, other 3.1%, silver-colored chemical and physical phase is：Ag2O18.6%、
AgS74.4%, other 7%）Drying and dehydrating, then adds reducing agent simultaneously（Carbon dust, addition is high ferro zinc leaching residue quality 12%）With
Vulcanizing agent（Vulcanized sodium, addition is high ferro zinc leaching residue quality 1%）, carbon-sulphur mixed atmosphere is carried out under the conditions of temperature is 750 DEG C
Anti- 1.5h is calcined, after roasting terminates, nitrogen is passed through or argon gas makees protective gas, Slow cooling is carried out with 150 DEG C/h speed, treated
Temperature is down to water quenching after 200 DEG C and obtains Water Quenching Slag；
（2）By step（1）Obtained Water Quenching Slag carries out conventional flotation processing, obtains artificial sulphide concentrate（The concentrate is lead
Grade 14.5%, zinc grade 34.5%, silver-colored grade 1000g/t bulk concentrate）And flotation tailing；
（3）By step（2）Obtained flotation tailing carries out conventional magnetic separator（Fixed magnetic field intensity is 0.75T）Obtain zinc-iron
Oxide concentrate（Chemical composition is Zn21.5%, Fe44.1%, other 34.4%）, zinc-iron oxides concentrate is passed through gaseous reducing agent
（CO volumetric concentrations are 50%, H in gaseous reducing agent2Volumetric concentration is 15%, and remaining component is N2）And be 1150 DEG C of reduction in temperature
Volatiling reaction 1.0h, after reduction volatilization terminates, the zinc product containing indium is obtained after the gas evaporated is reclaimed（Zinc production containing indium
Product are oxide powder and zinc, and the composition of oxide powder and zinc is Zn70.5%, In1.7% other 27.8%）, after remaining solid cooling of volatilizing
To iron product（Composition is Fe92.3%, other 7.7%）.
Lead, zinc recovery are respectively 92% and 95% in whole flow process, and the silver-colored rate of recovery is 80%, and the rate of recovery of iron is 90%.
Embodiment 2
As shown in figure 1, the high ferro zinc leaching residue clean utilization method, it is comprised the following steps that：
（1）First by high ferro zinc leaching residue（Its chemical composition is：Pb2.3%、Zn14.4%、Fe19.8%、Ag389.6g/t、
Cu1.4%, In278.5g/t and Bi0.96%, the chemical and physical phase of lead is PbSO468.9%th, PbS12%, other 9.1%, the chemistry of zinc
Thing is mutually：ZnSO442.5%、ZnFe2O453.8%, other 3.7%, silver-colored chemical and physical phase is：Ag2O13.8%, AgS71.2%, it is other
15%, the chemical and physical phase of copper is：CuO84.2%, CuS13.9%, other 1.9%, the chemical and physical phase of bismuth is：BiO76.2%、
BiS21.3%, other 2.5%）Drying and dehydrating, then adds reducing agent and vulcanizing agent simultaneously（Reducing agent and vulcanizing agent are high-sulfur
Carbon content is 80wt% in coal, sulphur coal, and sulfur content 5.5wt%, addition is high ferro zinc leaching residue quality 14.5%）, it is in temperature
Carbon-sulphur mixed atmosphere is carried out under the conditions of 850 DEG C and is calcined anti-2.0h, after roasting terminates, nitrogen is passed through or argon gas makees protective gas, with
300 DEG C/h speed carries out Slow cooling, and water quenching obtains Water Quenching Slag after temperature is down to 180 DEG C；
（2）By step（1）Obtained Water Quenching Slag carries out conventional flotation processing, obtains artificial sulphide concentrate（The concentrate is lead
Grade is 10.2%, zinc grade 38.8%, silver-colored grade 1870g/t, copper grade 4.3%, the bulk concentrate of bismuth grade 2.8%）And flotation
Mine tailing；
（3）By step（2）Obtained flotation tailing carries out conventional magnetic separator（Fixed magnetic field intensity is 0.8T）Obtain zinc-iron
Oxide concentrate（Chemical composition is Zn20.2%, Fe44.1%, other 35.7%）, zinc-iron oxides concentrate is passed through gaseous reducing agent
（CO volumetric concentrations are 60%, H in gaseous reducing agent2Volumetric concentration is 10%, and remaining component is N2）And be 1200 DEG C of reduction in temperature
Volatiling reaction 1.5h, after reduction volatilization terminates, the zinc product containing indium is obtained after the gas evaporated is reclaimed（Zinc production containing indium
Product are oxide powder and zinc, and the composition of oxide powder and zinc is Zn68.8%, In2.3%）, iron product is obtained after remaining solid cooling of volatilizing
（Composition is Fe95.1%）.
Lead, zinc recovery are respectively 95% and 95.5% in whole flow process, and the silver-colored rate of recovery is 87%, copper, the bismuth rate of recovery
84.5%, the rate of recovery of iron is 89%.
Embodiment 3
As shown in figure 1, the high ferro zinc leaching residue clean utilization method, it is comprised the following steps that：
（1）First by high ferro zinc leaching residue（Its chemical composition is：Pb3.4%, Zn10%, Fe25%, Ag350g/t, Cu2.4%,
In450g/t and Bi1.8%, the chemical and physical phase of lead is PbSO472.5%th, PbS2.5%, other 25%, the chemical and physical phase of zinc is：
ZnSO438.5%、ZnFe2O455.2%, other 6.3%, silver-colored chemical and physical phase is：Ag2O21.5%, AgS74.5%, other 4%, copper
Chemical and physical phase is：CuO78.5%, CuS14.5%, other 7%, the chemical and physical phase of bismuth is：BiO68.4%, BiS19.6%, other 12%）
Drying and dehydrating, then adds reducing agent simultaneously（Reducing agent is that volume ratio is 1:1 carbon monoxide and producer gas mixed gas
Reducing agent, reducing agent intake is 2L/min units, gaseous reducing agent volumetric concentration containing CO 50%, the H2Volumetric concentration 12%, its
Remaining component is N2）And vulcanizing agent（Vulcanizing agent is pyrite, and addition is high ferro zinc leaching residue quality 4%）, it is 400 DEG C of bars in temperature
Carbon-sulphur mixed atmosphere is carried out under part and is calcined anti-3.5h, after roasting terminates, nitrogen is passed through or argon gas makees protective gas, with 250 DEG C/h
Speed carry out Slow cooling, water quenching obtains Water Quenching Slag after temperature is down to 180 DEG C；
（2）By step（1）Obtained Water Quenching Slag carries out conventional flotation processing, obtains artificial sulphide concentrate（The concentrate is lead
Grade is 14.5%, zinc grade 34.2%, silver-colored grade 1950g/t, copper grade 6.2%, the bulk concentrate of bismuth grade 4.2%）And flotation
Mine tailing；
（3）By step（2）Obtained flotation tailing carries out conventional magnetic separator（Fixed magnetic field intensity is 0.5T）Obtain zinc-iron
Oxide concentrate（Chemical composition is Zn18.5%, Fe42.5%, other 39%）, zinc-iron oxides concentrate is passed through gaseous reducing agent（Gas
CO volumetric concentrations are 90%, H in body reducing agent2Volumetric concentration is 8%, and remaining component is N2）And be 950 DEG C of reduction volatilizations in temperature
4.0h is reacted, after reduction volatilization terminates, the zinc product containing indium is obtained after the gas evaporated is reclaimed（Zinc product containing indium is
Oxide powder and zinc, the composition of oxide powder and zinc is Zn70.5%, In3.5%）, iron product is obtained after remaining solid cooling of volatilizing（Composition
For Fe94.5%）.
Lead, zinc recovery are respectively 96% and 94.2% in whole flow process, and the silver-colored rate of recovery is 85.5%, copper, the bismuth rate of recovery
84.5%, the rate of recovery of iron is 90%.
Embodiment 4
As shown in figure 1, the high ferro zinc leaching residue clean utilization method, it is comprised the following steps that：
（1）First by high ferro zinc leaching residue（Its chemical composition is：Pb5%, Zn19.4%, Fe15%, Ag200g/t, Cu2.4%,
In150g/t and Bi1.5%, the chemical and physical phase of lead is PbSO475.4%th, PbS3.5%, other 21.1%, the chemical and physical phase of zinc is：
ZnSO441.5%、ZnFe2O457.5%, other 1%, silver-colored chemical and physical phase is：Ag2O20.4%, AgS75.6%, other 4%, the change of copper
Learning thing is mutually：CuO46.8%, CuS51.4%, other 1.8%, the chemical and physical phase of bismuth is：BiO38.2%, BiS56.8%, other 5%）
Drying and dehydrating, then adds reducing agent simultaneously（Reducing agent is coke, and addition is high ferro zinc leaching residue quality 5%）And vulcanizing agent（Sulphur
Agent is sulphur, and addition is high ferro zinc leaching residue quality 3%）, carbon-sulphur mixed atmosphere roasting is carried out under the conditions of temperature is 600 DEG C
Anti- 0.5h, after roasting terminates, is passed through nitrogen or argon gas makees protective gas, carries out Slow cooling with 200 DEG C/h speed, treats temperature
It is down to water quenching after 180 DEG C and obtains Water Quenching Slag；
（2）By step（1）Obtained Water Quenching Slag carries out conventional flotation processing, obtains artificial sulphide concentrate（The concentrate is lead
Grade is 11.6%, zinc grade 28.9%, silver-colored grade 1785g/t, copper grade 5%, the bulk concentrate of bismuth grade 3%）And flotation tailing；
（3）By step（2）Obtained flotation tailing carries out conventional magnetic separator（Fixed magnetic field intensity is 1.0T）Obtain zinc-iron
Oxide concentrate（Chemical composition is Zn19.2%, Fe46.4%, other 35.4%）, zinc-iron oxides concentrate is passed through gaseous reducing agent
（CO volumetric concentrations are 30%, H in gaseous reducing agent2Volumetric concentration is 60%, and remaining component is N2）And be 1300 DEG C of reduction in temperature
Volatiling reaction 2.0h, after reduction volatilization terminates, the zinc product containing indium is obtained after the gas evaporated is reclaimed（Zinc production containing indium
Product are oxide powder and zinc, and the composition of oxide powder and zinc is Zn65.6%, In2.8%）, iron product is obtained after remaining solid cooling of volatilizing
（Composition is Fe 90.8%）.
Lead, zinc recovery are respectively 92.5% and 95.2% in whole flow process, and the silver-colored rate of recovery is 81.5%, copper, the bismuth rate of recovery
82.5%, the rate of recovery of iron is 88%.
Above in association with accompanying drawing to the present invention embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, can also be before present inventive concept not be departed from the knowledge that those of ordinary skill in the art possess
Put that various changes can be made.
Claims (9)
1. a kind of high ferro zinc leaching residue clean utilization method, it is characterised in that comprise the following steps that：
（1）First by high ferro zinc leaching residue drying and dehydrating, reducing agent and vulcanizing agent are then added simultaneously, are 400 DEG C ~ 900 in temperature
Carbon-sulphur mixed atmosphere is carried out under the conditions of DEG C and is calcined anti-0.5h ~ 3.5h, after roasting terminates, nitrogen is passed through or argon gas makees protective gas,
Slow cooling is carried out with 150 DEG C/h ~ 300 DEG C/h speed, water quenching obtains Water Quenching Slag after temperature is down to below 200 DEG C；
（2）By step（1）Obtained Water Quenching Slag carries out conventional flotation processing, obtains artificial sulphide concentrate and flotation tailing；
（3）By step（2）Obtained flotation tailing carries out conventional magnetic separator and obtains zinc-iron oxides concentrate, zinc-iron oxides
Concentrate is passed through gaseous reducing agent and is 950 DEG C ~ 1300 DEG C reduction volatilization reaction 1.0h ~ 4.0h in temperature, after reduction volatilization terminates,
The zinc product containing indium is obtained after the gas evaporated is reclaimed, iron product is obtained after remaining solid cooling of volatilizing.
2. high ferro zinc leaching residue clean utilization method according to claim 1, it is characterised in that：The high ferro zinc leaching residue includes
Following mass percent component：Pb2 ~ 5%, Zn10 ~ 20%, Fe15 ~ 25%, Ag200 ~ 400g/t and In150 ~ 450g/t.
3. high ferro zinc leaching residue clean utilization method according to claim 1, it is characterised in that：The step（1）Middle reduction
Agent and vulcanizing agent be in sulphur coal, sulphur coal carbon content be 70wt% ~ 85wt%, sulfur content 3wt% ~ 6wt%, addition is high ferro
Zinc leaching residue quality 6% ~ 15%.
4. high ferro zinc leaching residue clean utilization method according to claim 1, it is characterised in that：The step（1）Middle reduction
Agent is solid reductant or gaseous reducing agent.
5. high ferro zinc leaching residue clean utilization method according to claim 4, it is characterised in that：The solid reductant is work
Property charcoal, coke, one or more of arbitrary proportion mixtures in carbon dust, addition is high ferro zinc leaching residue quality 5% ~ 12%.
6. high ferro zinc leaching residue clean utilization method according to claim 4, it is characterised in that：The gaseous reducing agent is one
Carbonoxide, hydrogen, producer gas, one or more of arbitrary proportion mixtures of coke-stove gas；The gaseous reducing agent body containing CO
Product concentration 10% ~ 50%, H2Volumetric concentration 1% ~ 12%, remaining component is N2。
7. high ferro zinc leaching residue clean utilization method according to claim 1, it is characterised in that：The step（1）Middle vulcanization
Agent is vulcanized sodium, pyrite or sulphur, and addition is high ferro zinc leaching residue quality 1% ~ 4%.
8. high ferro zinc leaching residue clean utilization method according to claim 1, it is characterised in that：The step（3）In strong magnetic
Magnetic separation magnetic field intensity is 0.5 ~ 1T.
9. high ferro zinc leaching residue clean utilization method according to claim 1, it is characterised in that：The step（3）Middle gas
CO volumetric concentrations are 30% ~ 90%, H in reducing agent2Volumetric concentration is 8% ~ 60%, and remaining component is N2。
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| CN110983029A (en) * | 2019-11-18 | 2020-04-10 | 中南大学 | Method for carrying out synergistic vulcanization roasting on lead-zinc smelting slag and gypsum slag |
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| CN111850305A (en) * | 2020-07-28 | 2020-10-30 | 昆明理工大学 | Method for leaching cobalt and manganese from manganese-rich cobalt slag |
| CN112813277A (en) * | 2020-12-28 | 2021-05-18 | 中南大学 | Method for separating and recovering valuable metals from copper smelting slag through chlorination roasting |
| CN113522518A (en) * | 2021-06-30 | 2021-10-22 | 韶关市青绿环保科技有限公司 | Water quenching kiln slag treatment method |
| CN114606400A (en) * | 2022-01-28 | 2022-06-10 | 云锡文山锌铟冶炼有限公司 | Method for treating arsenic-zinc-containing leaching residues of high-iron |
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| CN114606400B (en) * | 2022-01-28 | 2023-09-22 | 云锡文山锌铟冶炼有限公司 | Treatment method of high-iron arsenic-zinc-containing leaching residues |
| CN114752781A (en) * | 2022-03-25 | 2022-07-15 | 桂林理工大学 | Method for roasting and leaching zinc concentrate by adding carbon and oxidizing |
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