CN106367603B - A kind of method of zinc in recovery blast furnace dust - Google Patents

A kind of method of zinc in recovery blast furnace dust Download PDF

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Publication number
CN106367603B
CN106367603B CN201611113182.9A CN201611113182A CN106367603B CN 106367603 B CN106367603 B CN 106367603B CN 201611113182 A CN201611113182 A CN 201611113182A CN 106367603 B CN106367603 B CN 106367603B
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zinc
leaching
blast furnace
ammonia
solution
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CN106367603A (en
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张杜超
张新望
令红斌
杨天足
刘伟锋
陈霖
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Tangshan Hexing Waste Comprehensive Utilization Technology Co., Ltd.
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • 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
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C22B19/24—Obtaining zinc otherwise than by distilling with leaching with alkaline solutions, e.g. ammonia
    • 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
    • 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
    • C22B7/02—Working-up flue dust
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A kind of method of zinc in recovery blast furnace dust, gas ash is carried out coordination leaching by the present invention in the Leaching Systems that iminodiacetic acid ammonium sulfate ammoniacal liquor forms first, most of zinc is entered in solution, and suppress the dissolving of iron, realize the separation of zinc and iron in gas ash；For containing zinc lixiviating solution, carrying out ammonia still process and the absorption of ammonia, gained ammoniacal liquor returns to leaching process recycling；Liquid adjusts pH value of solution by adding dilute sulfuric acid after ammonia still process, recrystallizes the iminodiacetic acid in leachate and separates out, and liquid is solution of zinc sulfate after filtering gained separates out, and can reclaim zinc procedure connection with traditional solvent extraction electrodeposition.The present invention not only avoids corrosion of the highly acid system to leaching equipment, and the sodium zincate that it also avoid generating in strong basicity system is difficult to recovery problem.The leaching rate of zinc is more than 65%, and iron is not almost leached, and employs ammonium sulfate as one of mixed ligand leaching agent, and the dissolving of lead in gas ash, calcium impurities element is avoided in leaching process.

Description

A kind of method of zinc in recovery blast furnace dust
Technical field
The present invention relates to the hydrometallurgy process in field of metallurgy, particularly a kind of side for reclaiming zinc in blast furnace dust Method.
Technical background
Blast furnace dust is one kind secondary resource containing zinc that steel plant obtain when reclaiming flue dust during blast furnace ironmaking, its Mainly contain the elements such as Zn, Fe, Pb, Ca and Si.According to the difference of blast furnace raw material composition, in gas ash the content of zinc for 0.5~ 10%.Because China's iron and steel output is huge, and 10~15kg or so gas ash, therefore gas will be produced by often producing 1 ton of steel The yield of ash is also very huge, it is necessary to is acted upon.
In order to recycle iron therein, the method for conventional process blast furnace dust is using gas ash as raw materials for sintering weight It is new to return to blast fumance system.But in this closed circuit circulatory system, zinc can be accumulated gradually, and the property of its low melting point can be to blast furnace Produce and produce a series of detrimental effects, such as destroy blast furnace lining, block blast furnace flue gas increase in pipeline and cause gas ash certainly Combustion etc..Therefore, the recovery for realizing zinc in gas ash is very necessary.
The method of tradition recovery metallic zinc is broadly divided into pyrometallurgical smelting and the major class of hydrometallurgy two.Wherein occupy leading position Pyrometallurgical smelting method be watt Wurz method, this method is to be used as fuel by adding coke etc. and reducing agent makes zinc in gas ash Evaporated with simple substance form, and the iron rule in gas ash is retained in smelting slag, realizes the separation of zinc and iron.Pyrogenic attack Although blast furnace dust can obtain higher zinc recovery, this method can not only consume substantial amounts of energy, Er Qiehui A series of problems, such as causing environmental pollution, (Liu Jianhui, king are runed counter to current national energy-saving emission reduction and the policy for strengthening environmental protection Ancestral's honor Weirs hereby technique harmless treatment and the production practices Hunan's nonferrous metals for comprehensively utilizing material containing zinc, 2008,24 (6):16~18).
Some scholars also studied using wet-treating gas ash, i.e., using dilute sulfuric acid, (the sulfuric acid such as Huangping is from high tile Leaching Zinc, indium experimental study hydrometallurgys in this grey (mud), 2014,33 (5):365~367), sodium hydroxide (build, Yang Bao by hair Grow alkali leaching zinc and its dynamics research hydrometallurgys, 2014,33 (6) from gas ash:429~432) leached as leaching agent Zinc in gas ash, and then zinc is reclaimed from leachate using solvent extraction or ion-exchange.The advantages of wet method is pollution Small, consumption little energy.However, when using sulfuric acid leaching, not only can Leaching Zinc, while can also make substantial amounts of iron in gas ash Into in leachate, the purification difficulty of follow-up leachate is caused to increase.And when using sodium hydroxide as leaching agent, leachate Middle zinc can exist in the form of sodium zincate, cause the electrolysis of zinc in subsequent handling difficult.
Therefore, a kind of method for finding green and zinc efficiently being reclaimed from gas ash is very urgent.
The content of the invention
In order to overcome the shortcomings of existing blast furnace dust processing method, the present invention, which provides one kind, can efficiently reclaim high tile The method of zinc in this ash.
In order to achieve the above object, the technical solution adopted by the present invention is：Utilize matching somebody with somebody between zinc and iron and organic ligand The notable difference of capability realizes the separation of metallic zinc and iron in gas ash, and then zinc is reclaimed from leachate.First, gas ash Coordination leaching is carried out in the Leaching Systems of iminodiacetic acid-ammonium sulfate-ammoniacal liquor composition, most of zinc is entered in solution, And suppress the dissolving of iron, so as to realize the separation of zinc and iron in gas ash；For containing zinc lixiviating solution, carrying out ammonia still process and the suction of ammonia Receive, gained ammoniacal liquor returns to leaching process recycling；Liquid adjusts pH value of solution by adding appropriate dilute sulfuric acid after ammonia still process, makes leaching Iminodiacetic acid recrystallization in liquid separates out, and liquid is then solution of zinc sulfate after filtering gained separates out, and can extract with traditional solvent Take-electrodeposition recovery zinc process be connected.
Specific technical process and technological parameter are as follows：
1. collaboration coordination is leached
0.1~0.3mol/L iminodiacetic acid and 0.5~1mol/L ammonium sulfate are added first into pure water, will be soaked Go out liquid temperature degree and rise to 20 DEG C~60 DEG C, stirring dissolves iminodiacetic acid and ammonium sulfate.A certain amount of ammoniacal liquor is added, makes to mix It is 2 to close the mol ratio of ammonia and ammonium sulfate in coordination leachate：1, and it is 2~4mol/L to control total ammonia density.Soaked by mixed ligand It is 10~20 to go out liquid and blast furnace dust liquid-solid ratio：1, unit mL/g, addition blast furnace dust, control extraction time 100~ 140min, 20~60 DEG C of reaction temperature and mixing speed are 200~600r/min.After leaching terminates, filtering, obtain leaching containing zinc Liquid and leached mud.It can return to as raw materials for sintering after leached mud drying, be then further processed containing zinc lixiviating solution.
The main chemical reactions formula of leaching process is as follows：
ZnO+Ida2-+iNH3+H2O=[Zn (Ida) (NH3)i]+2OH- (1)
Zn2SiO4+2[Ida]2-+2iNH3+2H2O=2 [Zn (Ida) (NH3)i]+SiO2↓+4OH- (2)
2. the recovery of ammonia
To obtaining carrying out ammonia still process processing containing zinc lixiviating solution after leaching, it is 80~100 DEG C to control ammonia still process temperature, treats ammonia still process 1 ~2h, it is terminal that leachate volume, which is steamed to original 1/3~2/3,.Gained ammonia is inhaled in closed condensing unit using pure water Leaching process is can return to after receipts, liquid then carries out the recovery of iminodiacetic acid after gained ammonia still process.
3. the recovery of iminodiacetic acid
Liquid temperature degree is 80~100 DEG C after still keeping ammonia still process, adds appropriate 0.5~2mol/L dilute sulfuric acids regulation solution thereto PH value be 1.8~2.7, solution is cooled to room temperature after reacting 1~2h, iminodiacetic acid will crystallize precipitation.After filtering Obtained iminodiacetic acid precipitation can return to leaching process recycling, and the solution of zinc sulfate of gained can then be extracted by solvent Take-electrodeposition process recovery metallic zinc.
Described iminodiacetic acid, ammoniacal liquor, ammonium sulfate, sulfuric acid etc. are technical grade reagent.
The present invention is applied to caused blast furnace dust during blast furnace ironmaking, and its main component scope is with quality percentage Than being calculated as (wt%)：Zn 0.5~20%, Fe 30~60%, Pb 0.1~1.0%, Ca 0.5~10.0%.
It is of the invention compared with traditional processing method, have the advantage that：1. a mixed ligand Leaching Systems belongs to gentle anti- System is answered, not only avoids corrosion of the highly acid system to leaching equipment, it also avoid the sodium zincate generated in strong basicity system It is difficult to recovery problem；2. body series are coordinated objects system, using mixed ligand to the obvious of element zinc and iron mating capability Difference, the separation of the zinc and iron in gas ash being realized, the leaching rate of zinc is more than 65%, and iron is not almost leached, from And avoid cumbersome conventional wet iron removal step；3. a technique employs ammonium sulfate as one of mixed ligand leaching agent, because This, avoids the dissolving of lead in gas ash, calcium impurities element in leaching process；4. the technique can be by containing in zinc lixiviating solution Zinc is effectively separated with coordination leaching agent, is not only realized the high efficiente callback of coordination leaching agent with recycling, is advantageous to drop Low production cost, and gained solution of zinc sulfate can be connected with traditional solvent extraction-electrodeposition process after conversion, be advantageous to The subsequent recovery of zinc.
Brief description of the drawings
Fig. 1：Present invention process schematic flow sheet.
Embodiment
Embodiment 1
Blast furnace dust main component is by percentage to the quality：Zn 5.103%, Fe 38.49%, Pb 0.94%, Ca 3.00%.Technical grade iminodiacetic acid, wherein iminodiacetic acid (butt) >=95%, chloride (in terms of NaCl)≤ 0.10%, water-insoluble≤0.20%；Technical grade sulfuric acid ammonium, wherein nitrogen content >=20.5%, moisture≤1.0%；Technical grade ammonia Water, wherein NH3>=25%；Technical grade sulfuric acid, wherein H2SO4>=98.0%.
Iminodiacetic acid 5.6g is weighed, ammonium sulfate 28g, measures ammoniacal liquor 30mL, is added into 150mL pure water, temperature adds Heat is to 40 DEG C, and stirring and dissolving is settled to 200mL, and preparation turns into mixed ligand leachate.Blast furnace dust 10g is weighed, addition is matched somebody with somebody In good leachate, regulation mixing speed is 400r/min, temperature is maintained at 40 DEG C, extraction time 120min.Reaction terminates After filter, gained volume containing zinc lixiviating solution is 190ml, and its constituent concentration is：Zn 1.74g/L, Fe 0.01g/L, Pb 0.012g/L, Ca 0.002g/L.Leached mud drying after weight is referred to as 9.19g, its main component is：Zn 1.96%, Fe 41.86%, Pb 0.01%, Ca 3.26%.In the leaching process, the leaching rate of zinc is 64.73%, and the leaching rate of iron is 0.05%, the leaching rate of lead is 0.02%, and the leaching rate of calcium is 0.1%.
Zinc lixiviating solution will be contained to add in ammonia steaming device, open cooling water circulation, pure water volume is used in absorbing ammonia steam 100mL, heating leachate make its temperature be maintained at 90 DEG C or so, stop heating after 2 hours.Liquid product is 90mL after ammonia still process. Gained ammoniacal liquor can return to leaching process use after reaching industrial standard.
After ammonia still process terminates, liquid temperature degree is 90 DEG C after keeping ammonia still process, is slowly added to 1mol/L dilute sulfuric acids about 9mL, pH thereto It is down to 2.2.Now there is substantial amounts of white iminodiacetic acid Precipitation.Liquid to be leached is cooled to room temperature, filters, drying, institute It is 5.41g to obtain white solid weight.The solution of zinc sulfate volume being filtrated to get is 98ml, and main component is：Zn 3.36g/L, Fe0.019g/L, Pb 0.023g/L, Ca 0.004g/L, iminodiacetic acid 8.04g/L.Calculate the rate of recovery of zinc is 64.53%, the rate of recovery of iminodiacetic acid is 85.93%.
Embodiment 2
Blast furnace dust main component is by percentage to the quality：Zn 0.934%, Fe 41.64%, Pb 0.32%, Ca 9.70%.Technical grade iminodiacetic acid, wherein iminodiacetic acid (butt) >=95%, chloride (in terms of NaCl)≤ 0.10%, water-insoluble≤0.20%；Technical grade sulfuric acid ammonium, wherein nitrogen content >=20.5%, moisture≤1.0%；Technical grade ammonia Water, wherein NH3>=25%；Technical grade sulfuric acid, wherein H2SO4>=98.0%.
Iminodiacetic acid 2.8g is weighed, ammonium sulfate 14g, measures ammoniacal liquor 15mL, is added into 80mL pure water, temperature heating To 40 DEG C, stirring and dissolving constant volume, 200mL mixed ligand leachates are configured to.Blast furnace dust 10g is weighed, adds mixed ligand In leachate, regulation mixing speed is 400r/min, and temperature is maintained at 40 DEG C.Extraction time is 120min.Mistake after reaction terminates Filter, gained volume containing zinc lixiviating solution is 100ml, and its constituent concentration is：Zn 0.65g/L, Fe 0.046g/L, Pb 0.032mg/ L, Ca 0.007g/L.Leached mud drying after weight is referred to as 9.12g, its main component is：Zn 0.31%, Fe 45.16%, Pb 0.35%, Ca10.63%.It is computed, in the leaching process, the leaching rate of zinc is 69.40%, and the leaching rate of iron is 0.11%, the leaching rate of lead is 0.01%, and the leaching rate of calcium is 0.07%.
Leachate is added in ammonia steaming device, wherein, pure water volume used in ammonia vapor absorption is 100mL.Heat leachate To 90 DEG C, stop heating after 2 hours of ammonia still process.Now liquid product is 45mL after ammonia still process.After multiple ammonia still process operation, ammoniacal liquor is reachable To industrial standard, return to leaching process and use.
After ammonia still process terminates, it is 90 DEG C to keep leachate temperature, is slowly added to 1mol/L dilute sulfuric acids 5mL thereto, and pH is down to 2.1, iminodiacetic acid is separated out with white precipitate.Liquid to be leached filters after being cooled to room temperature, drying precipitation, weight is referred to as 2.8g.50mL solution of zinc sulfate is filtrated to get, its main component is：Zn 1.30g/L, Fe 0.092g/L, Pb 0.064mg/L, Ca 0.014g/L, iminodiacetic acid 6.57g/L.Calculate zinc the rate of recovery be 69.33%, the recovery of iminodiacetic acid Rate is 88.76%.

Claims (3)

  1. A kind of 1. method for reclaiming zinc in blast furnace dust, it is characterised in that comprise the following steps：
    A collaboration coordinations are leached
    0.1~0.3mol/L iminodiacetic acid and 0.5~1mol/L ammonium sulfate are added first into pure water, by leachate Temperature rises to 20 DEG C~60 DEG C, and stirring dissolves iminodiacetic acid and ammonium sulfate, adds ammoniacal liquor, makes mixed ligand leachate The mol ratio of middle ammonia and ammonium sulfate is 2：1, and it is 2~4mol/L to control total ammonia density, by mixed ligand leachate and high tile This grey liquid-solid ratio is 10~20：1, unit mL/g, add blast furnace dust, 100~140min of control extraction time, reaction temperature 20~60 DEG C of degree and mixing speed are 200~600r/min, after leaching terminates, filtering, obtain containing zinc lixiviating solution and leached mud, contain Zinc lixiviating solution is then further processed；
    The recovery of B ammonia
    To obtaining carrying out ammonia still process processing containing zinc lixiviating solution after leaching, it is 80~100 DEG C to control ammonia still process temperature, treats 1~2h of ammonia still process, It is terminal that leachate volume, which is steamed to original 1/3~2/3,；Gained ammonia returns after using absorbing pure water in closed condensing unit Return and leach process, liquid then carries out the recovery of iminodiacetic acid after gained ammonia still process；
    The recovery of C iminodiacetic acids
    Liquid temperature degree is 80~100 DEG C after keeping ammonia still process, and the pH value for adding 0.5~2mol/L dilute sulfuric acids regulation solution thereto is Solution is cooled to room temperature after 1.8~2.7,1~2h of reaction, iminodiacetic acid will crystallize precipitation；The Asia obtained after filtering Aminodiacetic acid precipitation returns to leaching process recycling, and the solution of zinc sulfate of gained is then returned by solvent extraction-electrodeposition process Receive metallic zinc.
  2. 2. the method for zinc in blast furnace dust is reclaimed as claimed in claim 1, it is characterised in that：Described iminodiacetic acid (salt) Acid, ammoniacal liquor, ammonium sulfate and sulfuric acid are technical grade reagent.
  3. 3. the method for zinc in blast furnace dust is reclaimed as claimed in claim 1, it is characterised in that：Described blast furnace ironmaking process In caused blast furnace dust, main component scope is by percentage to the quality：Zn 0.5~20%, Fe 30~60%, Pb 0.1~1.0%, Ca 0.5~10.0%.
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CN111979420B (en) * 2019-05-24 2021-09-17 东北大学 Comprehensive utilization method of blast furnace gas ash
CN110218872A (en) * 2019-06-04 2019-09-10 王俊英 A kind of pyrogenic process enrichment-wet separation multistage coupling integration processing method
CN112126792B (en) * 2020-08-28 2022-06-21 江苏大学 Method for zinc hydrometallurgy of zinc calcine in short process

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JP3080947B1 (en) * 1999-02-05 2000-08-28 日本磁力選鉱株式会社 Electric furnace dust treatment method
CN104762473B (en) * 2015-04-29 2016-09-28 中南大学 A kind of method leaching low-grade zinc oxide ore

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Address after: 063100 No. 3 Hongbei Road, Guye Economic Development Zone, Tangshan City, Hebei Province

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Address before: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932

Patentee before: Central South University