CN108486383A - A kind of method of zinc oxide fumes high efficiency extraction zinc germanium - Google Patents
A kind of method of zinc oxide fumes high efficiency extraction zinc germanium Download PDFInfo
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- CN108486383A CN108486383A CN201810417628.XA CN201810417628A CN108486383A CN 108486383 A CN108486383 A CN 108486383A CN 201810417628 A CN201810417628 A CN 201810417628A CN 108486383 A CN108486383 A CN 108486383A
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- germanium
- zinc oxide
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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
- C22B7/02—Working-up flue dust
-
- 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
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
-
- 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
- C22B41/00—Obtaining germanium
-
- 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
- C22B7/007—Wet processes by acid leaching
-
- 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
The present invention relates to a kind of methods of zinc oxide fumes high efficiency extraction zinc germanium, belong to smelting field of nonferrous metal, and the present invention uses two sections of counterflow leachings, specifically includes following steps:1)I section of atmospheric low-temperature Weak-acid leaching:Zinc oxide fumes and sulfuric acid solution are subjected to normal pressure acid-leaching reaction, I section of leachate and I section of leached mud are obtained after solid-liquor separation, send zinc germanium system to carry out zinc germanium recycling I section of leachate;2)II section of oxygen forces down warm high acidic oils:I section of leached mud and the useless electric effusion of zinc are subjected to oxygen under an increased pressure and press acid-leaching reaction, II leachate and II section of leached mud are obtained after solid-liquor separation, by II section of leachate return to step 1)In, it is used for the normal pressure acidleach of zinc oxide fumes, II section of leached mud is sent to lead smelting system recycling lead silver;The method and process of the present invention is simple, zinc germanium leaching rate is high, energy consumption is relatively low, equipment investment is few, it is environmental-friendly, be easy to and prior art is mating dock realization industrialized production.
Description
Technical field
The invention belongs to smelting field of nonferrous metal, specifically, are related to a kind of zinc oxide fumes high efficiency extraction zinc germanium
Method.
Background technology
In Lead-zinc Smelting Enterprises, zinc oxide fumes are a kind of important secondary resources, but zinc oxide fumes property is changeable, no
The property for generating flue dust with enterprise also has difference.
The form that is primarily present of zinc is zinc oxide, zinc sulfate and zinc sulphide in usual zinc oxide fumes, zinc oxide and sulfuric acid
Zinc can be leached into solution under normal pressure acid condition, be difficult to leach under zinc sulphide condition of normal pressure, cause conventional treatment process
Zinc leaching rate is relatively low.The existence form of germanium is complex in zinc oxide fumes, has soluble germanium and property germanium hard to tolerate, soluble germanium normal
Rule technique can leach, and there are no methods to leach completely for slightly solubility germanium.
Currently, the related patents of zinc oxide fumes treatment process are substantially based on defluorinate chlorine both at home and abroad, in small part technique
The comprehensive reutilization of valuable metal zinc germanium is realized using conventional treatment process;Also have and germanium-containing material is handled using pressure leaching
(Lead concentrate, zinc concentrate etc.), but it is different from zinc oxide fumes property.Zinc oxide fumes conventional treatment process is to use two sections at present
It leaching, one section of neutrality and two sections of acidic leachings, generally speaking, conventional treatment process zinc germanium leaching rate is relatively low, zinc leaching rate 80 ~
90%, germanium leaching rate 50 ~ 70% causes the zinc oxide fumes zinc germanium rate of recovery low, and two sections of slag germanium containing zinc cause zinc germanium loss big compared with high.
Invention content
In order to solve the problems, such as background technology, the present invention provides a kind of zinc oxide fumes high efficiency extraction zinc germanium
Method, two sections of counterflow leaching techniques that warm high acidic oils are forced down in conjunction with atmospheric low-temperature Weak-acid leaching and oxygen are high from zinc oxide fumes
Effect extraction zinc and germanium, technological process is simple, zinc germanium leaching rate is high, low energy consumption, environmentally protective, is easy to and existing lead-zinc smelting principal series
Set under unified central planning linking, zinc and germanium that can utmostly in comprehensive reutilization zinc oxide fumes, improves the rate of recovery of valuable metal, drops
Low production cost.
To achieve the above object, the present invention is achieved through the following technical solutions:
The method of the zinc oxide fumes high efficiency extraction zinc germanium, specifically includes following steps:
1)I section of atmospheric low-temperature Weak-acid leaching:Zinc oxide fumes are mixed progress leaching with sulfuric acid solution to react, solid-liquor separation
After obtain I section of leachate and I section of leached mud;
2)II section of oxygen forces down warm high acidic oils:By step 1)In I section of leached mud mixed with useless electric effusion, it is appropriate to adjust acid, be added
II section of oxygen is carried out in autoclave and presses acid-leaching reaction, and II section of leachate and II section of leached mud, II section of leached mud are obtained after solid-liquor separation
Cleaning solution and II section of washed-residue are obtained after three sections of countercurrent washings, solid-liquor separations;II section of leachate and cleaning solution are mixed, adjust acid simultaneously
After adding water to adjust volume I section of atmospheric low-temperature Weak-acid leaching process is returned to as sulfuric acid solution;
3)I section of leachate is sent to germanium zinc abstraction system and recycles zinc and germanium, II section of washed-residue enters lead smelting system recycling lead.
Further, step 1)In, sulfuric acid solution dosage be by 0. 3 ~ 1.0 times of lead zinc gauge sulfuric acid theoretical consumption,
The liquid-solid ratio of sulfuric acid solution and zinc oxide fumes is 2 ~ 6:1.
Further, step 1)In, I section of atmospheric low-temperature Weak-acid leaching condition:Reaction temperature is 20 ~ 90 DEG C, the reaction time
For 10-120min, control reaction end pH1.0 ~ 3.0.
Further, step 2)In, sulfuric acid concentration is 120 ~ 200g/L in the electric effusion that gives up, and zinc concentration is 40 ~ 70g/L.
Further, step 2)In, the liquid-solid ratio of useless electric effusion and I section of leached mud is 2 ~ 7:1.
Further, step 2)In, appropriate tune acid refers to pressing I with sulfuric acid including the sulfuric acid content in waste electrolyte
1.4 ~ 1.8 times of dosage of section Zinc in Leaching Residue gauge sulfuric acid theoretical consumption carries out adjusting acid.
Further, step 2)In, II section of oxygen forces down warm high acidic oils condition:Control kettle in oxygen pressure be 0.1 ~
0.9MPa, reaction temperature are 40 ~ 95 DEG C, and the reaction time is 0.5 ~ 6h.
Further, step 2)In, acid is 40 ~ 95g/L to II section of leachate eventually.
Further, step 3)In, it refers to I section of leachate warp that I section of leachate, which is sent to cadmia smelting system Ti recovery and zinc,
Dearsenification, heavy germanium obtain liquid after germanic slag and heavy germanium, and germanic slag leaching handles to obtain germanium concentrate, and liquid is sent to zinc abstraction system after heavy germanium.
Beneficial effects of the present invention:
1, using two sections of counterflow leaching techniques of " low-II section of oxygen of acidleach of I section of normal pressure forces down the high acidleach of temperature ", zinc oxide cigarette can be realized
The efficient leaching of zinc and germanium in dirt, for zinc leaching rate up to 98% or more, germanium leaching rate solves regular oxidation zinc up to 85% or more
The low problem of the zinc germanium leaching rate of dust treatment technology.
2, this method is related to reaction can carry out at a lower temperature, reduce energy consumption;Technological process is simple, existing lead zinc
Smelting system main flow is easy mating linking, is easy to industrializing implementation;Environmentally protective, equipment investment is few, and production cost is low.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
It, below will be to the preferred reality of the present invention in order to keep the purpose of the present invention, technical solution and advantageous effect clearer
It applies example to be described in detail, to facilitate the technical staff to understand.
Embodiment 1
The main component of the present embodiment zinc oxide fumes is:Zn44.54%、Pb19.83%、Fe3.56%、、S5.06%、
Ge666.70g/t。
By 600g zinc oxide fumes and sulfuric acid solution containing zinc(Zn105g/L, H2SO4114g/L)Mixing, in condition:Sulfuric acid is used
Amount is by 0.75 times, liquid-solid ratio 5 of lead zinc gauge sulfuric acid theoretical consumption:1, it is reacted under temperature 60 C, time 0.5h, instead
After should completing I section of leachate and I section of leached mud are obtained through solid-liquor separation.The whole acid 5.73g/L of I section of leachate, I section of Zinc in Leaching Residue
13.56%, germanic 336.4g/t, I section of zinc, germanium leaching rate are respectively 85.40% and 76.15%.
I section of leached mud is mixed with useless electric effusion(Useless electric effusion main component is Zn51.21g/L, H2SO4154.31g/L、
Mn4.14g/L), in condition:Sulfuric acid dosage is 1.6 times, liquid-solid ratio 5 by lead zinc gauge sulfuric acid theoretical consumption:1, temperature 95
DEG C, oxygen pressure 0.8MPa, reacted under time 3h, reaction through solid-liquor separation obtains II section of leachate and II section of leaching after completing
Slag.II section of leachate H2SO486.75g/L, II section of Zinc in Leaching Residue 1.56%, germanic 244.35g/t.It is leached through two sections, the leaching of zinc germanium
Extracting rate is respectively 98.64%, 85.80%.
Embodiment 2
The main component of the present embodiment zinc oxide fumes is:Zn50.79%、Pb16.85%、Fe1.52%、、S8.13%、
Ge1112.40g/t。
By 600g zinc oxide fumes and sulfuric acid solution containing zinc(Zn113g/L, H2SO4158g/L)Mixing, in condition:Sulfuric acid is used
Amount is by 0.75 times, liquid-solid ratio 4 of lead zinc gauge sulfuric acid theoretical consumption:1, it is reacted under 80 DEG C of temperature, time 0.5h, instead
After should completing I section of leachate and I section of leached mud are obtained through solid-liquor separation.The whole acid 7.86g/L of I section of leachate, I section of Zinc in Leaching Residue
11.79%, germanic 477.4g/t, I section of zinc, germanium leaching rate are respectively 88.20% and 78.19%.
I section of leached mud is mixed with useless electric effusion(Useless electric effusion main component is Zn51.21g/L, H2SO4154.31g/L、
Mn4.14g/L), in condition:Sulfuric acid dosage is 1.8 times, liquid-solid ratio 4 by lead zinc gauge sulfuric acid theoretical consumption:1, temperature 60
DEG C, oxygen pressure 0.8MPa, reacted under time 2h, reaction through solid-liquor separation obtains II section of leachate and II section of leaching after completing
Slag.II section of leachate H2SO494.36g/L, II section of Zinc in Leaching Residue 0.78%, germanic 372.1g/t.It is leached through two sections, the leaching of zinc germanium
Extracting rate is respectively 99.40%, 87.01%.
The main technological route of the present invention is as follows:Zinc oxide fumes are reacted by I section of normal pressure Weak-acid leaching, by zinc oxide cigarette
Acid-soluble zinc and most of soluble germanium leaching are transferred to I section of leachate in dirt, and I section of leachate send to zinc germanium recovery system and recycle
Zinc germanium;I section of leached mud and the zinc electric effusion that gives up are blended in autoclave and carry out II oxygen and force down warm high acidic oils react, will hardly possible under normal pressure
The zinc sulphide leaching of leaching is transferred to solution, and II section of leachate is containing acid I section of leaching for being used for zinc oxide fumes of higher return, II section of leaching
Wash heat is sent after washing to lead smelting system recycling lead silver.In this technical solution, in zinc oxide fumes zinc leaching rate up to 98% with
On, germanium leaching rate is up to 85% or more.
Finally illustrate, preferred embodiment above is only used to illustrate the technical scheme of the present invention and unrestricted, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (9)
1. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium, it is characterised in that:Specifically include following steps:
1)I section of atmospheric low-temperature Weak-acid leaching:Zinc oxide fumes are mixed progress leaching with sulfuric acid solution to react, solid-liquor separation
After obtain I section of leachate and I section of leached mud;
2)II section of oxygen forces down warm high acidic oils:By step 1)In I section of leached mud mixed with useless electric effusion, it is appropriate to adjust acid, be added
II section of oxygen is carried out in autoclave and presses acid-leaching reaction, and II section of leachate and II section of leached mud, II section of leached mud are obtained after solid-liquor separation
Cleaning solution and II section of washed-residue are obtained after three sections of countercurrent washings, solid-liquor separations;II section of leachate and cleaning solution are mixed, adjust acid simultaneously
After adding water to adjust volume I section of atmospheric low-temperature Weak-acid leaching process is returned to as sulfuric acid solution;
3)I section of leachate is sent to germanium zinc abstraction system and recycles zinc and germanium, II section of washed-residue enters lead smelting system recycling lead.
2. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 1)
In, sulfuric acid solution dosage be by 0. 3 ~ 1.0 times of lead zinc gauge sulfuric acid theoretical consumption, sulfuric acid solution and zinc oxide fumes
Liquid-solid ratio is 2 ~ 6:1.
3. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 1)
In, I section of atmospheric low-temperature Weak-acid leaching condition:Reaction temperature is 20 ~ 90 DEG C, reaction time 10-120min, controls reaction end
pH1.0~3.0。
4. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 2)
In, sulfuric acid concentration is 120 ~ 200g/L in the electric effusion that gives up, and zinc concentration is 40 ~ 70g/L.
5. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 2)
In, the liquid-solid ratio of useless electric effusion and I section of leached mud is 2 ~ 7:1.
6. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 2)
In, appropriate tune acid refers to including the sulfuric acid content in waste electrolyte, with sulfuric acid by I section of Zinc in Leaching Residue gauge sulfuric acid theory
1.4 ~ 1.8 times of dosage of consumption carries out adjusting acid.
7. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 2)
In, II section of oxygen forces down warm high acidic oils condition:It is 0.1 ~ 0.9MPa to control oxygen pressure in kettle, and reaction temperature is 40 ~ 95 DEG C, instead
It is 0.5 ~ 6h between seasonable.
8. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 2)
In, acid is 40 ~ 95g/L to II section of leachate eventually.
9. a kind of method of zinc oxide fumes high efficiency extraction zinc germanium according to claim 1, it is characterised in that:Step 3)
In, I section of leachate is sent to cadmia smelting system Ti recovery and zinc, and to refer to I section of leachate obtain germanic slag and heavy through dearsenification, heavy germanium
Liquid after germanium, germanic slag leaching handle to obtain germanium concentrate, and liquid is sent to zinc abstraction system after heavy germanium.
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111961869A (en) * | 2020-09-13 | 2020-11-20 | 湖北大江环保科技股份有限公司 | Non-ferrous smelting waste recovery system and use method thereof |
CN114317986A (en) * | 2021-11-30 | 2022-04-12 | 西安建筑科技大学 | Process for extracting lead from zinc-lead dust |
CN114836627A (en) * | 2022-06-01 | 2022-08-02 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of indium-containing zinc oxide smoke dust |
CN115011801A (en) * | 2022-01-21 | 2022-09-06 | 昆明理工大学 | Method for ultrasonically enhancing germanate leaching in zinc oxide smoke dust |
CN115216651A (en) * | 2022-09-06 | 2022-10-21 | 昆明冶金研究院有限公司 | Method for efficiently recycling zinc and germanium in zinc oxide smoke dust |
CN115261643A (en) * | 2022-08-03 | 2022-11-01 | 昆明理工大学 | Method for enhancing deep leaching of germanium in germanium-containing zinc oxide smoke dust by countercurrent ultrasonic |
CN115386732A (en) * | 2022-09-06 | 2022-11-25 | 昆明冶金研究院有限公司 | Method for efficiently recycling zinc, germanium and indium in zinc oxide smoke dust |
CN115874058A (en) * | 2023-03-02 | 2023-03-31 | 昆明理工大学 | Method for efficiently enriching germanium by pre-dezincification and neutralization of zinc oxide smoke dust containing germanium |
CN116574908A (en) * | 2023-04-03 | 2023-08-11 | 西部矿业股份有限公司 | Process for jointly recycling zinc and indium by means of open-circuit impurity removal of electrolyte in zinc smelting process |
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CN103060552A (en) * | 2013-01-30 | 2013-04-24 | 昆明理工大学 | Method for extracting valuable metals from neutral leaching residue of zinc oxide |
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CN111961869A (en) * | 2020-09-13 | 2020-11-20 | 湖北大江环保科技股份有限公司 | Non-ferrous smelting waste recovery system and use method thereof |
CN114317986A (en) * | 2021-11-30 | 2022-04-12 | 西安建筑科技大学 | Process for extracting lead from zinc-lead dust |
CN114317986B (en) * | 2021-11-30 | 2023-10-13 | 西安建筑科技大学 | Process for extracting lead from zinc-lead dust |
CN115011801A (en) * | 2022-01-21 | 2022-09-06 | 昆明理工大学 | Method for ultrasonically enhancing germanate leaching in zinc oxide smoke dust |
CN115011801B (en) * | 2022-01-21 | 2024-06-07 | 昆明理工大学 | Method for leaching germanate in ultrasonic reinforced zinc oxide smoke dust |
CN114836627A (en) * | 2022-06-01 | 2022-08-02 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of indium-containing zinc oxide smoke dust |
CN114836627B (en) * | 2022-06-01 | 2024-01-30 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method for indium-containing zinc oxide smoke dust |
CN115261643A (en) * | 2022-08-03 | 2022-11-01 | 昆明理工大学 | Method for enhancing deep leaching of germanium in germanium-containing zinc oxide smoke dust by countercurrent ultrasonic |
CN115261643B (en) * | 2022-08-03 | 2024-02-06 | 昆明理工大学 | Method for deep leaching of germanium in countercurrent ultrasonic reinforced germanium-containing zinc oxide smoke dust |
CN115216651A (en) * | 2022-09-06 | 2022-10-21 | 昆明冶金研究院有限公司 | Method for efficiently recycling zinc and germanium in zinc oxide smoke dust |
CN115386732A (en) * | 2022-09-06 | 2022-11-25 | 昆明冶金研究院有限公司 | Method for efficiently recycling zinc, germanium and indium in zinc oxide smoke dust |
CN115874058A (en) * | 2023-03-02 | 2023-03-31 | 昆明理工大学 | Method for efficiently enriching germanium by pre-dezincification and neutralization of zinc oxide smoke dust containing germanium |
CN116574908A (en) * | 2023-04-03 | 2023-08-11 | 西部矿业股份有限公司 | Process for jointly recycling zinc and indium by means of open-circuit impurity removal of electrolyte in zinc smelting process |
CN116574908B (en) * | 2023-04-03 | 2024-03-12 | 西部矿业股份有限公司 | Process for jointly recycling zinc and indium by means of open-circuit impurity removal of electrolyte in zinc smelting process |
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Application publication date: 20180904 |