CN113667834A - Method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation - Google Patents

Method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation Download PDF

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CN113667834A
CN113667834A CN202110960394.5A CN202110960394A CN113667834A CN 113667834 A CN113667834 A CN 113667834A CN 202110960394 A CN202110960394 A CN 202110960394A CN 113667834 A CN113667834 A CN 113667834A
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leaching
dust
oxygen
zinc
temperature
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张新智
杨尚聪
杨学贵
杨智娟
覃刚
颜茂昌
杨晓冬
熊云
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Yunnan Jinding Zinc Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/30Obtaining zinc or zinc oxide from metallic residues or scraps
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/08Sulfides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/20Obtaining zinc otherwise than by distilling
    • C22B19/22Obtaining zinc otherwise than by distilling with leaching with acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/16Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Metallurgy (AREA)
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Abstract

The invention discloses a method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation, and relates to the technical field of zinc hydrometallurgy. The invention comprises the following steps: s1: laying aeration pipes on the upper, middle and lower layers in the leaching tank; s2: cooling the acidic oxidant liquid; s3: putting the cooled acidic oxidant liquid into a leaching tank; s4: adding the calcine dust collected from the mineral roasting dust settling tower into a leaching tank, continuously stirring by using stirring equipment in the adding process, uniformly mixing the calcine dust into an acid oxidant, and carrying out primary normal-pressure low-temperature acid leaching. The invention utilizes the existing roasting sand dust high-temperature peracid leaching section operation tank, leaches zinc sulfide which is not leached originally by introducing oxygen for oxidation in the leaching process, completes the whole process of zinc production by combining the original procedures of purification, electrolysis and casting, and solves the problem that the zinc in the roasting sand dust is difficult to be leached completely by the existing roasting sand dust high-temperature peracid leaching operation.

Description

Method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation
Technical Field
The invention belongs to the technical field of zinc hydrometallurgy, and particularly relates to a method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation.
Background
The zinc hydrometallurgy is a process of dissolving zinc in zinc calcine or other zinc sulfide materials and zinc in zinc sulfide concentrate in an aqueous solution and extracting metal zinc or zinc compounds from the zinc calcine or other zinc sulfide materials and zinc sulfide concentrate, and is a modern zinc hydrometallurgy main method which comprises three large links of zinc leaching, purification from a zinc solution and zinc electrolytic deposition, and the zinc hydrometallurgy mainly comprises the working procedures of roasting, leaching, leachate purification, electrodeposition and the like.
In the roasting procedure, the flotation zinc sulfide concentrate is roasted through a roasting furnace, but the roasting process is difficult to completely roast, so the produced roasted dust often contains part of zinc sulfide metal, and the zinc sulfide metal needs to be recycled.
In the prior art, the roasted sand dust is leached by normal-pressure acid leaching, but zinc in the roasted sand dust is difficult to leach completely, and the leached slag has high zinc content, so that zinc resources are difficult to recycle, resources are wasted, and the cost is increased indirectly.
Therefore, the existing method for leaching zinc sulfide from calcine dust under normal pressure cannot meet the requirements in practical use, so that an improved technology is urgently needed in the market to solve the problems.
Disclosure of Invention
The invention aims to provide a method for leaching zinc sulfide in roasted sand dust under normal pressure by using oxygen oxidation, which utilizes the existing operation tank of the high-temperature and high-acid leaching section of the roasted sand dust to leach out zinc sulfide which is not leached originally by introducing oxygen for oxidation in the leaching process and combines the original procedures of purification, electrolysis and casting to complete the whole process of zinc production, thereby solving the problem that the zinc in the roasted sand dust is difficult to be leached completely by the existing high-temperature and high-acid leaching operation of the roasted sand dust.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation, which comprises the following steps:
s1: laying aeration pipes on the upper, middle and lower layers in the leaching tank;
s2: cooling the acidic oxidant liquid;
s3: putting the cooled acidic oxidant liquid into a leaching tank;
s4: adding the calcine dust collected from the mineral roasting dust settling tower into a leaching tank, continuously stirring by using stirring equipment in the adding process to enable the calcine dust to be uniformly mixed into an acid oxidant, and carrying out primary normal-pressure low-temperature acid leaching;
s5: introducing oxygen for oxidation in a section of normal-pressure low-temperature acid leaching process, assisting in acid leaching, continuously stirring through stirring equipment, and leaching for 0.5-1 h;
s6: then heating, and carrying out two-stage normal-pressure high-temperature acid leaching under the condition of high-temperature high-acid stirring;
s7: introducing oxygen for oxidation in the two-stage normal-pressure high-temperature acid leaching process, assisting in acid leaching, continuously stirring through stirring equipment, leaching for 2-3 hours, and completely leaching zinc in the roasted sand dust;
s8: and purifying, electrolyzing and casting the leaching solution to recycle the zinc.
Further, S1 middle and lower layer aeration pipes are arranged at the bottom of the tank, upper layer aeration pipes are arranged at positions 20cm away from the liquid level, the upper layer aeration pipes, the middle and lower layers are distributed in the leaching tank at equal intervals, the upper layer aeration pipes, the middle and lower layers are arranged, the contact surface of liquid and oxygen is increased, the speed of oxygen dissolving into water can be increased, the dissolved oxygen amount of the liquid is rapidly increased, and the aeration effect is increased.
Further, the temperature of the acidic oxidant liquid after the temperature reduction treatment in S2 is set to 10 to 12 ℃, and the lower the water temperature is, the higher the content of dissolved oxygen in water is, so that the temperature reduction treatment of the acidic oxidant liquid can increase the dissolved amount of oxygen, so that the oxygen is sufficiently dissolved.
Further, the liquid-solid ratio of the acidic oxidant liquid to the roasted sand dust in S4 is set to 8-10: 1, and the leaching effect of the roasted sand dust is improved in a high-acid environment.
Further, the temperature of the second-stage normal-pressure high-temperature acid leaching in the S6 is kept at 85-90 ℃, and the leaching effect of the roasted sand dust is improved in a high-temperature environment.
Further, oxygen gas introduced into S5 and S7 is pure oxygen, and the upper aeration flow rate is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3And each layer is provided with reasonable aeration flow, so that oxygen can be saved, and the utilization rate of the oxygen is improved.
Furthermore, the acidity of the leaching end point is controlled to be more than 20 g/L.
And further, detecting the zinc content of the leaching residue in the step S8, and putting the leaching residue with the excessive zinc content into a leaching tank for two-stage normal-pressure high-temperature acid leaching.
The invention has the following beneficial effects:
1. the invention utilizes the existing high-temperature and high-acid leaching section operation tank for roasted sand dust, and introduces oxygen to oxidize in the leaching process, so as to leach out zinc sulfide which is not leached originally, and combines the original procedures of purification, electrolysis and casting to complete the whole process of zinc production, so that zinc in the roasted sand dust can be leached thoroughly, the zinc content in slag is greatly reduced, the recycling of zinc is completed, the comprehensive utilization of resources is effectively improved, and a new idea is provided for zinc wet smelting.
2. The aeration pipe is provided with the upper layer, the middle layer and the lower layer, so that the contact surface between liquid and oxygen is increased, the speed of dissolving oxygen into water can be increased, the dissolved oxygen amount of the liquid is rapidly increased, the aeration effect is increased, and each layer is provided with reasonable aeration flow, so that oxygen can be saved, and the utilization rate of the oxygen is increased.
3. The process method adopts the first-stage normal-pressure low-temperature acid leaching and the second-stage normal-pressure high-temperature acid leaching, improves the dissolution amount of oxygen by reducing the temperature of the acidic oxidant liquid, fully dissolves oxygen, fully reacts the roasted sand dust and the acidic oxidant by heating, and improves the leaching effect.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example one
Referring to fig. 1, the present invention is a method for atmospheric leaching of zinc sulfide from calcine dust by oxygen oxidation, comprising the following steps:
s1: aeration pipes are laid in the upper, middle and lower layers in the leaching tank, the lower layer aeration pipe is arranged at the bottom of the tank, the upper layer aeration pipe is arranged at a position 20cm away from the liquid level, and the upper, middle and lower layers of aeration pipes are distributed in the leaching tank at equal intervals;
s2: cooling the acidic oxidant liquid to 10 ℃;
s3: putting the cooled acidic oxidant liquid into a leaching tank;
s4: adding the calcine dust collected from the mineral roasting dust settling tower into a leaching tank, continuously stirring by using stirring equipment in the adding process to enable the calcine dust to be uniformly mixed into an acidic oxidant, and carrying out primary normal-pressure low-temperature acid leaching, wherein the liquid-solid ratio of the acidic oxidant liquid to the calcine dust is set to be 8: 1;
s5: introducing oxygen for oxidation in a section of normal-pressure low-temperature acid leaching process, assisting in acid leaching,continuously stirring by stirring equipment, leaching for 0.5h, wherein the introduced oxygen is pure oxygen, and the upper layer aeration flow is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3/h;
S6: heating, and carrying out second-stage normal-pressure high-temperature acid leaching under the condition of high-temperature high-acid stirring, wherein the temperature of the second-stage normal-pressure high-temperature acid leaching is kept at 85 ℃;
s7: introducing oxygen for oxidation in the two-stage normal-pressure high-temperature acid leaching process, performing auxiliary acid leaching, continuously stirring by using stirring equipment, leaching for 2h, and completely leaching zinc in the roasted sand dust, wherein the introduced oxygen is pure oxygen, and the aeration flow of the upper layer is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3Controlling the acidity of the leaching end point to be more than 20 g/L;
s8: and (3) purifying, electrolyzing and casting the leachate to recycle zinc, detecting the zinc content of the leached residues, and putting the leached residues with overhigh zinc content into a leaching tank to carry out two-stage normal-pressure high-temperature acid leaching.
Example two
Referring to fig. 1, the present invention is a method for atmospheric leaching of zinc sulfide from calcine dust by oxygen oxidation, comprising the following steps:
s1: aeration pipes are laid in the upper, middle and lower layers in the leaching tank, the lower layer aeration pipe is arranged at the bottom of the tank, the upper layer aeration pipe is arranged at a position 20cm away from the liquid level, and the upper, middle and lower layers of aeration pipes are distributed in the leaching tank at equal intervals;
s2: cooling the acidic oxidant liquid to 11 ℃;
s3: putting the cooled acidic oxidant liquid into a leaching tank;
s4: adding the calcine dust collected from the mineral roasting dust settling tower into a leaching tank, continuously stirring by using stirring equipment in the adding process to enable the calcine dust to be uniformly mixed into an acidic oxidant, and carrying out primary normal-pressure low-temperature acid leaching, wherein the liquid-solid ratio of the acidic oxidant liquid to the calcine dust is set to be 9: 1;
s5: at one stageIntroducing oxygen for oxidation in the normal-pressure low-temperature acid leaching process, assisting acid leaching, continuously stirring by using stirring equipment, and leaching for 0.75h, wherein the introduced oxygen is pure oxygen, and the aeration flow of the upper layer is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3/h;
S6: heating again, and carrying out second-stage normal-pressure high-temperature acid leaching under the condition of high-temperature high-acid stirring, wherein the temperature of the second-stage normal-pressure high-temperature acid leaching is kept at 87.5 ℃;
s7: introducing oxygen for oxidation in the two-stage normal-pressure high-temperature acid leaching process, performing auxiliary acid leaching, continuously stirring by using stirring equipment, leaching for 2.5h, and completely leaching zinc in the roasted sand dust, wherein the introduced oxygen is pure oxygen, and the aeration flow of the upper layer is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3Controlling the acidity of the leaching end point to be more than 20 g/L;
s8: and (3) purifying, electrolyzing and casting the leachate to recycle zinc, detecting the zinc content of the leached residues, and putting the leached residues with overhigh zinc content into a leaching tank to carry out two-stage normal-pressure high-temperature acid leaching.
EXAMPLE III
Referring to fig. 1, the present invention is a method for atmospheric leaching of zinc sulfide from calcine dust by oxygen oxidation, comprising the following steps:
s1: aeration pipes are laid in the upper, middle and lower layers in the leaching tank, the lower layer aeration pipe is arranged at the bottom of the tank, the upper layer aeration pipe is arranged at a position 20cm away from the liquid level, and the upper, middle and lower layers of aeration pipes are distributed in the leaching tank at equal intervals;
s2: cooling the acidic oxidant liquid to 12 ℃;
s3: putting the cooled acidic oxidant liquid into a leaching tank;
s4: adding the calcine dust collected from the mineral roasting dust settling tower into a leaching tank, continuously stirring by using stirring equipment in the adding process to enable the calcine dust to be uniformly mixed into an acidic oxidant, and carrying out primary normal-pressure low-temperature acid leaching, wherein the liquid-solid ratio of the acidic oxidant liquid to the calcine dust is set to be 10: 1;
s5: introducing oxygen for oxidation in a section of normal-pressure low-temperature acid leaching process, assisting in acid leaching, continuously stirring by using stirring equipment, and leaching for 1h, wherein the introduced oxygen is pure oxygen, and the aeration flow of the upper layer is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3/h;
S6: heating, and carrying out second-stage normal-pressure high-temperature acid leaching under the condition of high-temperature high-acid stirring, wherein the temperature of the second-stage normal-pressure high-temperature acid leaching is kept at 90 ℃;
s7: introducing oxygen for oxidation in the two-stage normal-pressure high-temperature acid leaching process, performing auxiliary acid leaching, continuously stirring by using stirring equipment, leaching for 3h, and completely leaching zinc in the roasted sand dust, wherein the introduced oxygen is pure oxygen, and the aeration flow of the upper layer is set to be 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3Controlling the acidity of the leaching end point to be more than 20 g/L;
s8: and (3) purifying, electrolyzing and casting the leachate to recycle zinc, detecting the zinc content of the leached residues, and putting the leached residues with overhigh zinc content into a leaching tank to carry out two-stage normal-pressure high-temperature acid leaching.
Comparison of calcine dust normal pressure high temperature high acid leaching test:
introducing oxygen into the roasted sand dust through high-temperature peracid leaching and not introducing the oxygen, and comparing zinc content of slag at leaching end points in different leaching time:
Figure 418240DEST_PATH_IMAGE002
as can be seen from the above table: under the original operation condition, the zinc content of the leaching residue of the calcine dust can be greatly reduced by introducing oxygen for oxidation, and the zinc sulfide which is not leached originally is leached out, so that the leaching rate is improved, and the production output value is increased.
The above are only preferred embodiments of the present invention, and the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made to the technical solutions described in the above embodiments, and to some of the technical features thereof, are included in the scope of the present invention.

Claims (8)

1. A method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation is characterized in that: the method comprises the following steps:
s1: laying aeration pipes on the upper, middle and lower layers in the leaching tank;
s2: cooling the acidic oxidant liquid;
s3: putting the cooled acidic oxidant liquid into a leaching tank;
s4: adding the calcine dust collected from the mineral roasting dust settling tower into a leaching tank, continuously stirring by using stirring equipment in the adding process to enable the calcine dust to be uniformly mixed into an acid oxidant, and carrying out primary normal-pressure low-temperature acid leaching;
s5: introducing oxygen for oxidation in a section of normal-pressure low-temperature acid leaching process, assisting in acid leaching, continuously stirring through stirring equipment, and leaching for 0.5-1 h;
s6: then heating, and carrying out two-stage normal-pressure high-temperature acid leaching under the condition of high-temperature high-acid stirring;
s7: introducing oxygen for oxidation in the two-stage normal-pressure high-temperature acid leaching process, assisting in acid leaching, continuously stirring through stirring equipment, leaching for 2-3 hours, and completely leaching zinc in the roasted sand dust;
s8: and purifying, electrolyzing and casting the leaching solution to recycle the zinc.
2. The method as claimed in claim 1, wherein the aeration pipe of the lower layer of S1 is arranged at the bottom of the tank, the aeration pipe of the upper layer is arranged at a distance of 20cm from the liquid level, and the aeration pipes of the upper, middle and lower layers are distributed in the leaching tank at equal intervals.
3. The method for atmospheric pressure leaching of zinc sulfide in calcine dust by using oxygen as claimed in claim 1, wherein the temperature of the acidic oxidant liquid in S2 after temperature reduction treatment is set to 10-12 ℃.
4. The method for atmospheric pressure leaching of zinc sulfide in roasted-sand dust by using oxygen as claimed in claim 1, wherein the liquid-solid ratio of the acidic oxidant liquid to the roasted-sand dust in S4 is set to 8-10: 1.
5. The method for atmospheric pressure leaching of zinc sulfide in calcine dust by oxygen oxidation according to claim 1, wherein the temperature of the secondary atmospheric pressure high temperature acid leaching in S6 is maintained at 85-90 ℃.
6. The method for atmospheric leaching of zinc sulfide from calcine dust by oxygen as claimed in claim 1, wherein the oxygen introduced in S5 and S7 is pure oxygen, and the aeration flow rate of the upper layer is set to 0.05m3H, setting the aeration flow rate of the middle layer to be 0.10m3The aeration flow rate of the lower layer is set to be 0.15m3/h。
7. The method for atmospheric pressure leaching of zinc sulfide from calcine dust by oxygen oxidation as claimed in claim 1, wherein the acidity of the leaching end point is controlled to be more than 20 g/L.
8. The method for atmospheric leaching of zinc sulfide from calcine dust by oxygen oxidation as claimed in claim 1, wherein said S8 is characterized in that the leached residue is subjected to zinc content detection, and the leached residue with excessive zinc content is put into a leaching tank for secondary atmospheric high-temperature acid leaching.
CN202110960394.5A 2021-08-20 2021-08-20 Method for leaching zinc sulfide in calcine dust under normal pressure by using oxygen oxidation Pending CN113667834A (en)

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CN117625956A (en) * 2024-01-25 2024-03-01 昆明理工大学 Efficient zinc extraction method for zinc calcine

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CN110117723A (en) * 2019-05-10 2019-08-13 昆明理工大学 A kind of richness germanium zinc oxide fumes leaching method
CN113005289A (en) * 2019-12-19 2021-06-22 有研资源环境技术研究院(北京)有限公司 Method for improving zinc oxygen pressure leaching rate by using calcine waste heat and oxygen pressure leaching kettle exhaust

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BE1007417A3 (en) * 1993-08-27 1995-06-13 Union Miniere Sa Leaching method for zinc sulphide concentrate and zinc ferrite
CN1477216A (en) * 2002-08-24 2004-02-25 祥云县飞龙实业有限责任公司 Zinc sulfide concentrate calcines and zinc ide ore combined leaching process
CN101845548A (en) * 2009-03-27 2010-09-29 北京建新力拓科技有限公司 Ozone leaching method for zinc sulfide concentrates at normal pressure
WO2012040829A1 (en) * 2010-09-30 2012-04-05 Yava Technologies Inc. Selective leach recovery of zinc from a composite sulphide ore deposit, tailings, crushed ore or mine sludge
US20140212348A1 (en) * 2012-07-16 2014-07-31 Ram5, S.L. Hydrometallurgical method for recovery of zinc in sulphuric medium starting from sulphidic zinc concentrates with high iron content
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CN105331801A (en) * 2015-11-27 2016-02-17 中南大学 Cooperative roasting method for zinc concentrate and iron pyrite
CN106893873A (en) * 2016-12-28 2017-06-27 呼伦贝尔驰宏矿业有限公司 A kind of common association concentrate zinc metallurgy method of zinc sulphide containing indium, silver, arsenic
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CN110117723A (en) * 2019-05-10 2019-08-13 昆明理工大学 A kind of richness germanium zinc oxide fumes leaching method
CN113005289A (en) * 2019-12-19 2021-06-22 有研资源环境技术研究院(北京)有限公司 Method for improving zinc oxygen pressure leaching rate by using calcine waste heat and oxygen pressure leaching kettle exhaust

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117625956A (en) * 2024-01-25 2024-03-01 昆明理工大学 Efficient zinc extraction method for zinc calcine
CN117625956B (en) * 2024-01-25 2024-03-22 昆明理工大学 Efficient zinc extraction method for zinc calcine

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Application publication date: 20211119