CN109777962A - A kind of method of lead anode slurry removing arsenic - Google Patents
A kind of method of lead anode slurry removing arsenic Download PDFInfo
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- CN109777962A CN109777962A CN201910154270.0A CN201910154270A CN109777962A CN 109777962 A CN109777962 A CN 109777962A CN 201910154270 A CN201910154270 A CN 201910154270A CN 109777962 A CN109777962 A CN 109777962A
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- arsenic
- anode slurry
- lead anode
- lead
- elemental
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- 239000006256 anode slurry Substances 0.000 title claims abstract description 48
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 47
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- LULLIKNODDLMDQ-UHFFFAOYSA-N arsenic(3+) Chemical compound [As+3] LULLIKNODDLMDQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229960002594 arsenic trioxide Drugs 0.000 claims abstract 5
- 229910000413 arsenic oxide Inorganic materials 0.000 claims abstract 4
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- IKWTVSLWAPBBKU-UHFFFAOYSA-N a1010_sial Chemical compound O=[As]O[As]=O IKWTVSLWAPBBKU-UHFFFAOYSA-N 0.000 claims 3
- 239000011133 lead Substances 0.000 abstract description 53
- 229910052709 silver Inorganic materials 0.000 abstract description 13
- 229910052802 copper Inorganic materials 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 10
- 150000002739 metals Chemical class 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052745 lead Inorganic materials 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 2
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 abstract 2
- 231100000053 low toxicity Toxicity 0.000 abstract 1
- 229910052787 antimony Inorganic materials 0.000 description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 10
- 239000010949 copper Substances 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- 229910052737 gold Inorganic materials 0.000 description 8
- 239000010931 gold Substances 0.000 description 8
- 229910000510 noble metal Inorganic materials 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 7
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000001698 pyrogenic effect Effects 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000003500 flue dust Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- DLISVFCFLGSHAB-UHFFFAOYSA-N antimony arsenic Chemical compound [As].[Sb] DLISVFCFLGSHAB-UHFFFAOYSA-N 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- COHDHYZHOPQOFD-UHFFFAOYSA-N arsenic pentoxide Chemical compound O=[As](=O)O[As](=O)=O COHDHYZHOPQOFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229910001254 electrum Inorganic materials 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- XXOYNJXVWVNOOJ-UHFFFAOYSA-N fenuron Chemical compound CN(C)C(=O)NC1=CC=CC=C1 XXOYNJXVWVNOOJ-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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 discloses a kind of method that arsenic is removed from lead anode slurry, belongs to field of thermometallurgical technology.First by lead anode slurry drying and dewatering, calcination process lead anode slurry, makes arsenic oxide and elemental arsenic in lead anode slurry volatilize at high temperature, achievees the purpose that dearsenification under vacuum conditions;The hypertoxic arsenic oxide of volatilization can also be reduced into the elemental arsenic of low toxicity by adding carbon-coating on lead anode slurry raw material top.This method process is simple, dearsenification significant effect, only the arsenic in lead anode slurry can be removed 90% or more by a step vacuum volatilization, direct yield > 95% of direct yield > 99%, Pb of other valuable metals Ag, Cu;This method cost of investment is low, high financial profit, there is extraordinary industrial prospect.
Description
Technical field
A kind of method that the present invention discloses lead anode slurry removing arsenic, belongs to pyrometallurgy field.
Background technique
Lead anode slurry be mainly derived from lead bullion electrorefining be attached to anode substrate surface or be deposited in cell bottom or
The purees being suspended in electrolyte.Since the composition of lead anode slurry is more complex, wherein usually contain containing a large amount of antimony, lead,
Bismuth, arsenic, silver and the multiple elements such as gold, copper, and the presence in the form of a variety of object phases on a small quantity.Arsenide has severe toxicity, contains in lead anode slurry
Arsenic amount is up to 40%, therefore a large amount of lead anode slurries cannot recycle.The content of noble metal is generally than exploitation in lead anode slurry
Precious metal ore it is much higher, be the important source material for extracting noble metal Au, Ag and other valuable metals Pb, Sb, Se, Te etc..
Lead anode slurry is in addition to containing arsenic, also rich in valuable metals such as gold, silver, copper, lead, antimony, if lead anode slurry directly returned
Smeltery's melting is returned, arsenic can constantly be enriched with, both influence the purity of main metal, can also cause damages to operating environment.Currently, lead is positive
Pole mud main process includes pyrogenic attack technique, wet processing process, wet process-pyrogenic process process integration.Pyrogenic attack technique
Main flow includes reduction melting, refinement oxide, electrolytic separation extraction noble metal, and pyrogenic attack technique is strong to adaptability to raw material,
It is easy to operate, but there are arsenic, the bad recycling of antimony, pollute environment, the disadvantages such as the production cycle is long, and gold, silver direct yield is low.Wet-treating
Technique usually leaches the metals such as As, Cu, Bi, Sb in lead anode slurry in aqueous solution, then separates lead simultaneously in leached mud
The noble metals such as gold, silver are recycled, with short production cycle, noble metal and the associated metal rate of recovery are high, but can generate simultaneously largely useless containing arsenic
Water, complex procedures.Wet process-pyrogenic process process integration uses wet processing to remove the alkali metal such as As, Cu, Bi in the earth of positive pole first, obtains
To the leached mud rich in noble metals such as gold, silver;Leached mud generates electrum plate, further electrolytic recovery using pyrogenic attack
The noble metals such as gold, silver.The advantages of wet process-pyrogenic process process integration has been provided simultaneously with wet processing and thermal process, exists simultaneously examination
The disadvantages of agent consumption is big, cost of investment and equipment maintenance cost are high.Patent of invention (CN105296764A) propose it is a kind of from
The method of pre- removing arsenic and antimony simultaneously in lead anode slurry, this method roast lead anode slurry at 400 ~ 600 DEG C, in roasting process
Air constantly is blasted, is oxidized arsenic and antimony in lead anode slurry, is volatilized in the form of arsenic trioxide and antimony oxide de-
It removes.This method process is simple, and about 90% arsenic antimony concentrates in flue dust in lead anode slurry, is conducive to the post-processing of lead anode slurry,
But there are the excessive oxidation phenomenon of arsenic, it is easy to generate the diarsenic pentoxide of difficult volatilization, influences dearsenification effect.Patent of invention
(CN1403603A) a kind of Dearsenifying process for anode mud with high As and Pb content is proposed, this method is steamed with water at a certain temperature using elemental arsenic
Solid/liquid/gas reactions generate volatile As2O3, by being passed through vapor into rotary kiln, in 400 ~ 750 DEG C of roasting temperatures, lead anode
Most of arsenic in mud is entered in flue dust in the form of arsenic trioxide, and valuable metal Pb, Sb are stayed in calcining.This method dearsenification effect
Fruit is good, can reach 90% or so, and production cost is low, but can generate a large amount of arsenic-containing waste water.
Summary of the invention
It is an object of the present invention to provide a kind of methods of lead anode slurry removing arsenic, specifically includes the following steps: by lead anode slurry
Raw material stoving is placed in tube type resistance furnace, is vacuumized, and when pressure in furnace in 1 ~ 10000Pa, controls resistance furnace with 15 ~ 25
DEG C/heating rate of min heating lead anode slurry to 500 ~ 800 DEG C, keep the temperature 2 ~ 5h, control 100 ~ 450 DEG C of condensation zones, lead sun
Arsenic in the mud of pole is volatilized in the form of arsenic trioxide and elemental arsenic, is collected in condensation end, and condensate object is mutually mainly arsenic oxidation
Object.
Preferably, contain arsenic >=30% in step (1) of the present invention in lead anode slurry, arsenic is mainly aoxidized in lead anode slurry with arsenic
Object, elemental arsenic form exist.
Preferably, drying condition in step (1) of the present invention are as follows: at 100~150 DEG C dry 5 ~ for 24 hours.
Further, one layer of carbonaceous reducing agent is placed at 5 ~ 10cm of top of lead anode slurry raw material, carbon-coating temperature is 600
~ 1000 DEG C, volatile matter is reduced across carbon-coating, is collected in condensation end, and condensate object is mutually mainly arsenic.
Beneficial effects of the present invention:
The present invention realizes Volatile Elements As and other yuan using the saturated vapour pressure difference of each metallic compound in lead anode slurry
The separation of element achievees the effect that remove the valuable metals such as arsenic and high efficiente callback Ag, Pb, Cu;Dearsenification effect is good, process is simple,
Operation under vacuum tightness environment avoids harm of the toxic volatile matter to ambient enviroment;Lead anode slurry after processing rich in copper,
The noble metals such as the valuable metals such as lead, antimony and gold, silver, conducive to the synthetical recovery of later period metal.
Detailed description of the invention
Fig. 1 is the process flow chart for the method that lead anode slurry of the present invention removes arsenic.
Fig. 2 is that the XRD of 1 condensate of the embodiment of the present invention is composed.
Fig. 3 is that the XRD of 3 condensate of the embodiment of the present invention is composed.
Specific embodiment
With reference to the accompanying drawing and the specific embodiment present invention is described in further detail, but protection scope of the present invention is simultaneously
It is not limited to the content.
Lead anode slurry ingredient in the embodiment of the present invention: arsenic 40.31%, antimony 22.94%, lead 11.72%, silver-colored 7.13%, copper
2.55%, carbon 1.25%, silicon 0.25%, tin 0.27%, sulphur 0.78%.
Embodiment 1
200g lead anode slurry is taken to be put into electric drying oven with forced convection, dry 5h, weightlessness 25.05% at 105 DEG C;After taking 30g dry
Lead anode slurry grinding uniformly, be put into crucible, be fitted into tube type resistance furnace;It vacuumizes, when furnace internal pressure strong stability in 5Pa, control
Resistance furnace processed is heated to 600 DEG C with the heating rate of 17 DEG C/min, keeps the temperature 3h, in insulating process in reactor pressure 1 ~
It is fluctuated within the scope of 500Pa;Reaction terminates to collect residue and condensate in crucible, obtains residue containing arsenic 3.83%, arsenic-removing rate is
98.04%, condensate is arsenic trioxide (as shown in Figure 2), and silver, copper direct yield > 99%, the direct yield of antimony is 55.66%, vertical
Yield is 98.22%.
Embodiment 2
500g lead anode slurry is taken to be put into electric drying oven with forced convection, dry 20h, weightlessness 28.18% at 120 DEG C;Take 30g dry
Lead anode slurry grinding afterwards uniformly, is put into crucible, is fitted into tube type resistance furnace;It vacuumizes, to furnace internal pressure strong stability in 10000Pa
When, control resistance furnace with 22 DEG C/min and be warming up to 800 DEG C, keep the temperature 2h, in insulating process in reactor pressure in 1 ~ 500Pa range
Interior fluctuation;Residue and condensate are collected after reaction, obtain residue containing arsenic 8.16%, arsenic-removing rate 91.81%, condensate
Main object is mutually arsenic trioxide, and direct yield > 99% of copper, silver, the direct yield of antimony is 62.75%, the direct yield of lead is 91.21%.
Embodiment 3
500g lead anode slurry is put into electric drying oven with forced convection, dry 10h, weightlessness 27.43% at 150 DEG C;Take 30g dry
Lead anode slurry grinding afterwards uniformly, is put into crucible, the wooden carbon-coating is placed at the 8cm of crucible top, is fitted into tube type resistance furnace;It takes out true
Sky controls resistance furnace with 18 DEG C/min and is warming up to 700 DEG C when furnace internal pressure strong stability in 100Pa, keeps the temperature 4h, in insulating process
Pressure fluctuates within the scope of 1 ~ 500Pa in reactor;Residue and condensate are collected after reaction, obtain residue containing arsenic
8.52%, arsenic-removing rate 92.80%, condensate is mainly elemental arsenic (as shown in Figure 3), direct yield > 99% of copper, silver, the straight receipts of antimony
Rate is 57.86%, the direct yield of lead is 93.35%.
Claims (4)
1. a kind of method of lead anode slurry removing arsenic, which is characterized in that specifically includes the following steps: by lead anode slurry raw material stoving
It is placed in tube type resistance furnace, vacuumizes, when pressure in furnace in 1 ~ 10000Pa, control resistance furnace with the liter of 15 ~ 25 DEG C/min
Warm rate heating lead anode slurry keeps the temperature 2 ~ 5h, controls 100 ~ 450 DEG C of condensation zones, the arsenic in lead anode slurry to 500 ~ 800 DEG C
It is volatilized in the form of arsenic trioxide and elemental arsenic, is collected in condensation end, condensate object is mutually mainly arsenic oxide.
2. the method for lead anode slurry removing arsenic according to claim 1, it is characterised in that: contain in lead anode slurry in step (1)
Arsenic >=30%, arsenic mainly exist in the form of arsenic oxide, elemental arsenic in lead anode slurry.
3. the method for lead anode slurry removing arsenic according to claim 1, it is characterised in that: drying condition in step (1) are as follows:
At 100~150 DEG C drying 5 ~ for 24 hours.
4. according to claim 1 lead anode slurry removing arsenic method, it is characterised in that: the top of lead anode slurry raw material 5 ~
One layer of carbonaceous reducing agent is placed at 10cm, carbon-coating temperature is 600 ~ 1000 DEG C, and volatile matter is reduced across carbon-coating, is received in condensation end
Collection, condensate object are mutually mainly arsenic.
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CN201910154270.0A CN109777962B (en) | 2019-03-01 | 2019-03-01 | Method for removing arsenic from lead anode mud |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112359209A (en) * | 2020-11-09 | 2021-02-12 | 昆明理工大学 | Method for enriching and recovering noble metal in lead anode slime |
CN113528846A (en) * | 2021-06-18 | 2021-10-22 | 广西壮族自治区环境保护科学研究院 | Treatment method for resource utilization of arsenic-containing waste residues |
CN113846222A (en) * | 2021-10-13 | 2021-12-28 | 昆明理工大学 | Method for recovering valuable metals in copper anode slime |
CN115011804A (en) * | 2021-12-23 | 2022-09-06 | 昆明理工大学 | Method for removing arsenic by co-roasting high-arsenic antimony-lead anode mud air and water vapor |
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CN1079510A (en) * | 1992-06-02 | 1993-12-15 | 中国有色金属工业总公司昆明贵金属研究所 | Treatment method of high arsonium lead anode mud wet process |
US20100116090A1 (en) * | 2007-04-19 | 2010-05-13 | Nippon Sheet Glass Company, Limited | Method for recovering metal |
CN101942567A (en) * | 2010-10-22 | 2011-01-12 | 中南大学 | Method for removing arsenic and antimonic from anode sludge containing polyvalence composite type arsenic-antimonic compound |
CN107779608A (en) * | 2017-11-21 | 2018-03-09 | 红河砷业有限责任公司 | A kind of equipment and production method that arsenic is directly produced using high-arsenic dust |
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2019
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Patent Citations (4)
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CN1079510A (en) * | 1992-06-02 | 1993-12-15 | 中国有色金属工业总公司昆明贵金属研究所 | Treatment method of high arsonium lead anode mud wet process |
US20100116090A1 (en) * | 2007-04-19 | 2010-05-13 | Nippon Sheet Glass Company, Limited | Method for recovering metal |
CN101942567A (en) * | 2010-10-22 | 2011-01-12 | 中南大学 | Method for removing arsenic and antimonic from anode sludge containing polyvalence composite type arsenic-antimonic compound |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112359209A (en) * | 2020-11-09 | 2021-02-12 | 昆明理工大学 | Method for enriching and recovering noble metal in lead anode slime |
CN113528846A (en) * | 2021-06-18 | 2021-10-22 | 广西壮族自治区环境保护科学研究院 | Treatment method for resource utilization of arsenic-containing waste residues |
CN113846222A (en) * | 2021-10-13 | 2021-12-28 | 昆明理工大学 | Method for recovering valuable metals in copper anode slime |
WO2023061389A1 (en) * | 2021-10-13 | 2023-04-20 | 昆明理工大学 | Recovery method for valuable metal in copper anode mud |
CN115011804A (en) * | 2021-12-23 | 2022-09-06 | 昆明理工大学 | Method for removing arsenic by co-roasting high-arsenic antimony-lead anode mud air and water vapor |
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