CN114369724A - Method for quickly producing antimony white from high-arsenic antimony-lead anode mud - Google Patents
Method for quickly producing antimony white from high-arsenic antimony-lead anode mud Download PDFInfo
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- CN114369724A CN114369724A CN202111635317.9A CN202111635317A CN114369724A CN 114369724 A CN114369724 A CN 114369724A CN 202111635317 A CN202111635317 A CN 202111635317A CN 114369724 A CN114369724 A CN 114369724A
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- antimony
- arsenic
- lead anode
- white
- anode slime
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- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 63
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 32
- QQHJESKHUUVSIC-UHFFFAOYSA-N antimony lead Chemical compound [Sb].[Pb] QQHJESKHUUVSIC-UHFFFAOYSA-N 0.000 title claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 32
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 32
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003723 Smelting Methods 0.000 claims abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 claims abstract description 17
- 239000004332 silver Substances 0.000 claims abstract description 17
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001245 Sb alloy Inorganic materials 0.000 claims abstract description 14
- 239000002140 antimony alloy Substances 0.000 claims abstract description 14
- 229910052737 gold Inorganic materials 0.000 claims abstract description 14
- 239000010931 gold Substances 0.000 claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 14
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000000571 coke Substances 0.000 claims abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 9
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 239000004071 soot Substances 0.000 claims abstract description 4
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 229910000978 Pb alloy Inorganic materials 0.000 claims description 5
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910000510 noble metal Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 16
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009853 pyrometallurgy Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 10
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001152 Bi alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000009874 alkali refining Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
Images
Classifications
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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
- C22B7/001—Dry processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic 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 invention relates to the technical field of pyrometallurgical process, in particular to a method for quickly producing antimony white from high-arsenic antimony lead anode slime, which comprises the following steps: s1 lead anode slime, coke and soda ash are mixed according to a certain proportion and are subjected to reduction smelting at the temperature of 1150-; s2 adding caustic soda flakes into the low-arsenic crude antimony alloy at the temperature of 580-650 ℃ by using a refining pot to reduce the arsenic content in the low-arsenic crude antimony to be below 0.015 percent, thereby realizing the removal of arsenic impurity elements in the low-arsenic crude antimony alloy; and S3, after removing arsenic, the crude antimony alloy is transferred to an oxidation pot to be blown to produce antimony white, so that the antimony element is rapidly extracted from the high-arsenic antimony-lead anode mud to produce an antimony white product. The invention has the beneficial effects that: the method has the advantages of realizing the rapid production of antimony white, reducing the dispersion of gold and silver in the treatment process, improving the direct yield of antimony and gold and silver, avoiding the secondary treatment of slag and soot, and reducing the environmental protection pressure and the production cost.
Description
Technical Field
The invention relates to the technical field of pyrometallurgical process, in particular to a method for quickly producing antimony white from high-arsenic antimony lead anode slime.
Background
The anode mud is conventionally treated by converter reduction smelting, arsenic and antimony leakage and oxidation refining to produce a qualified silver anode plate, and the qualified silver anode plate is subjected to silver electrolysis to produce national standard No. 1 silver powder, and the qualified silver anode plate is subjected to black gold powder conversion refining to produce national standard No. 1 gold ingots after electrolysis. The process mainly recovers gold and silver, bismuth is enriched and recovered in a bismuth slag form, further burdening reduction smelting is carried out to produce crude bismuth alloy, then copper removal, arsenic and antimony removal, lead removal by chlorination, alkali refining and purification are carried out to produce bismuth ingot products, antimony is recovered in an open circuit mode in the form of antimony slag and arsenic and antimony ash, further burdening reduction smelting is carried out to produce crude antimony alloy, and antimony white products are produced through alkali dearsenization and oxidation converting.
In the traditional antimony white production, antimony slag and antimony-containing soot generated in the lead anode mud treatment process are mainly used as raw materials, for example, patent No. CN1800423B, the patent name "process for producing antimony white by using slag for treating lead anode mud", and antimony slag generated in the lead anode mud reduction smelting process is used as a raw material for reduction smelting to produce crude alloy, which is a secondary recovery of antimony in the lead anode mud smelting process, and has the problems of metal dispersion and low recovery rate, so that a method for efficiently and rapidly producing antimony white in high-arsenic antimony lead anode mud is provided, which is very important.
Disclosure of Invention
The invention aims to provide a method for quickly producing antimony white from high-arsenic antimony-lead anode slime, which shortens the treatment process, reduces the generation amount of dust in the smelting process, reduces the generation amount of slag, and reduces the dispersion of noble metals and the secondary smelting of antimony slag caused by antimony slag produced by the traditional process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for rapidly producing antimony white from high-arsenic antimony-lead anode slime comprises the following steps:
s1 lead anode slime, coke and soda ash are mixed according to a certain proportion and are subjected to reduction smelting at the temperature of 1150-;
s2 adding caustic soda flakes into the low-arsenic crude antimony alloy at the temperature of 580-650 ℃ by using a refining pot to reduce the arsenic content in the low-arsenic crude antimony to be below 0.015 percent, thereby realizing the removal of arsenic impurity elements in the low-arsenic crude antimony alloy;
and S3, after removing arsenic, the crude antimony alloy is transferred to an oxidation pot to be blown to produce antimony white, so that the antimony element is rapidly extracted from the high-arsenic antimony-lead anode mud to produce an antimony white product.
According to the further scheme, the lead anode slime directly enters a converter for deep reduction smelting, the temperature is reduced to 850-1000 ℃ in the later stage of the lead anode slime reduction smelting, the converter efficient removal of arsenic is realized, the refining period is shortened for the subsequent deep removal of arsenic, and the dispersion of precious metals and the secondary smelting of antimony slag caused by the fact that antimony slag is produced in the traditional process and a large amount of antimony elements enter soot are avoided.
In a further scheme, the low-arsenic crude antimony alloy produced in the step S1 contains 1% -3% of arsenic.
In a further scheme, in the step S1, the ratio of the lead anode slime to coke and soda ash is 100: (3-5): (2-5) ore blending.
In a further scheme, in the step S1, the lead anode slime, coke and soda ash are mixed according to the ratio of 100:4: 3.
In a further scheme, the antimony white product in the step S3 conforms to Sb in the nonferrous metal industry standard YS/T1117-20162O398-1 designation, i.e. Sb2O3The content is not less than 99.50%.
In a further scheme, the residual bottom lead after the antimony white is produced in the step S3 enters a vacuum furnace, gold and silver are further recovered, and the high-bismuth lead alloy is produced.
Compared with the prior art, the invention has the beneficial effects that:
1. in the process of treating the high-arsenic antimony-lead anode slime, the rapid production of antimony white is realized, the use of auxiliary materials is reduced, the dispersion of gold and silver in the treatment process of the lead anode slime is reduced, the direct recovery rate of the gold and silver is improved, the secondary treatment of slag and ash is avoided, the environmental protection pressure and the production cost of the subsequent production are reduced, and meanwhile, the direct recovery rate of antimony can be obviously improved.
2. The method has the remarkable advantages of low production cost, simple operation, excellent environment and high recovery rate of gold, silver, bismuth, antimony and lead elements in lead anode slime treatment. The recovery rate of gold and silver reaches more than 99.0 percent, the recovery rate of antimony reaches more than 95 percent, and the recovery rate of lead and bismuth reaches more than 90 percent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments of the present invention will be briefly described below. It is obvious that the drawings described below are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a process flow diagram of an embodiment of the invention.
Detailed Description
For a better understanding of the present invention, the following detailed description is given in conjunction with the accompanying drawings and examples, which are not intended to limit the present invention to the following examples.
Example 1: the content of each element of the lead anode mud is shown as table one:
table-lead anode mud contains the elements in percentage
Remarking: band element unit is g/t.
The method comprises the following steps: carrying out reduction smelting on lead anode mud, coke and sodium carbonate according to a ratio of 100:4:3 in an ore blending manner at the temperature of 1150-1170 ℃, then cooling to 930 ℃, adding caustic soda flakes (sodium hydroxide) to efficiently remove arsenic until low-arsenic crude antimony containing 2% of arsenic is produced; adding caustic soda flakes (sodium hydroxide) into the low-arsenic crude antimony at the temperature of 600-630 ℃ by using a refining pot to deeply remove arsenic from the low-arsenic crude antimony until the arsenic content is below 0.015 percent; the crude antimony alloy after arsenic removal is transferred to an oxidation pot for converting antimony white to produce Sb2O3The content is 99.80%; and (4) treating the residual bottom lead after antimony white production in a vacuum furnace, and further recovering gold and silver and producing the high-bismuth lead alloy.
Table two under this experimental condition, the recovery rates of gold, silver and antimony in the lead anode slime were as follows:
example 2: the contents of the elements of the lead anode mud are as shown in the table III:
content of each element in the anode mud of the lead-acid battery
Remarking: band element unit is g/t.
The method comprises the following steps: lead anode slime is mixed with coke and sodium carbonate according to the ratio of 100:4:3 and is reduced and smelted at the temperature of 1160-1190 ℃,then cooling to 950 ℃, adding caustic soda flakes (sodium hydroxide) to remove arsenic efficiently, and producing low-arsenic crude antimony containing 2.5% of arsenic; adding caustic soda flakes (sodium hydroxide) into the low-arsenic crude antimony at the temperature of 590-620 ℃ by using a refining pot to deeply remove arsenic from the low-arsenic crude antimony until the arsenic content is below 0.015 percent; the crude antimony alloy after arsenic removal is transferred to an oxidation pot for converting antimony white to produce Sb2O3The content is 99.80%; and (4) treating the residual bottom lead after antimony white production in a vacuum furnace, and further recovering gold and silver and producing the high-bismuth lead alloy.
Table four under this experimental condition, the recovery rates of gold, silver and antimony in the lead anode slime were as follows:
it should be understood that the above-described embodiments are merely preferred embodiments of the invention and the technical principles applied thereto. It will be understood by those skilled in the art that various modifications, equivalents, changes, and the like can be made to the present invention. However, such variations are within the scope of the invention as long as they do not depart from the spirit of the invention. In addition, certain terms used in the specification and claims of the present application are not limiting, but are used merely for convenience of description.
Claims (7)
1. A method for rapidly producing antimony white from high-arsenic antimony-lead anode slime is characterized by comprising the following steps:
s1 lead anode slime, coke and soda ash are mixed according to a certain proportion and are subjected to reduction smelting at the temperature of 1150-;
s2 adding caustic soda flakes into the low-arsenic crude antimony alloy at the temperature of 580-650 ℃ by using a refining pot to reduce the arsenic content in the low-arsenic crude antimony to be below 0.015 percent, thereby realizing the removal of arsenic impurity elements in the low-arsenic crude antimony alloy;
and S3, after removing arsenic, the crude antimony alloy is transferred to an oxidation pot to be blown to produce antimony white, so that the antimony element is rapidly extracted from the high-arsenic antimony-lead anode mud to produce an antimony white product.
2. The method for rapidly producing antimony white from high-arsenic antimony-lead anode slime according to claim 1, characterized in that: and S1, directly feeding the lead anode slime into a converter for deep reduction smelting, and cooling to 850-1000 ℃ in the later stage of the lead anode slime reduction smelting to realize converter-based efficient removal of arsenic, shorten the refining period for subsequent deep arsenic removal, and avoid the dispersion of noble metals and the secondary smelting of antimony slag caused by antimony slag produced by the traditional process and a large amount of antimony elements entering soot.
3. The method for rapidly producing antimony white from high-arsenic antimony-lead anode slime according to claim 1, characterized in that: the low-arsenic crude antimony alloy produced in the step S1 contains 1% -3% of arsenic.
4. The method for rapidly producing antimony white from high-arsenic antimony-lead anode slime according to claim 1, characterized in that: in the step S1, the ratio of the lead anode slime to coke and soda ash is 100: (3-5): (2-5) ore blending.
5. The method for rapidly producing antimony white from high-arsenic antimony-lead anode slime according to claim 4, characterized in that: and in the step S1, blending the lead anode slime with coke and soda ash according to the ratio of 100:4: 3.
6. The method for rapidly producing antimony white from high-arsenic antimony-lead anode slime according to claim 1, characterized in that: the antimony white product in the step S3 conforms to Sb in the nonferrous metal industry standard YS/T1117-20162O398-1 designation, i.e. Sb2O3The content is not less than 99.50%.
7. The method for rapidly producing antimony white from high-arsenic antimony-lead anode slime according to claim 1, characterized in that: and (S3) feeding the residual bottom lead alloy after antimony white production in the step into a vacuum furnace, and further recovering gold and silver and producing the high-bismuth lead alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111635317.9A CN114369724A (en) | 2021-12-29 | 2021-12-29 | Method for quickly producing antimony white from high-arsenic antimony-lead anode mud |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111635317.9A CN114369724A (en) | 2021-12-29 | 2021-12-29 | Method for quickly producing antimony white from high-arsenic antimony-lead anode mud |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115058599A (en) * | 2022-07-12 | 2022-09-16 | 山东恒邦冶炼股份有限公司 | Method for removing arsenic and recovering tin and antimony from tin-lead-containing anode slime through oxidation refining |
| CN115305356A (en) * | 2022-08-30 | 2022-11-08 | 河南豫光金铅股份有限公司 | Method for recovering valuable metals from lead anode slime antimony smelting smoke dust |
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| CN107858531A (en) * | 2017-12-01 | 2018-03-30 | 云南驰宏资源综合利用有限公司 | A kind of high-arsenic antimony thick bismuth improves the method and device of bismuth direct yield when refining |
| CN109628761A (en) * | 2018-12-29 | 2019-04-16 | 焱鑫环保科技有限公司 | A method of stibium trioxide is produced using high antimony secondary smoke dearsenification |
| CN110512077A (en) * | 2019-05-16 | 2019-11-29 | 山东恒邦冶炼股份有限公司 | A kind of method of lead anode slurry high efficiente callback gold and silver bismuth antimony tellurium |
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2021
- 2021-12-29 CN CN202111635317.9A patent/CN114369724A/en active Pending
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| CN109628761A (en) * | 2018-12-29 | 2019-04-16 | 焱鑫环保科技有限公司 | A method of stibium trioxide is produced using high antimony secondary smoke dearsenification |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115058599A (en) * | 2022-07-12 | 2022-09-16 | 山东恒邦冶炼股份有限公司 | Method for removing arsenic and recovering tin and antimony from tin-lead-containing anode slime through oxidation refining |
| CN115305356A (en) * | 2022-08-30 | 2022-11-08 | 河南豫光金铅股份有限公司 | Method for recovering valuable metals from lead anode slime antimony smelting smoke dust |
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