CN1059938A - Wet process for preparing silver nitrate from anode mud of electrolytic lead - Google Patents
Wet process for preparing silver nitrate from anode mud of electrolytic lead Download PDFInfo
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- CN1059938A CN1059938A CN90107798A CN90107798A CN1059938A CN 1059938 A CN1059938 A CN 1059938A CN 90107798 A CN90107798 A CN 90107798A CN 90107798 A CN90107798 A CN 90107798A CN 1059938 A CN1059938 A CN 1059938A
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- Prior art keywords
- silver
- add
- nitric acid
- acid
- lead
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001961 silver nitrate Inorganic materials 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title description 3
- 229910052709 silver Inorganic materials 0.000 claims abstract description 33
- 239000004332 silver Substances 0.000 claims abstract description 32
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 20
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 16
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims abstract description 12
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 5
- 238000002386 leaching Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 239000010802 sludge Substances 0.000 claims description 17
- 230000000536 complexating effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000011133 lead Substances 0.000 abstract description 30
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052787 antimony Inorganic materials 0.000 abstract description 5
- 239000002893 slag Substances 0.000 abstract description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 229910000365 copper sulfate Inorganic materials 0.000 abstract description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 abstract description 3
- -1 silver ions Chemical class 0.000 abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 229910052785 arsenic Inorganic materials 0.000 abstract 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract 1
- ONVGIJBNBDUBCM-UHFFFAOYSA-N silver;silver Chemical compound [Ag].[Ag+] ONVGIJBNBDUBCM-UHFFFAOYSA-N 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 10
- 238000004176 ammonification Methods 0.000 description 5
- 238000006073 displacement reaction Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 239000003337 fertilizer Substances 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 241001417490 Sillaginidae Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- VXFYKYABEJYWMR-UHFFFAOYSA-N [Sb].[As].[Cu] Chemical compound [Sb].[As].[Cu] VXFYKYABEJYWMR-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 150000004699 copper complex Chemical class 0.000 description 1
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 description 1
- 229910052955 covellite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- DTPQZKZONQKKSU-UHFFFAOYSA-N silver azanide silver Chemical compound [NH2-].[Ag].[Ag].[Ag+] DTPQZKZONQKKSU-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- 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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- Manufacture And Refinement Of Metals (AREA)
Abstract
The silver nitrate is directly prepared by wet separation from the anode mud of the electrolytic lead. The method takes dilute nitric acid as a solvent to carry out acid leaching on electrolytic lead anode mud containing compounds such as silver, lead, copper, antimony, arsenic and the like; adding industrial ammonia water into acid-soluble clear liquid to complex copper and silver ions; adding nitric acid into the complex solution, and then adding hydrochloric acid to precipitate silver chloride; adding water, zinc sheets and sulfuric acid into silver chloride to replace silver; silver was dissolved with the reagent nitric acid and hydrolyzed. Can directly prepare silver nitrate. The recovery rate of the silver reaches 89-94%. The waste liquid produced can be used for preparing copper sulfate and ammonium nitrate, and the slag can be used as lead ore for treating and recovering lead.
Description
The present invention is that the silver-bearing copper lead etc. of the electrolytic lead anode sludge of compound such as a kind of argentiferous lead copper-stibium-arsenic separates the method that reclaims, and particularly separates the method for producing Silver Nitrate.
The treatment process one of the present existing electrolytic lead anode sludge is the smelting method, directly smelts with pyrogenic process and reclaims silver and other metal, and the rate of recovery of silver has only about 84%.The 2nd, the leaching substitution method is got silver with acidleach and with zinc or other material the silver ions in the solution is replaced into silver again.The finished product of two kinds of method gained are argents, need further deep processing just can obtain series product such as Silver Nitrate.Through the Searches of Patent Literature, still useless wet method is separated the method for producing Silver Nitrate in the prior art from the electrolytic lead anode sludge.
Purpose of the present invention is to seek the contained silver-bearing copper lead of the electrolytic lead anode sludge etc. and separates the effective ways that reclaim, and provides a kind of and directly produces the method for Silver Nitrate by the electrolytic lead anode sludge, to reclaim national precious resource, realizes comprehensive utilization.
Content of the present invention and implementation method comprise molten silver, ammonification complexing, the heavy silver of acidifying, zinc displacement silver chloride, five steps of sour molten hydrolysis of soaking of acid, and existing division is as follows:
1, the molten silver that soaks of acid: be that 30~40% nitric acid (mainly contains Pb with the electrolytic lead anode sludge with concentration under 50~70 ℃ of temperature
2O
3, CuS, Ag, Sb, pbS, Sb
2O
3, Cu
3AS) reaction, solid-to-liquid ratio is 1: 2.5~3.5, reacts 4~6 hours.Principal reaction is:
Silver-bearing copper and most of lead etc. exist in solution with ionic species, and most of antimony and insolubles (S etc.) are present in the slag and are separated.
2, ammonification complexing: in the molten clear liquid of above-mentioned acid in room temperature under continuous condition of stirring, be controlled at slowly added in 3~4 hours ammoniacal liquor to PH be till 10~11.Principal reaction is:
Form (Ag(NH
3)
2)
+And (Cu(NH
3)
4)
++Complex ion, and solubility lead salt and ammonium hydroxide reaction generate precipitation:
Silver-bearing copper enters solution with the complex ion form, and plumbous antimony etc. become precipitation with oxyhydroxide or other material.Like this, just can be with copper silver and other separating substances.
3, the heavy silver of acidifying: add industrial nitric acid in the silver-bearing copper complex solution, control adds the acid amount for being till 1~2 to solution PH, added excessive in a subtle way hydrochloric acid again and constantly stir heavy silver chloride in 2~3 hours.Principal reaction is
Separate silver nitride precipitation.
Add ammoniacal liquor in remaining mother liquor, add-on to solution PH is about 6, and the mantoquita that settles out etc. is processed as copper sulfate.Mother liquor through concentrate chemical fertilizer ammonium nitrate.
4, zinc displacement silver chloride: 2.5~3 times of water with silver chloride weight add in the silver chlorides, add excessive zinc metal sheet, and add sulfuric acid in batches, and adding sulfuric acid amount, to control the PH of solution all the time be 3~4, and stirring.Principal reaction is
Replace and to remove unnecessary zinc.
5, sour molten hydrolysis: add concentration and be 30~35% reagent nitric acid and dissolve silver, temperature is 40~50 ℃, solid-to-liquid ratio is 1: 2, reacted 3 hours, and continue 70~80 ℃ of insulation reaction half an hour, adding water afterwards in solution is 3.5~4.5 to PH, and a spot of impurity forms precipitation and is removed after filtration, and silver nitrate solution is purified.Through condensing crystal, separate oven dry and can get analytical pure, chemical pure or technical grade Silver Nitrate again.Mother liquor after the separation can be recycled.
The precipitation of above-mentioned 1,2 liang of step gained mainly contains a certain amount of antimony and 40% above lead, can be used as lead ore and handles.
The technological process synoptic diagram of invention sees accompanying drawing for details.
The present invention compared with prior art, major advantage is the rate of recovery height of argent, total recovery reaches 89~94%, can reclaim silver effectively, improves the use value of the electrolytic lead anode sludge; Need not be silver,, and directly produce Silver Nitrate by the electrolytic lead anode sludge again by the process of silvery silver products through electrolytic lead anode sludge refining; Slag can be made lead ore and handle, and reclaims plumbous; Byproduct is copper sulfate and chemical fertilizer ammonium nitrate, and does not have the three wastes, and pollution-free, raw material has obtained comprehensive utilization.
Example one
The main chemical of the electrolytic lead anode sludge (%) pb14.8, Cu8.98, Ag6.17, Bi0.23, Sb.
Main processes: molten silver, ammonification complexing, the heavy silver of acidifying, the zinc displacement silver chloride of soaking of acid.
1, the molten reaction conditions that soaks silver of acid: concentration of nitric acid 41%, anode sludge granularity 70 orders, sour consumption solid-to-liquid ratio=1: 2.7,3.5 hours reaction times, about 52 ℃ of temperature of reaction.
2, the reaction conditions of ammonification complexing: processing industry ammoniacal liquor is to PH=10.5, temperature of reaction normal temperature
3, the reaction conditions of the heavy silver of acidifying: processing industry nitric acid adds little excessive hydrochloric acid, normal-temperature reaction to PH=2 about 2 hours
4, the reaction conditions of zinc displacement silver chloride: amount of water press silver chloride water=1: 2.5, the zinc overdose of adding, and control adds sulfuric acid, and to make PH be 3~4, stirring
5, the reaction conditions of sour molten hydrolysis: the reagent concentration of nitric acid is 31%, silver: nitric acid=1: 2,50 ℃ of reactions 3 hours, add water to PH3.5 at 72 ℃ of insulation reaction half an hour
Drop into the electrolytic lead anode sludge by 500 grams, can obtain following product and index:
1, chemical pure Silver Nitrate (21 gram): AgNO
3>99.8% vitriol<0.004%
Technical grade Silver Nitrate (22.75 gram): AgNO
3>99.5% vitriol<0.005%
Add up to Silver Nitrate 43.75 grams
2, alkali type nantokite (108 gram): Cu41 gram
3, chemical fertilizer ammonium nitrate (14.5 gram): N30.5%
4, the slag of using as lead ore (170 gram): pb67 gram, Sb44 gram
Example two
The main chemical of the electrolytic lead anode sludge is with example one
Main processes is with example one
1, the molten reaction conditions that soaks silver of acid: concentration of nitric acid 31%, anode sludge granularity 90 orders, sour consumption solid-to-liquid ratio=1: 3.5,5.5 hours reaction times, about 68 ℃ of temperature of reaction
2, the reaction conditions of ammonification complexing: processing industry ammoniacal liquor is to PH=11, temperature of reaction normal temperature
3, the reaction conditions of the heavy silver of acidifying: control adds industrial nitric acid to PH=1; About 3 hours, add excessive in a subtle way hydrochloric acid, normal-temperature reaction
4, the reaction conditions of zinc displacement silver chloride: amount of water is pressed silver chloride: the zinc overdose of water=adding in 1: 2.7, control adds sulfuric acid amount makes PH3~4, stirs
5, acidification hydrolization reaction conditions: reagent concentration of nitric acid 34%, silver: nitric acid=1: 2,45 ℃ of reactions 3 hours add water to PH4.5 and drop into the electrolytic lead anode sludge by 500 grams 80 ℃ of insulation reaction half an hour, can obtain following product and index:
1, chemical pure Silver Nitrate (20.5 gram): AgNO
3>99.8%
Vitriol<0.004%
Industrial nitric acid silver (25 gram): AgNO
3>99.5%
Vitriol<0.005%
Amount to Silver Nitrate 45.5 grams
2, alkali type nantokite (112 gram): Cu41.5 gram
3, chemical fertilizer ammonium nitrate (17 gram): N30.5%
4, the slag of using as lead ore (185 gram): pb69 gram, Sb49 gram
Claims (6)
1, a kind ofly separates the method produce Silver Nitrate from the electrolytic lead anode sludge, it is characterized in that: following steps with wet method
1.1 making solvent with rare nitric acid is that 70~100 purpose electrolytic lead anode sludge leach to granularity.
1.2 in the clear liquid of the molten leaching of acid, add excessive industrial ammonia, make Cu
++Ag
+Complexing is a complex ion; Separate and remove impurity.
1.3 in the complex solution of silver-bearing copper, add the nitric acid acidifying, in 2~3 hours, add the heavy silver chloride of excessive in a subtle way hydrochloric acid then.
1.4 in silver chloride, add entry, excessive zinc metal sheet and sulfuric acid, silver chloride be replaced into silver.
1.5 dissolve silver with reagent nitric acid, in its solution, add entry and be hydrolyzed.
2, method according to claim 11 is characterized in that: concentration of nitric acid is 30~40%, and solid-to-liquid ratio is 1: 2.5~3.5, and leaching temperature of reaction is 50~70 ℃, reacts 4~6 hours.
3, method according to claim 12 is characterized in that: under the stirred solution situation, adding ammoniacal liquor in 3~4 hours is till 10~11 to PH.
4, method according to claim 13 is characterized in that: add industrial nitric acid in solution, add-on is controlled at till solution PH to 1~2.
5, method according to claim 14 is characterized in that: the water yield of adding is a silver chloride: water=1: 2.5~3, add sulfuric acid in batches, and add-on is 3~4 for control PH, and stirs often.
6, method according to claim 15, it is characterized in that: the concentration of nitric acid of adding is 30~35%, and add-on solid-to-liquid ratio=1: 2 was 40~50 ℃ of reactions 3 hours, and continue 70~80 ℃ of insulation reaction half an hour, controlling amount of water afterwards is 3.5~4.5 to the PH of solution.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN90107798A CN1059938A (en) | 1990-09-12 | 1990-09-12 | Wet process for preparing silver nitrate from anode mud of electrolytic lead |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN90107798A CN1059938A (en) | 1990-09-12 | 1990-09-12 | Wet process for preparing silver nitrate from anode mud of electrolytic lead |
Publications (1)
Publication Number | Publication Date |
---|---|
CN1059938A true CN1059938A (en) | 1992-04-01 |
Family
ID=4880718
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---|---|---|---|
CN90107798A Pending CN1059938A (en) | 1990-09-12 | 1990-09-12 | Wet process for preparing silver nitrate from anode mud of electrolytic lead |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1045795C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis |
CN1306268C (en) * | 2004-11-25 | 2007-03-21 | 广州有色金属研究院 | Analysis method for silver in copper anode mud |
CN100547094C (en) * | 2007-11-30 | 2009-10-07 | 浙江工业大学 | The recoverying and utilizing method of the acid waste liquid that the recycling lead of abandoned lead acid accumulator process produces |
CN102205987A (en) * | 2010-12-17 | 2011-10-05 | 何侠 | Method for preparing silver chloride and aluminum chloride by using ethylene oxidation method in presence of waste silver catalyst |
CN105886778A (en) * | 2016-05-16 | 2016-08-24 | 衢州学院 | Metal extracting method for waste electronic product |
CN108165749A (en) * | 2017-12-29 | 2018-06-15 | 广西生富锑业科技股份有限公司 | Silver-colored recovery method in a kind of jamesonite waste residue |
CN110964908A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recycling method of photovoltaic module |
-
1990
- 1990-09-12 CN CN90107798A patent/CN1059938A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1045795C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Method for recovering platinum and lead from anode slime of hydrogen peroxide production by electrolysis |
CN1306268C (en) * | 2004-11-25 | 2007-03-21 | 广州有色金属研究院 | Analysis method for silver in copper anode mud |
CN100547094C (en) * | 2007-11-30 | 2009-10-07 | 浙江工业大学 | The recoverying and utilizing method of the acid waste liquid that the recycling lead of abandoned lead acid accumulator process produces |
CN102205987A (en) * | 2010-12-17 | 2011-10-05 | 何侠 | Method for preparing silver chloride and aluminum chloride by using ethylene oxidation method in presence of waste silver catalyst |
CN105886778A (en) * | 2016-05-16 | 2016-08-24 | 衢州学院 | Metal extracting method for waste electronic product |
CN108165749A (en) * | 2017-12-29 | 2018-06-15 | 广西生富锑业科技股份有限公司 | Silver-colored recovery method in a kind of jamesonite waste residue |
CN108165749B (en) * | 2017-12-29 | 2019-09-03 | 广西生富锑业科技股份有限公司 | A method of recycling silver from jamesonite waste residue |
CN110964908A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recycling method of photovoltaic module |
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