CN110528026A - A kind of lead plaster acidity Solid phase electrolysis method - Google Patents
A kind of lead plaster acidity Solid phase electrolysis method Download PDFInfo
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- CN110528026A CN110528026A CN201910851298.XA CN201910851298A CN110528026A CN 110528026 A CN110528026 A CN 110528026A CN 201910851298 A CN201910851298 A CN 201910851298A CN 110528026 A CN110528026 A CN 110528026A
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- lead
- lead plaster
- solid phase
- cathode
- electrolysis
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- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 55
- 239000011505 plaster Substances 0.000 title claims abstract description 47
- 239000007790 solid phase Substances 0.000 title claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003792 electrolyte Substances 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 16
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 150000002611 lead compounds Chemical class 0.000 claims abstract description 8
- 229910000978 Pb alloy Inorganic materials 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 238000009938 salting Methods 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000010405 anode material Substances 0.000 claims description 4
- 239000012876 carrier material Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000011133 lead Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 13
- 239000003513 alkali Substances 0.000 abstract description 7
- 230000002378 acidificating effect Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000007772 electrode material Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010963 304 stainless steel Substances 0.000 description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910001245 Sb alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000002140 antimony alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011530 conductive current collector Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000002142 lead-calcium alloy Substances 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical group [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The present invention provides a kind of lead plaster acidity Solid phase electrolysis methods, the method is characterized in that the lead plaster for adjusting moisture is fitted into cathode carrier as cathode, using lead alloy plate as anode, anode and cathode, which is alternatively arranged, is put into electrolytic cell, using dilute sulfuric acid as electrolyte, direct current is passed to, various lead compounds are all reduced to metallic lead in lead plaster.The problem of present invention solves a large amount of sulfate radicals in lead plaster in the prior art and consumes high price alkali generation low price sulfate during alkaline electrolysis, and alkaline consumption and sulfate recycling greatly improve production cost.Above-mentioned cost can be eliminated using acid Solid phase electrolysis, reduce overall cost.The present invention uses acidic electrolysis, and electrolyte substitutes sodium hydroxide with diluted acid salt, adjusts electrode material, and production cost can be greatly reduced, and promotes economic benefit.
Description
Technical field
The present invention relates to lead plaster acidity Solid phase electrolysis methods, belong to metallurgical environmental protection technical field.
Background technique
In metallurgical environmental protection technical field, Solid phase electrolysis technology generallys use alkaline electrolysis, and lead plaster alkalinity Solid phase electrolysis returns
When receiving lead, the sulfate radical in lead plaster is completely converted into sulfate and consumes a large amount of alkali, and the recycling energy consumption of sulfate is also higher, makes this
Technology cost recovery is higher.
Solid phase electrolysis technical industry application at present is mainly used for the lead powder material disposition in waste and old lead acid accumulator recycling lead,
Lead powder material is adjusted into moisture mixing paste, is filled on cathode plate, as cathode, using stainless steel as anode, in alkaline electrolyte
Be electrolysed, various lead compounds are all reduced to metal lead powder under the action of direct current in cathode lead plaster, sulfate radical then or
Pre- desulfurization, or enter electrolyte and form sodium sulphate, as electrolysis carries out, when sodium sulphate reaches a certain concentration in electrolyte, pass through
It is concentrated by evaporation or decrease temperature crystalline mode separates, mother liquor returns to electrolyte, and alkali needs regular replenishment to keep electrolyte concentrations requirement.
1186478 C waste lead battery lead recovery process of notification number CN, electrolyte use NaOH solution;Notification number CN
100576626 C disclose a kind of process of achievable full cycle regeneration of lead acid battery, notification number CN
102296325 B provide process for treating waste lead accumulator through continuous solid phase electrolysis of rotating cathode, 104711637 B of notification number CN
It is a kind of from the patents such as method for recycling metallic lead in solid oxidation lead, lead compound, electrolysis are restored using Solid phase electrolysis method
Liquid all uses NaOH solution.
Above-mentioned alkali formula electrolytic method can realize high current density, and technology maturation is stablized, but lead oxides are dissolved in after alkali in yin
It is extremely upper to be precipitated, easily cause anode and cathode short-circuit, slot pressure should not be made to be difficult to decrease using smaller same pole span electrolysis, and alkaline consumption cost compared with
Height influences technical industryization popularization.
Summary of the invention
The object of the present invention is to provide a kind of lead plaster acidity Solid phase electrolysis methods, to solve to use alkaline electro in the prior art
Drawback brought by solving.
The present invention is achieved through the following technical solutions: a kind of lead plaster acidity Solid phase electrolysis method will adjust moisture
Lead plaster be fitted into cathode carrier as cathode, using lead alloy plate as anode, anode and cathode, which is alternatively arranged, is put into electrolytic cell, with diluted acid salt
Solution is electrolyte, passes to direct current, and various lead compounds are all reduced to metallic lead in lead plaster.
Further: the cathode carrier material is acid resistant metal material.
Further: the cathode carrier material is stainless steel or titanium or metal.
Further: the anode material is acidproof oxidation resistant material.
Further: the anode material is lead or metal or titanium or graphite.
Further: diluted acid salting liquid is sulfuric acid concentration 0 ~ 30%, sulfate concentration 0 ~ 10%, phosphoric acid concentration 0 ~ 20%, phosphoric acid
The arbitrary proportion mixed solution of salinity 0 ~ 10%.
Further: the electrolysis mode of Solid phase electrolysis is constant-potential electrolysis or constant-current electrolysis or constant voltage and current limiting electrolysis mode.
The invention has the advantages that it is acidic electrolysis that the present invention, which changes alkaline electrolysis, electrolyte is directly torn open using used and scrapped battery
The Waste Sulfuric Acid for solving output can be properly added phosphoric acid, sulfate, phosphate according to its concentration, alkali, nothing are not consumed during Solid phase electrolysis
The high cost of alkaline consumption;It is not necessarily to desulfurization conversion before lead plaster electroreduction, shortens process flow, reduces process, without sorbent consumption, reduces
Cost;The sulfate radical that lead sulfate electroreduction generates in lead plaster forms sulfuric acid, improves sulfuric acid concentration in electrolyte, is conducive to spent acid
Comprehensive utilization;Lead oxide forms the lead sulfate insoluble in electrolyte in sulfuric acid and lead plaster, solves solvable lead electrode in electrolyte
Precipitation causes anode and cathode short circuit problem, eliminate cathode fall off lead plaster and go out, tankage when lead plaster dissolve influence to electrolysis procedure,
Same pole span can suitably be reduced, reduce slot pressure, improve current efficiency, reduce and manage labor intensity on slot.
The present invention uses acidic electrolysis, and electrolyte substitutes sodium hydroxide with diluted acid salt, adjusts electrode material, can substantially drop
Low production cost promotes economic benefit.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
Lath is cut into thick 304 stainless steel plates of 2mm and is welded cathode carrier, and processing dimension is 60 × 90 × 30mm;Take 1mm thickness lead calcium
Alloy sheets are cut into two pieces of 60 × 120mm as anode plate;Storage battery coating plate scrap lead cream is taken, (being also possible to other scrap lead cream) adjustment
Mass content to moisture is 20%, is applied in filling cathode carrier, and 60 × 90 × 30mm of cathode plate is made, and the lead plaster amount of filling is 360g;
Density 1.05g/cm is poured into 1000ml beaker3Waste sulfuric acid solution, be added 10ml phosphoric acid, cathode-anode plate is put into rear liquid level
It is higher by cathode plate 10mm;Cathode is connected with rectifier cathode, and anode is connect with rectifier anode, checks errorless rear power transmission, adjustment
Slot pressure is 2.45V, and electric current is gradually increased by small, and current fluctuation becomes smaller and slowly drops after maintaining a period of time when reaching 6.8A or so
It is low, it was electrolysed through 20 hours, electric current is down to 1.6A, stops electrolysis at this time, takes out cathode and unloads lead powder inspection, various lead in former lead plaster
Compound is all reduced to metallic lead.
Embodiment 2
Using upper example cathode-anode plate, the lead plaster amount of filling is identical, and density 1.10g/cm is poured into 1000ml beaker3Waste Sulfuric Acid it is molten
10g anhydrous sodium sulfate is added in liquid, and liquid level is higher by cathode plate 10mm after cathode-anode plate is put into beaker;Pole plate is connect with rectifier,
Check the errorless rear power transmission of anode and cathode connection, adjustment electric current is 4.5A, and beginning voltage is higher, then rapid decrease, reaches the left side 2.4V
It tending towards stability when right and is slowly increased after maintaining a period of time, was electrolysed through 18 hours, voltage reaches 2.6V, stop electrolysis at this time,
It takes out cathode and unloads lead powder inspection, various lead compounds are all reduced to metallic lead in former lead plaster.
Embodiment 3
Lath is cut into thick 304 stainless steel plates of 2mm and is welded cathode carrier 2, and processing dimension is 300 × 450 × 30mm;Take 2mm
Thick lead-antimony alloy plate is cut into tri- pieces of 320 × 500mm as anode plate;It takes the pole plate of scrap battery to remove lower lead plaster and crushes, adjust
Whole moisture 18% applies in filling cathode carrier, and the lead plaster amount of filling is 9.5kg;It is poured into 500 × 800 × 600mm electrolytic cell beaker
Density 1.10g/cm3Waste sulfuric acid solution, cathode-anode plate is put into rear liquid level and is higher by 10 ~ 20mm of cathode plate;Pole plate and rectifier
Connection checks the errorless rear power transmission of anode and cathode connection, and adjustment tank pressure is 2.45V, and electric current is gradually increased by small, reaches current limit
300A time limit galvanic electricity solution simultaneously slowly reduces after maintaining a period of time, is electrolysed through 22 hours, and electric current is down to 80A, stops electrolysis at this time,
It takes out cathode and unloads lead powder inspection, various lead compounds are all reduced to metallic lead in former lead plaster.
To sum up, the present invention is with the acid resistant metal materials processing and fabricating cathode carrier such as stainless steel, titanium or metal, as lead plaster
Container and conductive current collector, all cathode carrier sizes are consistent.With the acidproof oxidation resistant material processing such as lead and its alloy, titanium, graphite
Make anode plate, anode plate suqare and cathode carrier lead plaster coating area equation or appropriate scaling, all anode plate area sizes one
It causes.Lead plaster adjusts moisture to being suitble to fill degree, is packed into that cathode carrier is tamped and both side surface smoothes out, and cathode plate is made, lead plaster is thick
Spend that uniform and all pole plates are identical, and lead plaster thickness is generally 10 ~ 50mm.Diluted acid salting liquid, the diluted acid are added into electrolytic cell
Salting liquid mass concentration is sulfuric acid concentration 0 ~ 30%, in sulfate concentration 0 ~ 10%, phosphoric acid concentration 0 ~ 20%, phosphate concn 0 ~ 10%
One or more kinds of arbitrary proportions mixing, liquid level can cover pole plate after cathode-anode plate and be advisable to be packed into, electricity
Solution liquid can be recycled in a manner of upper entering and lower leaving or bottom in and top out.Cathode-anode plate is alternatively arranged and is placed in electrolytic cell, plate face is parallel
And center is aligned, cathode-anode plate is connected respectively with conducting wire or conductive plate, is connect with rectifier, anode plate is connected with anode, cathode
Plate is connected with cathode, and power transmission electrolysis is until cathode lead compound is all reduced to metal lead powder.It can be adopted during Solid phase electrolysis
The modes such as it is electrolysed with constant-potential electrolysis, constant-current electrolysis and constant voltage and current limiting, because constant-potential electrolysis pilot process electric current is larger, and constant-current electrolysis
Start and latter stage voltage is higher, when practical operation is relatively difficult to achieve, and constant voltage and current limiting electrolysis mode is proper.
It is acidic electrolysis that the present invention, which changes alkaline electrolysis, and electrolyte directly uses the Waste Sulfuric Acid of used and scrapped battery dismantling output,
Phosphoric acid, sulfate, phosphate are optionally added, alkali, no high cost of alkaline consumption are not consumed during Solid phase electrolysis;Nothing before lead plaster electroreduction
Desulfurization conversion is needed, process flow is shortened, reducing process without sorbent consumption reduces cost;Lead sulfate electroreduction produces in lead plaster
Raw sulfate radical forms sulfuric acid, improves sulfuric acid concentration in electrolyte, is conducive to the comprehensive utilization of spent acid;Oxygen in sulfuric acid and lead plaster
Change lead sulfate of the lead formation insoluble in electrolyte, solves solvable lead electrode precipitation in electrolyte and cause anode and cathode short circuit problem, disappear
In addition to cathode fall off lead plaster and go out, tankage when lead plaster dissolve influence to electrolysis procedure, can suitably reduce same pole span, reduce slot
Pressure improves current efficiency, reduces and manages labor intensity on slot.
The present invention uses acidic electrolysis, and electrolyte substitutes sodium hydroxide with diluted acid salt, adjusts electrode material, can substantially drop
Low production cost promotes economic benefit.
Claims (8)
1. lead plaster acidity Solid phase electrolysis method is used as cathode it is characterized in that: the lead plaster for adjusting moisture is fitted into cathode carrier, with
Lead alloy plate is anode, and anode and cathode, which is alternatively arranged, is put into electrolytic cell, using diluted acid salting liquid as electrolyte, passes to direct current, lead plaster
In various lead compounds be all reduced to metallic lead.
2. lead plaster acidity Solid phase electrolysis method according to claim 1, it is characterized in that: the cathode carrier material is acidproof gold
Belong to material.
3. according to lead plaster acidity Solid phase electrolysis method described in claim or 2, it is characterized in that: the cathode carrier material is not
Become rusty steel or titanium or metal.
4. lead plaster acidity Solid phase electrolysis method according to claim 1, it is characterized in that: the anode material is acidproof resistance to
Oxidation material.
5. lead plaster acidity Solid phase electrolysis method according to claim 1 or 4, it is characterized in that: the anode material be lead or
Metal or titanium or graphite.
6. lead plaster acidity Solid phase electrolysis method according to claim 1, it is characterized in that: diluted acid salting liquid be sulfuric acid concentration 0 ~
30%, the arbitrary proportion mixed solution of sulfate concentration 0 ~ 10%, phosphoric acid concentration 0 ~ 20%, phosphate concn 0 ~ 10%.
7. lead plaster acidity Solid phase electrolysis method according to claim 1, it is characterized in that: the electrolysis mode of Solid phase electrolysis is perseverance
Piezoelectricity solution or constant-current electrolysis or constant voltage and current limiting electrolysis mode.
8. lead plaster acidity Solid phase electrolysis method according to claim 1, it is characterized in that: the moisture content of the lead plaster is
20%。
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CN201910851298.XA CN110528026A (en) | 2019-09-10 | 2019-09-10 | A kind of lead plaster acidity Solid phase electrolysis method |
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CN201910851298.XA CN110528026A (en) | 2019-09-10 | 2019-09-10 | A kind of lead plaster acidity Solid phase electrolysis method |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111455404A (en) * | 2020-04-29 | 2020-07-28 | 华中科技大学 | Method for recovering lead from waste lead paste by solid-phase electrolysis method |
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CN107204496A (en) * | 2017-06-21 | 2017-09-26 | 湘潭大学 | A kind of method that waste lead acid battery lead plaster prepares pure lead |
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2019
- 2019-09-10 CN CN201910851298.XA patent/CN110528026A/en active Pending
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CN111455404A (en) * | 2020-04-29 | 2020-07-28 | 华中科技大学 | Method for recovering lead from waste lead paste by solid-phase electrolysis method |
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