CN110453077A - A kind of method that scrap lead cream recycles - Google Patents
A kind of method that scrap lead cream recycles Download PDFInfo
- Publication number
- CN110453077A CN110453077A CN201910788415.2A CN201910788415A CN110453077A CN 110453077 A CN110453077 A CN 110453077A CN 201910788415 A CN201910788415 A CN 201910788415A CN 110453077 A CN110453077 A CN 110453077A
- Authority
- CN
- China
- Prior art keywords
- lead
- added
- acid
- obtains
- precipitating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—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
- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- 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
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to scrap lead cream processing technology fields, a kind of method that scrap lead cream recycles is disclosed, method includes: that scrap lead cream is added in acid solution to form slurry, and reducing agent is added into slurry, high price lead compound is reduced to plumbeous compound, obtains mixture;Mixture is filtered, filtrate and filter residue are respectively obtained;Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Desulfurization in desulfurizing agent solution is added in lead sulfate precipitation and obtains ceruse precipitating, ceruse precipitating is thermally decomposed to yield into lead oxide;Desulfurization precipitating in desulfurizing agent solution is added in filter residue, is dissolved after precipitating thermal decomposition, electro-deposition obtains elementary lead.Scrap lead cream can sufficiently be recycled by this method, obtain the lead of higher degree and the oxide of lead, not the impurity such as barium sulfate-containing and calcium sulfate, the lead of recycling and the oxide of lead can be directly applied in lead-acid accumulator.
Description
Technical field
The present invention relates to a kind of methods that scrap lead cream recovery technology field more particularly to scrap lead cream recycle.
Background technique
Lead-acid accumulator is a kind of battery that yield is maximum in all kinds of batteries in the world, purposes is most wide, lead consumed by it
Account for the 82% of global total lead.But the explored lead reserves in the world are 1.25 hundred million tons, and annual yield is 5,770,000 tons, by
This calculates that the time limit of exploiting of global lead ore is only 22 years.China is the maximum lead-acid storage battery production state in the whole world and exported country,
The lead-acid accumulator generated every year reaches millions of tons.
Waste and old lead acid accumulator is a kind of hazardous waste, if arbitrarily thrown without processing, decomposites the weight come
Metallic lead and toxic waste liquid can bring serious pollution to environment, extremely be detrimental to health;And lead sulfate and titanium dioxide in lead plaster
The content of lead is higher, is the most important part of waste lead acid battery lead resource reclaim.
Main component in scrap lead cream is PbSO4、PbO2, PbO and Pb, in addition there are some other impurity.Master when recycling
If the oxide of recycling lead or lead, in the prior art also has and scrap lead cream is recycled, it is usually that scrap lead cream is whole
Body recycles, but this recovery method haves the shortcomings that very big, there is impurity, such as: barium sulfate, calcium sulfate removal separation are stranded
Difficulty, when application, are restricted.Also have and directly dissolve scrap lead cream, then electro-deposition obtains elementary lead, but this power consumption
Huge, practicability is poor.
Summary of the invention
In view of this, the present invention provides a kind of scrap lead cream recycle method, by this method can to scrap lead cream into
Row sufficiently recycling, obtains the lead of higher degree and the oxide of lead.
A kind of method that scrap lead cream recycles, method include:
S1. scrap lead cream is added in acid solution and forms slurry, reducing agent is added into slurry, high price lead compound is restored
For plumbeous compound, mixture is obtained;
S2. mixture is filtered, respectively obtains filtrate and filter residue;
S3. sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Desulfurization in desulfurizing agent solution is added in lead sulfate precipitation to obtain
It is precipitated to ceruse, ceruse precipitating is thermally decomposed to yield into lead oxide;
S4. desulfurization in desulfurizing agent solution is added in filter residue to precipitate, is dissolved after precipitating thermal decomposition, electro-deposition obtains simple substance
Lead.
Preferably, the acid solution in the S1 is organic sulfonic acid solution.
Preferably, the organic sulfonic acid is Loprazolam, ethane sulfonic acid, trifluoromethayl sulfonic acid and 3- hydroxypropanesulfonic acid
One of or it is a variety of.
Preferably, acid amount and the mass ratio of the material of scrap lead cream are (0.1-100) in the S1: 1.
Preferably, the acid amount and the amount of the substance of scrap lead cream are (1-10): 1.
Preferably, the reducing agent is one of hydrogen peroxide, ethanedioic acid, sodium sulfite and glucose or a variety of.
Preferably, the desulfurizing agent is one of ammonium carbonate, ammonium hydrogen carbonate, sodium carbonate or a variety of.
Preferably, the S3 specifically:
Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Lead sulfate precipitation is added in desulfurizing agent solution, 40- is stirred
70min, desulfurization obtain ceruse precipitating, thermally decompose to yield lead oxide at a temperature of ceruse is deposited in 420-460 DEG C.
Preferably, the S4 specifically:
Filter residue is added in desulfurizing agent solution, 40-70min is stirred, desulfurization precipitating is hot at a temperature of being deposited in 420-460 DEG C
Addition strong acid carries out precipitating dissolution and obtains electrolyte after decomposition, and electro-deposition electrolyte obtains elementary lead.
Preferably, the strong acid is fluosilicic acid.
The present invention provides a kind of methods that scrap lead cream recycles, and can sufficiently be returned to scrap lead cream by this method
It receives, obtains the lead of higher degree and the oxide of lead, not the impurity such as barium sulfate-containing and calcium sulfate, the lead of recycling and lead
Oxide can be directly applied in lead-acid accumulator;And when using organic sulfonic acid, it can effectively avoid using generation volatile nitrogen oxygen
The organic monoacids aqueous solution such as the nitric acid of compound and larger volatile formic acid, acetic acid, is conducive to environmental protection.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are some of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
It should be appreciated that ought use in this specification and in the appended claims, term " includes " and "comprising" instruction
Described feature, entirety, step, operation, the presence of element and/or component, but one or more of the other feature, whole is not precluded
Body, step, operation, the presence or addition of element, component and/or its set.
It will be further appreciated that the term "and/or" used in description of the invention and the appended claims is
Refer to any combination and all possible combinations of one or more of associated item listed, and including these combinations.
A kind of method that scrap lead cream recycles, method include:
Scrap lead cream is added in acid solution and forms slurry, reducing agent is added into slurry, high price lead compound is reduced to
Plumbeous compound obtains mixture;Wherein, acid amount and the mass ratio of the material of scrap lead cream are (0.1-100): 1, it is general using acid
Amount and the amount of the substance of scrap lead cream are (1-10): 1;Acid solution be generally organic sulfonic acid solution, organic sulfonic acid be Loprazolam,
One of ethane sulfonic acid, trifluoromethayl sulfonic acid and 3- hydroxypropanesulfonic acid are a variety of;Reducing agent is hydrogen peroxide, second two
One of acid, sodium sulfite and glucose are a variety of.
Mixture is filtered, filtrate and filter residue are respectively obtained;
Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Lead sulfate precipitation is added in desulfurizing agent solution, 40- is stirred
70min, desulfurization obtain ceruse precipitating, thermally decompose to yield lead oxide at a temperature of ceruse is deposited in 420-460 DEG C;
Filter residue is added in desulfurizing agent solution, 40-70min is stirred, desulfurization precipitating is hot at a temperature of being deposited in 420-460 DEG C
Addition strong acid carries out precipitating dissolution and obtains electrolyte after decomposition, and electro-deposition electrolyte obtains elementary lead;Strong acid is generally adopted as fluorine
Silicic acid;Desulfurizing agent is one of ammonium carbonate, ammonium hydrogen carbonate, sodium carbonate or a variety of.
Specific embodiment 1
The Loprazolam aqueous solution slurrying containing 200Kg is added in the 100Kg waste lead acid battery lead plaster of lead tolerance 71.3%,
Ethanedioic acid is added with stirring until releasing without gas, then filters, respectively obtains filter residue and filtrate.
Sulfuric acid is added into filtrate until the lead sulfate precipitation of generation, pure water is recovered by filtration there is no precipitating generation
Obtain lead sulfate 45Kg;The aqueous solution of the ammonium hydrogen carbonate containing 20Kg is added, stirs desulfurization in 60 minutes, ceruse filter cake is obtained by filtration,
It is decomposed at a temperature of 450 DEG C after Washing of Filter Cake and obtains lead oxide 38Kg, non-lead elementary metal impurities are free of in lead oxide.
The aqueous solution of the ammonium hydrogen carbonate containing 30Kg is added in filter residue, stirs desulfurization in 60 minutes, precipitated filter cakes, filter cake is obtained by filtration
It is decomposed at a temperature of 450 DEG C after washing and obtains secondary oxidative lead, silicate fluoride solution is added until complete molten, electro-deposition obtains high purity lead
37Kg, purity 99.91%;
Elementary lead quality m1, lead oxide m2, primeval lead amount is M, conversion ratio w;
According to w=(m1+207m2/ 239)/M, the conversion ratio for calculating lead recycling is 98%.
Specific embodiment 2
The ethane sulfonic acid aqueous solution slurrying containing 220Kg is added in the 100Kg waste lead acid battery lead plaster of lead tolerance 68.7%,
Hydrogenperoxide steam generator is added with stirring until releasing without gas, is then filtered, is divided into two and respectively obtains filter residue and filtrate.
Sulfuric acid is added into filtrate until the lead sulfate precipitation of generation, pure water is recovered by filtration there is no precipitating generation
Obtain lead sulfate 44Kg;The aqueous solution of the ammonium carbonate containing 25Kg is added, stirs desulfurization in 60 minutes, ceruse filter cake is obtained by filtration, filters
It is decomposed at a temperature of 430 DEG C after cake washing and obtains lead oxide 37Kg, lead oxide is free of non-lead elementary metal impurities.
The aqueous solution of the ammonium carbonate containing 30Kg is added in filter residue, stirs desulfurization in 60 minutes, precipitated filter cakes is obtained by filtration, filter cake is washed
It is decomposed at a temperature of 430 DEG C after washing and obtains secondary oxidative lead, silicate fluoride solution is added until complete molten, electro-deposition obtains high purity lead
36Kg, purity 99.90%.
Elementary lead quality m1, lead oxide m2, primeval lead amount is M, conversion ratio w;
According to w=(m1+207m2/ 239)/M, the conversion ratio for calculating lead recycling is 99%.
Specific embodiment 3
It is water-soluble that the 3- hydroxypropanesulfonic acid containing 230Kg is added in the 100Kg waste lead acid battery lead plaster of lead tolerance 71.1%
Liquefaction slurry is added with stirring hydrogenperoxide steam generator until releasing without gas, and filtering is divided into obtaining filter residue and filtrate.
Sulfuric acid is added into filtrate until the lead sulfate precipitation of generation, pure water is recovered by filtration there is no precipitating generation
Obtain lead sulfate 45Kg;The aqueous solution of the sodium carbonate containing 28Kg is added, stirs desulfurization in 50 minutes, ceruse filter cake is obtained by filtration, filters
It is decomposed at a temperature of 450 DEG C after cake washing and obtains lead oxide 38Kg, wherein lead oxide is free of non-lead elementary metal impurities.
The aqueous solution of the sodium carbonate containing 40Kg is added in filter residue, stirs desulfurization in 60 minutes, precipitated filter cakes is obtained by filtration, filter cake is washed
It is decomposed at a temperature of 440 DEG C after washing and obtains secondary oxidative lead, silicate fluoride solution is added until complete molten, electro-deposition obtains high purity lead
37.5Kg, purity 99.89%.
Elementary lead quality m1, lead oxide m2, primeval lead amount is M, conversion ratio w;
According to w=(m1+207m2/ 239)/M, the conversion ratio for calculating lead recycling is 99%.
Specific embodiment 4
The trifluoromethayl sulfonic acid aqueous solution containing 240Kg is added in the 100Kg waste lead acid battery lead plaster of lead tolerance 72.77%
Slurrying is added with stirring ethanedioic acid until releasing without gas, and filtering respectively obtains filter residue and filtrate.
Sulfuric acid is added into filtrate until the lead sulfate precipitation of generation, pure water is recovered by filtration there is no precipitating generation
Obtain lead sulfate 45.5Kg;The aqueous solution of the ammonium hydrogen carbonate containing 28Kg is added, stirs desulfurization in 50 minutes, ceruse filter is obtained by filtration
Cake decomposes after Washing of Filter Cake at a temperature of 450 DEG C and obtains lead oxide 38.7Kg, and lead oxide is free of non-lead elementary metal impurities.
The aqueous solution of the ammonium hydrogen carbonate containing 40Kg is added in filter residue, stirs desulfurization in 60 minutes, precipitated filter cakes, filter cake is obtained by filtration
It is decomposed at a temperature of 450 DEG C after washing and obtains secondary oxidative lead, silicate fluoride solution is added until complete molten, electro-deposition obtains high purity lead
37.8Kg, purity 99.92%.
Elementary lead quality m1, lead oxide m2, primeval lead amount is M, conversion ratio w;
According to w=(m1+207m2/ 239)/M, the conversion ratio for calculating lead recycling is 98%.
Specific embodiment 5
Scrap lead cream is added in Loprazolam and ethane sulfonic acid solution and forms slurry, sodium sulfite is added into slurry,
High price lead compound is reduced to plumbeous compound, obtains mixture;Wherein, Loprazolam and ethane sulfonic acid and scrap lead cream
The mass ratio of the material be 100:1;
Mixture is filtered, filtrate and filter residue are respectively obtained;
Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Ammonium hydrogen carbonate and sodium carbonate is added in lead sulfate precipitation
In solution, 70min is stirred, desulfurization obtains ceruse precipitating, ceruse is deposited at a temperature of 420 DEG C and thermally decomposes to yield oxidation
Lead;Lead oxide is free of non-lead elementary metal impurities.
Filter residue is added in sal volatile, 40min is stirred, desulfurization precipitating adds after thermally decomposing at a temperature of being deposited in 460 DEG C
Enter fluosilicic acid carry out precipitating dissolution obtain electrolyte, electro-deposition electrolyte obtains elementary lead, and elementary lead reaches purity 99.93%;
Conversion ratio by the recycling of above-mentioned calculating lead is 99%.
Specific embodiment 6
Scrap lead cream is added in trifluoromethayl sulfonic acid solution and forms slurry, sodium sulfite is added into slurry, by high price lead
Compound is reduced to plumbeous compound, obtains mixture;Wherein, acid amount and the mass ratio of the material of scrap lead cream are 0.1:1;
Mixture is filtered, filtrate and filter residue are respectively obtained;
Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Lead sulfate precipitation is added in ammonium bicarbonate soln, stirring
40min, desulfurization obtain ceruse precipitating, ceruse are deposited at a temperature of 460 DEG C and thermally decomposes to yield lead oxide;Lead oxide is free of
Non-lead elementary metal impurities.
Filter residue is added in sodium carbonate liquor, 70min is stirred, desulfurization precipitating adds after thermally decomposing at a temperature of being deposited in 420 DEG C
Enter fluosilicic acid carry out precipitating dissolution obtain electrolyte, electro-deposition electrolyte obtains elementary lead, and elementary lead reaches purity 99.91%.
Conversion ratio by the recycling of above-mentioned calculating lead is 98%.
Specific embodiment 7
Scrap lead cream is added in ethane sulfonic acid solution and forms slurry, glucose is added into slurry, by high price lead compound
It is reduced to plumbeous compound, obtains mixture;Wherein, acid amount and the mass ratio of the material of scrap lead cream are 8:1;
Mixture is filtered, filtrate and filter residue are respectively obtained;
Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Lead sulfate precipitation is added in ammonium bicarbonate soln, stirring
60min, desulfurization obtain ceruse precipitating, ceruse are deposited at a temperature of 450 DEG C and thermally decomposes to yield lead oxide;Lead oxide is free of
Non-lead elementary metal impurities.
Filter residue is added in sal volatile, 50min is stirred, desulfurization precipitating adds after thermally decomposing at a temperature of being deposited in 440 DEG C
Enter fluosilicic acid carry out precipitating dissolution obtain electrolyte, electro-deposition electrolyte obtains elementary lead;Elementary lead reaches purity 99.93%.
Conversion ratio by the recycling of above-mentioned calculating lead is 99%.
In specific embodiment 1-7, filtrate precipitating, then desulfurization obtain ceruse precipitating purity it is very high, so thermal decomposition system
The lead oxide purity is high obtained, is free of non-lead elementary metal impurities;And in filter residue other than lead sulfate, it is general that there are also some other miscellaneous
Matter by desulfurization and thermally decomposes, then obtains elementary lead by electro-deposition electrolyte;Elementary lead reaches 99.9% or more purity.It is logical
Cross and separate scrap lead cream, then carry out step recycling respectively so that the scrap lead cream rate of recovery is especially high, can achieve 98% with
On, and relative to simple electrolysis, save a large amount of electric resources.
Separated using step, utilize scrap lead cream lead resource method obtain two kinds of qualities lead sulfate: high purity sulphur lead plumbate and
Thick lead sulfate.High purity sulphur lead plumbate can obtain the high pure zirconia that ceruse obtains being free of after thermally decomposing other metallic elements after desulfurization
Lead, avoid existing method prepare lead oxide lead oxide power material not can be removed barium sulfate and sulfuric acid calcium impurities and problem, and
Lead resource in thick lead sulfate recycles to obtain high purity lead through desulfurization dissolution-electro-deposition.
And it is big when using the organic sulfonic acid substitution for showing as strong acid and the basic non-volatility of aqueous solution in aqueous solution can produce
Amount endangers the nitric acid of environment nitrogen oxides, aqueous solution still has the organic monoacids such as larger volatile formic acid, acetic acid as lysate
When, be conducive to environmental protection, and organic sulfonic acid does not consume actually, regeneration is realized during sulfuric acid is added.
It is free from foreign meter due to recovery product lead oxide and lead simple substance purity is high, lead-acid accumulator system can be directly applied to
In making.
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
It is described in detail herein, applies specific case and the principle of the present invention and embodiment are explained
It states, above embodiments are merely used to help understand method and its core concept of the invention;Meanwhile for the general skill of this field
Art personnel, according to the thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion this
Description should not be construed as limiting the invention.
It is apparent to those skilled in the art that for convenience and simplicity of description, the system of foregoing description
It with the specific work process of unit, can refer to corresponding processes in the foregoing method embodiment, details are not described herein.
Claims (10)
1. a kind of method that scrap lead cream recycles, which is characterized in that method includes:
S1. scrap lead cream is added in acid solution and forms slurry, reducing agent is added into slurry, high price lead compound is reduced to two
Valence lead compound, obtains mixture;
S2. mixture is filtered, respectively obtains filtrate and filter residue;
S3. sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Desulfurization in desulfurizing agent solution is added in lead sulfate precipitation and obtains carbon
Ceruse precipitating is thermally decomposed to yield lead oxide by lead plumbate precipitating;
S4. desulfurization in desulfurizing agent solution is added in filter residue to precipitate, is dissolved after precipitating thermal decomposition, electro-deposition obtains elementary lead.
2. the method according to claim 1, wherein the acid solution in the S1 is organic sulfonic acid solution.
3. according to the method described in claim 2, it is characterized in that, the organic sulfonic acid is Loprazolam, ethane sulfonic acid, trifluoro
One of Loprazolam and 3- hydroxypropanesulfonic acid are a variety of.
4. method according to claim 1 to 3, which is characterized in that the amount of acid amount and the substance of scrap lead cream in the S1
Than for (0.1-100): 1.
5. according to the method described in claim 4, it is characterized in that, the acid amount and the amount of the substance of scrap lead cream are (1-10):
1。
6. the method according to claim 1, wherein the reducing agent is hydrogen peroxide, ethanedioic acid, sodium sulfite
And one of glucose or a variety of.
7. the method according to claim 1, wherein the desulfurizing agent is ammonium carbonate, in ammonium hydrogen carbonate, sodium carbonate
It is one or more.
8. the method according to claim 1, wherein the S3 specifically:
Sulfuric acid is added into filtrate, obtains lead sulfate precipitation;Lead sulfate precipitation is added in desulfurizing agent solution, 40- is stirred
70min, desulfurization obtain ceruse precipitating, thermally decompose to yield lead oxide at a temperature of ceruse is deposited in 420-460 DEG C.
9. the method according to claim 1, wherein the S4 specifically:
Filter residue is added in desulfurizing agent solution, 40-70min is stirred, desulfurization precipitating thermally decomposes at a temperature of being deposited in 420-460 DEG C
Addition strong acid carries out precipitating dissolution and obtains electrolyte afterwards, and electro-deposition electrolyte obtains elementary lead.
10. according to the method described in claim 9, it is characterized in that, the strong acid is fluosilicic acid.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910788415.2A CN110453077A (en) | 2019-08-26 | 2019-08-26 | A kind of method that scrap lead cream recycles |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910788415.2A CN110453077A (en) | 2019-08-26 | 2019-08-26 | A kind of method that scrap lead cream recycles |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110453077A true CN110453077A (en) | 2019-11-15 |
Family
ID=68488962
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910788415.2A Pending CN110453077A (en) | 2019-08-26 | 2019-08-26 | A kind of method that scrap lead cream recycles |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110453077A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112430744A (en) * | 2020-10-09 | 2021-03-02 | 超威电源集团有限公司 | Waste lead plaster recovery method |
CN112614972A (en) * | 2020-12-15 | 2021-04-06 | 湘潭大学 | Preparation method of negative plate of lead-acid battery and lead-acid battery |
CN113481374A (en) * | 2021-07-13 | 2021-10-08 | 湘潭大学 | Self-coupling reaction method for lead and lead dioxide in waste lead paste |
CN113740320A (en) * | 2021-09-26 | 2021-12-03 | 北京化工大学 | Method for analyzing content of copper impurities in waste lead-acid storage battery recovery process |
CN114317947A (en) * | 2021-12-14 | 2022-04-12 | 北京工业大学 | Method and device for two-stage mechanical reinforced desulfurization of waste lead paste |
CN114438339A (en) * | 2022-01-07 | 2022-05-06 | 骆驼集团(安徽)再生资源有限公司 | Crude lead refining process for recycling lead-acid batteries |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101608264A (en) * | 2009-06-30 | 2009-12-23 | 张天任 | A kind of waste lead recovering method for lead-acid storage batteries |
CN101636512A (en) * | 2007-01-17 | 2010-01-27 | 米尔布鲁克铅再生科技有限公司 | From the scrap lead battery that contains electrode paste, reclaim the lead of high purity carbon lead plumbate form |
CN103627903A (en) * | 2013-11-01 | 2014-03-12 | 遵义市金狮金属合金有限公司 | Recovery method for recycling lead in waste lead-acid storage batteries |
CN104039991A (en) * | 2012-11-13 | 2014-09-10 | 巴斯夫欧洲公司 | Recovering lead from a mixed oxidized material |
WO2015195393A1 (en) * | 2014-06-20 | 2015-12-23 | Johnson Controls Technology Company | Systems and methods for closed-loop recycling of a liquid component of a leaching mixture when recycling lead from spent lead-acid batteries |
CN105895983A (en) * | 2014-12-12 | 2016-08-24 | 中国人民解放军63971部队 | Method for preparing high-purity PbO by cycle wet method |
CN106676270A (en) * | 2017-01-05 | 2017-05-17 | 中南大学 | All-wet method for extracting lead from lead plaster and lead sulfide concentrate |
CN107164636A (en) * | 2017-05-27 | 2017-09-15 | 湘潭大学 | A kind of method that high-purity lead oxide is reclaimed in waste lead acid battery processing |
-
2019
- 2019-08-26 CN CN201910788415.2A patent/CN110453077A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101636512A (en) * | 2007-01-17 | 2010-01-27 | 米尔布鲁克铅再生科技有限公司 | From the scrap lead battery that contains electrode paste, reclaim the lead of high purity carbon lead plumbate form |
CN101608264A (en) * | 2009-06-30 | 2009-12-23 | 张天任 | A kind of waste lead recovering method for lead-acid storage batteries |
CN104039991A (en) * | 2012-11-13 | 2014-09-10 | 巴斯夫欧洲公司 | Recovering lead from a mixed oxidized material |
CN103627903A (en) * | 2013-11-01 | 2014-03-12 | 遵义市金狮金属合金有限公司 | Recovery method for recycling lead in waste lead-acid storage batteries |
WO2015195393A1 (en) * | 2014-06-20 | 2015-12-23 | Johnson Controls Technology Company | Systems and methods for closed-loop recycling of a liquid component of a leaching mixture when recycling lead from spent lead-acid batteries |
CN105895983A (en) * | 2014-12-12 | 2016-08-24 | 中国人民解放军63971部队 | Method for preparing high-purity PbO by cycle wet method |
CN106676270A (en) * | 2017-01-05 | 2017-05-17 | 中南大学 | All-wet method for extracting lead from lead plaster and lead sulfide concentrate |
CN107164636A (en) * | 2017-05-27 | 2017-09-15 | 湘潭大学 | A kind of method that high-purity lead oxide is reclaimed in waste lead acid battery processing |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112430744A (en) * | 2020-10-09 | 2021-03-02 | 超威电源集团有限公司 | Waste lead plaster recovery method |
CN112614972A (en) * | 2020-12-15 | 2021-04-06 | 湘潭大学 | Preparation method of negative plate of lead-acid battery and lead-acid battery |
CN113481374A (en) * | 2021-07-13 | 2021-10-08 | 湘潭大学 | Self-coupling reaction method for lead and lead dioxide in waste lead paste |
CN113740320A (en) * | 2021-09-26 | 2021-12-03 | 北京化工大学 | Method for analyzing content of copper impurities in waste lead-acid storage battery recovery process |
CN114317947A (en) * | 2021-12-14 | 2022-04-12 | 北京工业大学 | Method and device for two-stage mechanical reinforced desulfurization of waste lead paste |
CN114317947B (en) * | 2021-12-14 | 2023-12-29 | 北京工业大学 | Method and device for mechanically strengthening desulfurization of waste lead plaster in two sections |
CN114438339A (en) * | 2022-01-07 | 2022-05-06 | 骆驼集团(安徽)再生资源有限公司 | Crude lead refining process for recycling lead-acid batteries |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110453077A (en) | A kind of method that scrap lead cream recycles | |
WO2021047352A1 (en) | Manganese-lithium separation and pre-extraction liquid preparation processes in comprehensive recovery of ternary battery waste, and method for comprehensive recovery of cobalt-nickel-manganese-lithium elements from ternary battery waste | |
CN110527836A (en) | A kind of method that ion-exchange recycles valuable metal in waste and old nickel cobalt manganese lithium ion battery | |
CN102618884B (en) | Lead regeneration method for recovering lead paste from waste lead acid storage battery by wet method | |
CN112768800B (en) | Recovery method of lithium iron phosphate anode material | |
CN103146923B (en) | Method for producing lead oxide by recovering waste lead-acid batteries based on atom economy way | |
CN111945002B (en) | Method for removing copper from waste lithium batteries by recovery wet process | |
CN110512080A (en) | Valuable metal separation and recovery method in a kind of waste and old nickel cobalt manganese lithium ion battery | |
CN104393364B (en) | A kind of method for preparing PbO from the direct wet method of waste lead acid battery | |
CN102534223B (en) | Method for recovering valuable metals from spent lithium-ion batteries | |
CN110474123B (en) | Comprehensive recovery method of waste lithium iron phosphate battery positive electrode material | |
CN106129511A (en) | A kind of method of comprehensively recovering valuable metal from waste and old lithium ion battery material | |
KR101718000B1 (en) | Method for Recycling Lead Oxide from Lead Oxide-Containing Waste Material | |
CN108622943A (en) | A method of LITHIUM BATTERY nickel sulfate and cobaltous sulfate are produced with useless nickel cobalt (alloy) | |
CN113896211A (en) | Resource treatment method for waste lithium iron phosphate batteries | |
CN113104897A (en) | Method for preparing battery-grade manganese sulfate by separating nickel, cobalt, lithium and manganese from battery black powder | |
CN115231537B (en) | Method for preparing ferric phosphate from iron-phosphorus slag, ferric phosphate and application thereof | |
US5630931A (en) | Process for the hydrometallurgical and electrochemical treatment of the active mass of exhausted lead batteries, to obtain electrolytic lead and elemental sulphur | |
CN110468281A (en) | Valuable metal separation and recovery method in a kind of waste and old cobalt acid lithium battery | |
CN113981232A (en) | Method for directly leaching and recovering lithium element in aluminum electrolyte waste residue by using aluminum sulfate | |
CN111118311B (en) | Manganese-lithium separation method in comprehensive recovery of ternary battery waste | |
WO2023029573A1 (en) | Method for extracting lithium from waste lithium battery | |
CN112853120A (en) | LiHCO recovered and leached from waste lithium battery3Method for deeply removing fluorine from solution | |
CN111180819A (en) | Preparation method of battery-grade Ni-Co-Mn mixed solution and battery-grade Mn solution | |
CN100389520C (en) | Method for removing sodium ion from recovered nickle sulfate solution of waste nickle-hydrogen and nickle-cadmium |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191115 |
|
RJ01 | Rejection of invention patent application after publication |