CN107164636A - A kind of method that high-purity lead oxide is reclaimed in waste lead acid battery processing - Google Patents
A kind of method that high-purity lead oxide is reclaimed in waste lead acid battery processing Download PDFInfo
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- CN107164636A CN107164636A CN201710388054.3A CN201710388054A CN107164636A CN 107164636 A CN107164636 A CN 107164636A CN 201710388054 A CN201710388054 A CN 201710388054A CN 107164636 A CN107164636 A CN 107164636A
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- lead
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- oxide
- reclaimed
- acid battery
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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
- C22B7/006—Wet processes
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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- 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
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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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- 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
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Secondary Cells (AREA)
Abstract
The present invention relates to the method that high-purity lead oxide is reclaimed in a kind of processing of waste lead acid battery.The method of the present invention includes using the PbO in nitrate reductase lead plaster under 1. acid condition2；2. lead powder reduction nitrate realizes the recycling of nitrate reductase agent into nitrite；3. the lead sulfate in lead plaster is extracted in the reduction lead plaster mixture salt dissolving obtained；4. lead solution addition carbonate deposition generation ceruse heat resolve strengthens the steps such as alkali direct preparation of high-purity lead oxide into high-purity mangesium oxide lead or directly.Present invention process is simple, it is high to obtain lead oxide purity, and reducing agent can be recycled.
Description
Technical field
The invention belongs to resource reclaim and technique is utilized, the lead plaster after more particularly to a kind of waste lead acid battery is broken apart
The method of the high-purity lead oxide obtained after processing, the technique can realize the regeneration and circulation of reducing agent, so that the technique
With good economy.
Background technology
Lead-acid accumulator is in the occasion extensive use such as automobile, electric car, submarine, mobile communication base station, according to incompletely statistics,
Lead accumulator manufacturing firm of China has reached 1500 or so, and about 1.1 hundred million lead-acid accumulators are produced every year, leaded
Amount of metal be about 2,000,000 tons, when estimating 2015, the metallic lead amount contained by used and scrapped battery is up to 3,000,000 tons.Production
Amount is average to be grown at top speed with every year about 20% speed, and lead accumulator yield accounts for the 1/3 of world wide production.Lead in the coming years
Acid accumulator regenerative system market demand is up to 80-100 bar production lines, is roughly equal to the market output values of 6-10 hundred million.
How efficiently, the lead in lead-acid accumulator that reclaims of cleaning turns into great technical need.The wet reclamation of lead plaster
It is considered as more environmentally friendly reviver technology of future generation.
PbSO is mainly contained in the lead plaster after waste lead acid battery is broken apart4(50~60%)、PbO2 (20~30%)、
PbO (10 ~ 20%), a small amount of metallic lead (less than 3%) and a small amount of impurity.If the high price lead economy in lead plaster can be converted
The ceruse of high-purity is prepared for plumbeous compound, then decomposing generation again can high pure oxygen of the direct reuse in battery production
Change lead（Purity>97%）, then very important meaning can be produced.
The content of the invention
It is an object of the invention to provide the method that high-purity lead oxide is reclaimed in a kind of processing of waste lead acid battery, the present invention is related to
And waste lead acid battery it is broken apart after the lead plaster method and technique of the lead oxide that are obtained after processing.The method bag of the present invention
Include the PbO used under 1. acid condition in nitrate reductase lead plaster2；2. lead powder reduction nitrate realizes nitrous acid into nitrite
The recycling of salt reducing agent；3. the lead sulfate in lead plaster is extracted in the reduction lead plaster mixture salt dissolving obtained；4. lead solution
Add carbonate deposition generation ceruse heat resolve and strengthen the oxidation of alkali direct preparation of high-purity into high-purity mangesium oxide lead or directly
The steps such as lead.The present invention has that technique is simple, high, the characteristics of reducing agent can be recycled that obtain lead oxide purity.
By the PbO in lead plaster in wet method prepares lead oxide technique2Divalence lead is reduced at low cost, is the technology key
The step of, the reduction reaction that this law is related to has:
(1) PbO2 + MNO2 + H2SO4 = PbSO4 + MNO3
(2) MNO3 + Pb = PbO + MNO2
It can be seen that reducing agent nitrite is not consumed in itself from reaction equation above, consumption is lead powder, and lead powder is in reaction
In can conversion cost technique target product PbO, therefore this is an Atom economy process.
The technical scheme is that：
A kind of method that high-purity lead oxide is reclaimed in waste lead acid battery processing, comprises the following steps：
（1）Lead plaster is reduced：Lead plaster of the waste lead acid battery after broken apart and nitrite solution are modulated into slurries, Ran Houjia
It is separated by filtration after entering dilute sulfuric acid, stirring reaction, obtains filtrate and lead sulfate filter cake；
（2）Nitrite regenerates：By step（1）Gained filtrate recycle is in step（1）Slurries, when matter of the nitrate in filtrate
Amount fraction reaches that more than 20% is evaporated or freezing and crystallizing, separates out nitrate solid；Heat is produced obtained nitrate altogether with lead powder
Lead oxide and nitrite, product are back to use step（1）；
（3）Lead salt dissolving-precipitation：By step（1）Gained lead sulfate filter cake, adds after salt solution and adds carbonate progress instead
Should, produce ceruse precipitation, gained precipitation separation, drying；
（4）Decompose：By step（3）Gained ceruse solid heat resolve obtains high-purity mangesium oxide lead.
Further, step（1）In, described nitrite is the alkali metal or alkali salt of nitrous acid, and it is added
Amount and PbO in lead plaster2Mol ratio be preferably 0.9 ~ 1.1：1, more preferably 1：1；The solid-to-liquid ratio of nitrite solution and lead plaster
（Volume：Weight）Preferably 1 ~ 10：1, more preferably 2：1；The mol ratio of sulfuric acid and nitrite is preferably 0.2 ~ 1：1, more preferably
For 0.5：1.
Further, step（2）In, described common heat, temperature is 100 ~ 400 DEG C, and the time is 0.1 ~ 3 hour；Nitrate
It is 1 with the ratio between the amount of material of lead powder：1.
Further, step（3）In, described salt is alkali metal salt, ammonium salt or the sodium chloride of acetic acid, its addition and lead
The ratio between amount of material of Pb elements is 3 ~ 10 in cream:1, preferably 5:1；The solid-to-liquid ratio of salting liquid and lead plaster（Volume：Weight）For 3 ~
10:1, preferably 6:1；Reaction temperature is 20 ~ 100 DEG C, and the time is 0.5 ~ 2 hour；The alkali metal salt or ammonium of the preferred carbonic acid of carbonate
The ratio between amount of material of lead element is 0.9 ~ 1.2 in salt, its addition and lysate:1, preferably 1:1.
Further, step（4）In, decomposition temperature is 300 ~ 750 DEG C, and the time is 0.5 ~ 6 hour.
The beneficial effects of the present invention are：
The technique of the present invention has Atom economy, and technique is simple, and reducing agent nitrite forms circulation in using and generating,
Nitrite is constantly recycled in the reduction of brown lead oxide, gained lead oxide purity is very high, can connect
Nearly 100%, direct reuse is fully achieved to the quality requirement of lead-acid accumulator, therefore the present invention can not only realize waste and old lead acid electricity
The recycling in pond, and preparation cost is low, it is good in economic efficiency, with extraordinary industrial application value.
Embodiment
The present invention is described in further details with reference to specific embodiment, but the present invention is not limited thereto.
Embodiment 1
（1）By lead plaster of the waste lead acid battery after broken apart and containing with PbO in lead plaster2The sodium nitrite solution of equimolar amounts
The mol ratio of modulation pulp, addition sulfuric acid solution, sulfuric acid and natrium nitrosum is 0.5:1, now in the middle of linen lead sulfate
Product is separated by filtration；Filtrate is circulated as with the adjusting slurry of lead plaster；
（2）Work as step（1）In the accumulation of sodium nitrate mass fraction to 40%, sodium nitrate of the heating evaporation concentration until in solution 80%
Separate out, the solid that this is filtered out is put into molten-bath, add the lead powder of equimolar amounts, be heated to 200 DEG C, reaction is led to after starting
Apparatus for supercooling regulation and control reaction is unlikely to excessively fierce, cool down and is dissolved in water after 1 hour, and solid is lead oxide, solution for containing
The solution of natrium nitrosum, is back to step（1）In；
（3）Step（1）In obtained lead sulfate product to add solid-to-liquid ratio be 10:1 mass fraction is 50% ammonium acetate solution,
After 80 DEG C of reaction temperature, 0.5 hour time, the mol ratio added with lead element in lysate is 1:1 sal volatile, is obtained
To the white precipitate of ceruse, wash, drying；
（4）Step（3）Obtained ceruse obtains yellow lead oxide product, purity in 500 DEG C of decomposition, time 2 h
99.96%。
Embodiment 2
（1）By lead plaster of the waste lead acid battery after broken apart and containing with PbO in lead plaster2The sodium nitrite solution of equimolar amounts
The mol ratio of modulation pulp, addition sulfuric acid solution, sulfuric acid and natrium nitrosum is 0.8:1, now in the middle of linen lead sulfate
Product is separated by filtration；Filtrate is circulated as with the adjusting slurry of lead plaster；
（2）Work as step（1）In the accumulation of sodium nitrate mass fraction to 30%, sodium nitrate of the heating evaporation concentration until in solution 85%
Separate out, the solid that this is filtered out is put into molten-bath, add the lead powder of equimolar amounts, be heated to 300 DEG C, reaction is led to after starting
Apparatus for supercooling regulation and control reaction is unlikely to excessively fierce, cools down and is dissolved in water after 0.5 hour, solid is lead oxide, solution is
Solution containing natrium nitrosum, is back to step（1）In；
（3）Step（1）In obtained lead sulfate product to add solid-to-liquid ratio be 8:1 mass fraction is 30% sodium chloride solution, instead
Temperature 70 C is answered, after 1 hour time, the mol ratio added with lead element in lysate is 1.2:1 sodium carbonate liquor, is obtained
The white precipitate of ceruse, is washed, drying；
（4）Step（3）Obtained ceruse 1 hour time, obtains yellow lead oxide product, purity in 600 DEG C of decomposition
99.85%。
Embodiment 3
（1）By lead plaster of the waste lead acid battery after broken apart and containing with PbO in lead plaster2The sodium nitrite solution of equimolar amounts
The mol ratio of modulation pulp, addition sulfuric acid solution, sulfuric acid and natrium nitrosum is 0.8:1, now in the middle of linen lead sulfate
Product is separated by filtration；Filtrate is circulated as with the adjusting slurry of lead plaster；
（2）Work as step（1）In the accumulation of sodium nitrate mass fraction to 50%, sodium nitrate analysis of the freezing and crystallizing until in solution 90%
Go out, the solid that this is filtered out is put into molten-bath, add the lead powder of equimolar amounts, be heated to 400 DEG C, reaction passes through after starting
Cooling device regulation and control reaction is unlikely to excessively fierce, cools down and is dissolved in water after 3 hours, and solid is lead oxide, and solution is containing Asia
The solution of sodium nitrate, is back to step（1）In；
（3）Step（1）In obtained lead sulfate product to add solid-to-liquid ratio be 8:1 mass fraction is 40% sodium acetate solution, instead
Answer after 100 DEG C of temperature, 1.5 hours time, the mol ratio added with lead element in lysate is 1.1:1 sodium carbonate liquor,
The white precipitate of ceruse is obtained, is washed, drying；
（4）Step（3）Obtained ceruse 3 hours time, obtains yellow lead oxide product, purity 99.97 in 550 DEG C of decomposition
%。
Claims (8)
1. a kind of method that high-purity lead oxide is reclaimed in waste lead acid battery processing, it is characterised in that comprise the following steps：
（1）Lead plaster is reduced：Lead plaster of the waste lead acid battery after broken apart and nitrite solution are modulated into slurries, Ran Houjia
It is separated by filtration after entering dilute sulfuric acid, stirring reaction, obtains filtrate and lead sulfate filter cake；
（2）Nitrite regenerates：By step（1）Gained filtrate recycle is in step（1）Slurries, when matter of the nitrate in filtrate
Amount fraction reaches that more than 20% is evaporated or freezing and crystallizing, separates out nitrate solid；Heat is produced obtained nitrate altogether with lead powder
Lead oxide and nitrite, product are back to use step（1）；
（3）Lead salt dissolving-precipitation：By step（1）Gained lead sulfate filter cake, adds after salt solution and adds carbonate progress instead
Should, produce ceruse precipitation, gained precipitation separation, drying；
（4）Decompose：By step（3）Gained ceruse solid heat resolve obtains high-purity mangesium oxide lead.
2. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that step
（1）In, described nitrite is the alkali metal or alkali salt of nitrous acid, its addition and PbO in lead plaster2Mol ratio
For 0.9 ~ 1.1：1；The solid-to-liquid ratio of nitrite solution and lead plaster is 1 ~ 10：1.
3. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that sulfuric acid
Mol ratio with nitrite is 0.2 ~ 1：1.
4. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that step
（2）In, described common heat, temperature is 100 ~ 400 DEG C, and the time is 0.1 ~ 3 hour；The ratio between amount of material of nitrate and lead powder is
1：1.
5. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that step
（3）In, described salt is alkali metal salt, ammonium salt or the sodium chloride of acetic acid, its addition and the amount of the material of Pb elements in lead plaster
The ratio between be 3 ~ 10:1；The solid-to-liquid ratio of salting liquid and lead plaster is 3 ~ 10:1.
6. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that step
（3）In, reaction temperature is 20 ~ 100 DEG C, and the time is 0.5 ~ 2 hour.
7. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that step
（3）In, carbonate is the alkali metal salts or ammonium salt of carbonic acid, and the ratio between its addition and the amount of material of lead element in lysate is
0.9~1.2:1。
8. the method that high-purity lead oxide is reclaimed in waste lead acid battery processing according to claim 1, it is characterised in that step
（4）In, decomposition temperature is 300 ~ 750 DEG C, and the time is 0.5 ~ 6 hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453077A (en) * | 2019-08-26 | 2019-11-15 | 湘潭大学 | A kind of method that scrap lead cream recycles |
| CN112359219A (en) * | 2020-11-09 | 2021-02-12 | 汨罗市锦胜科技有限公司 | Method for recovering lead oxide from waste lead-acid storage battery |
| 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 |
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| CN102747227A (en) * | 2012-06-18 | 2012-10-24 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
| CN103014347A (en) * | 2012-12-12 | 2013-04-03 | 北京化工大学 | Method for recycling waste lead-acid cells to directly produce lead oxide |
| CN103773972A (en) * | 2014-01-10 | 2014-05-07 | 张超 | Processing method for lead-bearing raw material |
| CN104789776A (en) * | 2014-01-16 | 2015-07-22 | 北京化工大学 | Method for recovering lead oxide from waste containing lead oxide |
| CN105441686A (en) * | 2016-01-06 | 2016-03-30 | 湘潭大学 | Reducing method for lead dioxide in waste lead plaster |
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2017
- 2017-05-27 CN CN201710388054.3A patent/CN107164636B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102747227A (en) * | 2012-06-18 | 2012-10-24 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
| CN103014347A (en) * | 2012-12-12 | 2013-04-03 | 北京化工大学 | Method for recycling waste lead-acid cells to directly produce lead oxide |
| CN103773972A (en) * | 2014-01-10 | 2014-05-07 | 张超 | Processing method for lead-bearing raw material |
| CN104789776A (en) * | 2014-01-16 | 2015-07-22 | 北京化工大学 | Method for recovering lead oxide from waste containing lead oxide |
| CN105441686A (en) * | 2016-01-06 | 2016-03-30 | 湘潭大学 | Reducing method for lead dioxide in waste lead plaster |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453077A (en) * | 2019-08-26 | 2019-11-15 | 湘潭大学 | A kind of method that scrap lead cream recycles |
| CN112359219A (en) * | 2020-11-09 | 2021-02-12 | 汨罗市锦胜科技有限公司 | Method for recovering lead oxide from waste lead-acid storage battery |
| 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 |
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