CN106629825A - Method for producing lead sulfate with electrochemical activity from waste lead-acid batteries - Google Patents
Method for producing lead sulfate with electrochemical activity from waste lead-acid batteries Download PDFInfo
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Abstract
The invention provides a method for producing lead sulfate with electrochemical activity from waste lead-acid batteries, belonging to the field of waste lead-acid battery recycling chemical techniques. By optimizing the waste lead-acid battery recycling process, the ammonium carbonate is used as a desulfurizer of lead sulfate, and a series of reactions are carried out to convert the lead sulfate which loses the electrochemical activity in the waste lead-acid batteries into lead sulfate with electrochemical activity; and the ammonium sulfate, ammonium acetate, ammonium sulfate solution and the like obtained by reaction can be used as reaction raw materials for the subsequent batches. The process is simple and easy to implement and forms a closed circulation; the method does not generate low-value byproducts, conforms to the clean production requirements, greatly reduces the pollution risk, lowers the production cost, and provides a new feasible scheme for recycling and sustainable production of waste lead-acid batteries.
Description
Technical field
The invention belongs to waste lead acid battery resource chemical process field, and in particular to one kind utilizes waste lead acid battery
Method of the production with electro-chemical activity lead sulfate.
Background technology
Lead sulfate is the electrode active material of lead-acid battery.Just define on two electrodes after lead-acid battery electric discharge
Lead sulfate.Research have shown that the lead sulfate of chemical synthesis can make lead-acid battery positive active material (Ke Zhang, Wei Liu,
Beibei Ma,Mohammed Adnan Mezaal,Guanghua Li,Rui Zhang and Lixu Lei,“Lead
sulfate used as the positive active material of lead acid batteries”,Journal
Of Solid StateElectrochemistry, 20,2267-2273 (2016)), it is also possible to make its negative electrode active material (Yi
Liu,Pengran Gao,Xianfu Bu,GuizhiKuang,Wei Liu,Lixu Lei,“Nanocrosses of lead
sulphate as the negative active material of lead acid batteries”,Journal of
Power Sources,263,1-6(2014)).Application for a patent for invention CN201510513062.7 and patent of invention ZL
The lead sulfate with electro-chemical activity is disclosed in 201310665446.1 and Pb is prepared with waste lead acid battery3O4And PbO2
Method, and they are used to produce the process route of new lead-acid battery.
In all these processes and other waste lead acid battery process for reclaiming, all exist using ammonium carbonate desulfurization
Step, as a result generates considerable amount of ammonium sulfate.Although ammonium sulfate can serve as chemical fertilizer, but price is very low, and sale is also compared
Difficulty, therefore should as far as possible reduce output.
The content of the invention
For the deficiencies in the prior art, the present invention is provided a kind of production using waste lead acid battery and has electro-chemical activity sulphur
The method of lead plumbate, makes the lead sulfate for losing electro-chemical activity in waste lead acid battery be converted into the sulfuric acid with electro-chemical activity
Lead, while not producing low value by-product..
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of method of the utilization waste lead acid battery production with electro-chemical activity lead sulfate, comprises the steps：
Step a：Lead sulfate is obtained from the positive powder and negative electrode powder of waste lead acid battery；
Step b：Sal volatile is added to be allowed to react in the lead sulfate obtained to step a, to the solution obtained after reaction
Separation of solid and liquid is carried out, solid carbon lead plumbate and ammonium sulfate is obtained；
Step c：Ammonium acetate solution, reaction is added to generate lead acetate and ammonium carbonate in solid carbon lead plumbate obtained in step b
Solution；
Or solid carbon lead plumbate obtained in step b is pyrolyzed, obtain lead monoxide；
Step d：Ammonium sulfate, reaction is added to obtain the sulphur with electro-chemical activity in lead acetate obtained in step c
Lead plumbate and ammonium acetate solution；
Or add ammonium sulfate, reaction to obtain the sulphur with electro-chemical activity in lead monoxide obtained in step c
Lead plumbate and ammoniacal liquor；
Or add ammonium acetate solution, reaction to obtain acetic acid lead solution and ammoniacal liquor in lead monoxide obtained in step c, so
Ammonium sulfate is added in backward gained acetic acid lead solution, reaction obtains the lead sulfate with electro-chemical activity and ammonium acetate is molten
Liquid.
Preferably, the reaction in step b, reaction temperature is room temperature～50 DEG C, and the reaction time is 0.5～3 hour.
Preferably, surfactant is added in the reaction in step d.
Preferably, in step c, solid carbon lead plumbate is carried out at boiling temperature with the reaction of ammonium acetate solution.
Preferably, in step d, the reaction of lead monoxide and ammonium sulfate, and lead monoxide is molten with ammonium acetate
The reaction of liquid is carried out at boiling temperature.
Preferably, the reaction that ammonium sulfate obtained in step b is used in step d as reaction raw materials.
Beneficial effects of the present invention are：By to waste lead acid battery process for reclaiming process optimization, making waste and old lead acid electricity
The lead sulfate for losing electro-chemical activity in pond is converted into the lead sulfate with electro-chemical activity, while not producing low value by-product
Product.Process is simple and forms the circulation of closure, meets clean manufacturing requirement, substantially reduces pollution risk, reduces life
Cost is produced, is that waste lead acid battery resource and sustainable production provide new feasible program.
Description of the drawings
Fig. 1 is by nonactive PbSO in embodiment 14Prepare the material circulation schematic diagram of electro-chemical activity lead sulfate；
Fig. 2 is by nonactive PbSO in embodiment 24Prepare the material circulation schematic diagram of electro-chemical activity lead sulfate；
Fig. 3 is by nonactive PbSO in embodiment 34Prepare the material circulation schematic diagram of electro-chemical activity lead sulfate.
Specific embodiment
When the pure lead sulphate using non-electroactive is used as raw material, if using ammonium carbonate as desulfurizing agent when, reaction
Formula is as follows：
PbSO4+(NH4)2CO3=PbCO3+(NH4)2SO4 (1)
In a heated condition, ceruse can produce lead acetate and ammonium carbonate with ammonium acetate reaction, and ammonium carbonate easily decomposes, with
The condensed water of part evaporation forms sal volatile：
PbCO3+2NH4Ac=PbAc2+(NH4)2CO3 (2)
The sal volatiles that obtain of reaction 2 can be directly used for sweetening process, that is, react 1, the acetic acid lead solution of formation and de-
The ammonium sulfate that reaction of Salmon-Saxl is produced reacts in impact reactor and obtains the lead sulfate with electro-chemical activity：
PbAc2+(NH4)2SO4=PbSO4+2NH4Ac (3)
In above process, under conditions of good control, all of material is obtained for and utilizes completely, and total effect is only
Only it is inactive PbSO4Become the PbSO of electro-chemical activity4。
When raw material sulphuric acid lead is mixed with PbO2When (to positive powder) or Pb (to negative electrode powder), then may have in the product for reacting 2
Solid residue.To positive powder, the solid is PbO2, additive can be directly used as, according to the side that CN201510513062.7 is announced
Case makes lead-acid battery positive pole.The metallic lead contained in negative electrode powder can obtain PbO by heated oxide in atmosphere, then with sulfuric acid
Reaction forms the PbSO of high electrochemical activity4。
Pb+1/2O2=PbO (4)
The lead sulfate that the lead sulfate of non-electroactive is converted into electro-chemical activity can also be used into following process route：
Step a：Using ammonium carbonate desulfurization, ceruse and ammonium sulfate (reaction 1) are obtained；
Step b：Ceruse pyrolysis is obtained into lead monoxide (reaction 5)：
PbCO3=PbO+CO2 (5)
Step c：The ammonium sulfate solution that the lead monoxide and reaction 1 that reaction 5 is obtained is obtained reacts at boiling temperature
To lead sulfate (reaction 6), ammonia and the water of generation distillate the CO formed with reaction 5 jointly2Reaction forms sal volatile.Ammonium carbonate
Can be used for desulphurization reaction 1：
PbO+(NH4)2SO4=PbSO4+2NH3+H2O (6)
In order to accelerate reaction speed, it is also possible to reaction (6) is split into two reactions, i.e. Schilling lead monoxide is anti-with ammonium acetate
Lead acetate (reaction 7) should be obtained, then the lead sulfate with electro-chemical activity is obtained using previous reaction 3：
PbO+2NH4Ac=PbAc2+2NH3+H2O (7)
When raw material is made using waste lead acid battery, waste lead acid battery positive powder (or negative electrode powder) is used into ammonium carbonate desulfurization
Afterwards, to positive powder, that what is obtained is PbCO3And PbO2Mixture.By the mixture pyrolysis, that is, form PbO and PbO2/Pb3O4It is mixed
Compound, while discharging CO2(reaction 5 and reaction 8)：
3PbO2=Pb3O4+O2 (8)
Then, by resulting PbO and PbO2/Pb3O4Mixture reacts with ammonium sulfate or ammonium acetate, finally by above-mentioned step
Suddenly the lead sulfate and PbO of electro-chemical activity are obtained2/Pb3O4Mixture, the mixture be used directly for produce lead-acid battery
Positive plate.
For the negative electrode powder of waste lead acid battery, the product after desulfurization is the mixture of ceruse and metallic lead.By it
Roasting in atmosphere, that is, obtain PbO.Afterwards the lead sulfate with electro-chemical activity can be obtained according to above-mentioned reaction 6～8.
In sum, the PbSO of high electrochemical activity is prepared by waste lead acid battery positive powder or negative electrode powder4Can have three
Bar route：
PbSO4→PbCO3→PbAc2→PbSO4
PbSO4→PbCO3→PbO→PbSO4
PbSO4→PbCO3→PbO→PbAc2→PbSO4
First route by react 1～3 totally 3 steps reaction constitute；Article 2 route is constituted by reacting 1,5 and 6；It is last a kind of
It is to be made up of reaction 1,5,7 and 3.
Described lead sulfate is formed in reaction 3 and 6, it is possible to use pattern controlling agent come control the size of lead sulfate crystal grain with
Exposure crystal face classification, reaches the purpose of control lead sulfate electro-chemical activity.Described pattern controlling agent is some surfactants,
As sulfate ion, organic sulfate, organic sulfonate, containing coordinating oxygen atoms functional group (such as carboxylic acid, alcohol, ether, ketone)
Surfactant etc..
Above-mentioned ammonium carbonate can be replaced by the carbonate of volatile organic amines, and ammonium acetate can also be by volatile organic amines
Acetate replaces.
Embodiment 1
Step (1)：Lead-acid battery is gently disassembled, positive plate and negative plate is obtained, then respectively metal grid with
Electrode powder is made available separately positive pole grid alloy, negative pole grid alloy, positive powder and negative electrode powder.Positive powder and negative electrode powder are analyzed respectively
The content of middle lead sulfate.
Step (2)：Resulting positive powder (or negative electrode powder) is put into a stirred reactor, then by wherein PbSO4
Content add enough sal volatile, stirring to react it.Between room temperature～50 DEG C, the reaction time exists reaction temperature
Between 0.5～3 hour.(to positive powder, solid is PbO for filtration or centrifugation solid2And PbCO3Mixture, negative electrode powder is then
It is Pb and PbCO3Mixture) and solution (ammonium sulfate may contain a small amount of ammonium carbonate), washing removes solid absorption
Soluble-salt.
Step (3)：Ammonium acetate solution, heating is added to make PbCO in the solid obtained by step (2)3React, it is raw
Into ammonium carbonate be collected in another container by distillation.Solid filtration/the centrifugation that can not be reacted, its main component is
PbO2(to positive powder) or Pb (to negative electrode powder), it is scrubbed after be respectively used to battery production；Filtrate is the solution of lead acetate.Carbonic acid
Ammonium salt solution can be directly used for step (2) reaction.
Step (4)：The ammonium sulfate that the lead acetate and step (2) that step (3) reaction is obtained is obtained reacts in impinging stream
Reaction in device obtains the ultra-fine PbSO with electro-chemical activity4, while what is obtained has ammonium acetate solution, the latter is used directly for
The reaction of step (3) and recycled.
In above-mentioned steps, described ammonium carbonate can be replaced by the carbonate of volatile organic amines, and ammonium acetate can also be by
The acetate of volatile organic amines replaces.
In step (4), a small amount of pattern controlling agent can be added in acetic acid lead solution to control the big of lead sulfate crystal grain
Little and exposure crystal face classification, reaches control PbSO4The purpose of electro-chemical activity.Described pattern controlling agent is some surface-actives
Agent, such as sulfate ion, organic sulfate, organic sulfonate, containing coordinating oxygen atoms functional group (such as carboxylic acid, alcohol, ether, ketone)
Surfactant etc..
Accompanying drawing 1 is by nonactive PbSO in embodiment 14The material circulation schematic diagram of electro-chemical activity lead sulfate is prepared, can
To find out that all of material is obtained for recycling, process can be without any discharge.
Embodiment 2
Step (1)：Lead-acid battery is gently disassembled, positive plate and negative plate is obtained, then respectively metal grid with
Electrode powder is made available separately positive pole grid alloy, negative pole grid alloy, positive powder and negative electrode powder.Positive powder and negative electrode powder are analyzed respectively
The content of middle lead sulfate.
Step (2)：Resulting positive powder (or negative electrode powder) is put into a stirred reactor, then by wherein PbSO4
Content add enough sal volatile, stirring to react it.Between room temperature～50 DEG C, the reaction time exists reaction temperature
Between 0.5～3 hour.(to positive powder, solid is PbO for filtration or centrifugation solid2And PbCO3Mixture, negative electrode powder is then
It is Pb and PbCO3Mixture) and solution (ammonium sulfate may contain a small amount of ammonium carbonate), washing removes solid absorption
Soluble-salt.
Step (3)：The pyrolysis obtained by step (2) are made under the conditions of 350～650 DEG C, PbO and PbO is obtained2(or
Pb3O4) mixture (to positive powder), or PbO (to negative electrode powder), while the CO for producing2It is passed through the ammonia that next step reaction is produced
In water, sal volatile is obtained.
Step (4)：The ammonium sulfate that the PbO and step (2) that step (3) reaction is obtained is obtained is in the case of ebuillition of heated
Reaction obtains the ultra-fine PbSO with electro-chemical activity4, while the ammonia for being formed is with partial solvent, and jointly evaporation obtains ammoniacal liquor, ammonia
The CO that water is obtained with step (3) reaction2Reaction obtains ammonium carbonate, and it is used directly for the reaction of step (2) and is circulated
Use.
In above-mentioned steps, described ammonium carbonate can be replaced by the carbonate of volatile organic amines, and ammonium acetate can also be by
The acetate of volatile organic amines replaces.
In step (4), a small amount of pattern controlling agent can be added in acetic acid lead solution to control the big of lead sulfate crystal grain
Little and exposure crystal face classification, reaches control PbSO4The purpose of electro-chemical activity.Described pattern controlling agent is some surface-actives
Agent, such as sulfate ion, organic sulfate, organic sulfonate, containing coordinating oxygen atoms functional group (such as carboxylic acid, alcohol, ether, ketone)
Surfactant etc..
Accompanying drawing 2 is by nonactive PbSO in embodiment 24The material circulation schematic diagram of electro-chemical activity lead sulfate is prepared, can
To find out that all of material is obtained for recycling, process can be without any discharge.
Embodiment 3
Step (1)：Lead-acid battery is gently disassembled, positive plate and negative plate is obtained, then respectively metal grid with
Electrode powder is made available separately positive pole grid alloy, negative pole grid alloy, positive powder and negative electrode powder.Positive powder and negative electrode powder are analyzed respectively
The content of middle lead sulfate.
Step (2)：Resulting positive powder (or negative electrode powder) is put into a stirred reactor, then by wherein PbSO4
Content add enough sal volatile, stirring to react it.Between room temperature～50 DEG C, the reaction time exists reaction temperature
Between 0.5～3 hour.(to positive powder, solid is PbO for filtration or centrifugation solid2And PbCO3Mixture, negative electrode powder is then
It is Pb and PbCO3Mixture) and solution (ammonium sulfate may contain a small amount of ammonium carbonate), washing removes solid absorption
Soluble-salt.
Step (3)：Pyrolysis obtained by making step 2 under the conditions of 350～650 DEG C, obtain PbO and PbO2(or
Pb3O4) mixture (to positive powder), or PbO (to negative electrode powder), while the CO for producing2It is passed through the ammonia that next step reaction is produced
In water, sal volatile is obtained.
Step (4)：The PbO and ammonium acetate solution that step (3) reaction is obtained reacts in the case of ebuillition of heated and obtains PbAc2
Solution, while the ammonia for being formed is with partial solvent, and jointly evaporation obtains ammoniacal liquor, the CO that ammoniacal liquor is obtained with step (3) reaction2Reaction
Ammonium carbonate is obtained, it is used directly for the reaction of step (2) and is recycled.
Step (5)：The PbAc that step (4) reaction is obtained2The ammonium sulfate that solution is obtained with step (2) is anti-in impinging stream
Reaction in device is answered to obtain the ultra-fine PbSO with electro-chemical activity4, while what is obtained has ammonium acetate solution, the latter can directly use
Recycled in the reaction of step (4).
In above-mentioned steps, described ammonium carbonate can be replaced by the carbonate of volatile organic amines, and ammonium acetate can also be by
The acetate of volatile organic amines replaces.
In step (5), a small amount of pattern controlling agent can be added in acetic acid lead solution to control the big of lead sulfate crystal grain
Little and exposure crystal face classification, reaches control PbSO4The purpose of electro-chemical activity.Described pattern controlling agent is some surface-actives
Agent, such as sulfate ion, organic sulfate, organic sulfonate, containing coordinating oxygen atoms functional group (such as carboxylic acid, alcohol, ether, ketone)
Surfactant etc..
Accompanying drawing 3 is by nonactive PbSO in embodiment 34The material circulation schematic diagram of electro-chemical activity lead sulfate is prepared, can
To find out that all of material is obtained for recycling, process can be without any discharge.
Claims (6)
1. a kind of method that utilization waste lead acid battery production has electro-chemical activity lead sulfate, it is characterised in that including as follows
Step：
Step a：Lead sulfate is obtained from the positive powder and negative electrode powder of waste lead acid battery；
Step b：Sal volatile is added to be allowed to react in the lead sulfate obtained to step a, the solution to obtaining after reaction is carried out
Separation of solid and liquid, obtains solid carbon lead plumbate and ammonium sulfate；
Step c：Ammonium acetate solution, reaction is added to generate lead acetate and sal volatile in solid carbon lead plumbate obtained in step b；
Or solid carbon lead plumbate obtained in step b is pyrolyzed, obtain lead monoxide；
Step d：Ammonium sulfate, reaction is added to obtain the lead sulfate with electro-chemical activity in lead acetate obtained in step c
And ammonium acetate solution；
Or add ammonium sulfate, reaction to obtain the lead sulfate with electro-chemical activity in lead monoxide obtained in step c
And ammoniacal liquor；
Or add ammonium acetate solution, reaction to obtain acetic acid lead solution and ammoniacal liquor, Ran Houxiang in lead monoxide obtained in step c
Ammonium sulfate, reaction is added to obtain the lead sulfate with electro-chemical activity and ammonium acetate solution in gained acetic acid lead solution.
2. the method that a kind of utilization waste lead acid battery production according to claim 1 has electro-chemical activity lead sulfate,
Characterized in that, the reaction in step b, reaction temperature is room temperature～50 DEG C, and the reaction time is 0.5～3 hour.
3. the method that a kind of utilization waste lead acid battery production according to claim 1 has electro-chemical activity lead sulfate,
Characterized in that, adding surfactant in the reaction in step d.
4. the method that a kind of utilization waste lead acid battery production according to claim 1 has electro-chemical activity lead sulfate,
Characterized in that, in step c, solid carbon lead plumbate is carried out at boiling temperature with the reaction of ammonium acetate solution.
5. the method that a kind of utilization waste lead acid battery production according to claim 1 has electro-chemical activity lead sulfate,
Characterized in that, in step d, the reaction of lead monoxide and ammonium sulfate, and lead monoxide and ammonium acetate solution
Reaction is carried out at boiling temperature.
6. the method that a kind of utilization waste lead acid battery production according to claim 1 has electro-chemical activity lead sulfate,
Characterized in that, the reaction that ammonium sulfate obtained in step b is used in step d as reaction raw materials.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108767333A (en) * | 2018-05-28 | 2018-11-06 | 东南大学 | A kind of circulation producing method of lead-acid battery |
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| CN105206800A (en) * | 2015-08-20 | 2015-12-30 | 东南大学 | Lead-acid cell positive electrode with lead sulfate as active material and method for preparing lead-acid cell through positive electrode |
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| CN102009996A (en) * | 2010-11-05 | 2011-04-13 | 江苏华富储能新技术发展有限公司 | Method for preparing tribasic lead sulfate by using waste acid spraying lead paste |
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