CN102747227A - Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries - Google Patents
Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries Download PDFInfo
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- CN102747227A CN102747227A CN2012102012729A CN201210201272A CN102747227A CN 102747227 A CN102747227 A CN 102747227A CN 2012102012729 A CN2012102012729 A CN 2012102012729A CN 201210201272 A CN201210201272 A CN 201210201272A CN 102747227 A CN102747227 A CN 102747227A
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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
Abstract
The invention discloses a method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries. According to the invention, the superfine powder disclosed herein can be directly used for producing new lead acid batteries by the prior art, lead acid batteries can be recycled, and the method is a production technology which accords with circular economy principles. The method can eliminate the pollution generated by the waste lead acid batteries at the source, has the characteristics of low production cost and high economic benefit, and is suitable for existing lead acid battery production enterprises to let practical and affordable lead acid batteries be used with persistence and reassurance.
Description
Technical field
The present invention relates to a kind of cyclic production technical field of lead-acid cell, be specifically related to have the method for the corresponding lead-acid cell electrode of high electrochemical activity with ultra-fine yellow lead oxide powder with waste lead acid battery positive pole and negative active core-shell material preparation.
Background technology
Lead-acid cell is a kind of rechargeable cell, has low price, safeguards demand simple, that can satisfy multiple user, in uninterruptible power supply, electromobile, automobile starting power supply, electric bicycle, has obtained using widely.Contain a large amount of lead in the lead-acid cell, also contain the sulfuric acid of some severe corrosives environment and human body harmful, arrive work-ing life after, as not handling well, then can produce serious environmental and pollute.
In order to reduce lead-acid cell resource utilization process required energy consumption and material consumption, thereby reduce the environmental influence that the resource utilization process produces, we carried out the cyclic production research of lead-acid cell from 2009.Its core concept is that the resource utilization process is not a target with the metallic element that extracts wherein; But various electrode materialss in the old and useless battery are come out with physical method for separation; Then with its positive active material and negative electrode active material through minimum chemical treatment, obtain can directly being used to produce new secondary battery electrode material respectively.The benefit of doing like this mainly contains, and chemical treatment is farthest reduced, and has therefore farthest reduced the environmental pollution risk.Secondly, the energy consumption material consumption reduces greatly, and remarkable in economical benefits increases.The 3rd, can realize the cyclic production of secondary cell.
We disclose in granted patent ZL 200910024467.9 and have used electrochemical method to form Pb and PbO to the material electrolysis in positive plate and the negative plate
2Method; In patented claim 201110172238.9, disclose the PbO in the positive plate
2And PbSO
4Be converted into PbO and Pb through the medium and low temperature chemical reduction, with Pb in the negative plate and PbSO
4Be converted into the method for PbO and Pb through the medium and low temperature atmospheric oxidation.This patent discloses a kind of novel method for preparing the ultra-fine yellow lead oxide of nano-micro level from waste lead acid battery negative or positive electrode active material.
In document, existing people reports the method for using waste lead acid battery active substance or its model substance such as lead sulfate, plumbic oxide to prepare ultra-fine lead oxide, and the method for using other pure lead compound to prepare ultra-fine lead oxide is also arranged.But, existing research does not separate positive electrode active materials and negative active core-shell material, does not manage controlled oxidation plumbous structure and pattern yet.For example; Australia Wollongong university has reported use solubility lead salt during 2001 ~ 2004 years; The a series of researchs that prepare the plumbous oxide of nano-micro level like lead nitrate; Wherein some data explains that also performance is superior to performance (Journal of Alloys and Compounds 2001,327 (1-2): the 141-145 that the leaded plumbous oxide of preparation is gone up in industry; Journal of Applied Electrochemistry 2004,34 (11): 1127-1133).Univ cambridge uk once reported a kind of technology of utilizing the Hydrocerol A wet method to produce ultra-fine lead oxide powder (Hydrometallurgy, 2009,95 (1-2): 53-60 in 2009; 95 (1-2): 82-86).This technology uses Hydrocerol A and Trisodium Citrate to handle lead sulfate, plumbous oxide and plumbic oxide in the waste and old electrode materials, makes them all change into lead citrate, passes through low-temperature bake (300～500 ° of C) then and obtains product.Afterwards; The wide study group of poplar man of the Central China University of Science and Technology has carried out further research to this technology; Also reported the corresponding research of using the waste lead acid battery active material (Hydrometallurgy, 2012.doi:10.1016/j.hydromet.2012.01.006).A subject matter of Hydrocerol A technology as above is, need add ydrogen peroxide 50 as reductive agent when handling plumbic oxide, and the Hydrocerol A of use and Trisodium Citrate are all somewhat expensive.So Technological Economy property existing problems.
Summary of the invention
The purpose of this invention is to provide a kind of novel method for preparing the nano-micro level yellow lead oxide powder (or claiming ultra-fine PbO powder) of high electrochemical activity from waste lead acid battery negative or positive electrode active material.
The technical scheme that the present invention adopts is: a kind of electrode active material with waste lead acid battery prepares the method for ultra-fine yellow lead oxide, and this method comprises the steps:
1) waste lead acid battery is cut from top, separate to obtain positive plate and negative plate, electrolytic solution sulfuric acid, plastic casing;
2) handle positive plate and negative plate respectively through current flushing, ultrasonic or mechanical impacting, obtain positive powder (positive active material powder), negative pole powder (negative electrode active material powder), anodal LY grid, negative electrode lead alloy grid;
3) said positive powder is mixed in a closed reaction kettle with a kind of reaction medium and a kind of reductive agent, stir down being no more than that reaction is no more than 24 hours under 300 ° of C conditions;
4) aqueous solution of adding pattern and/or constitution controller, carbonate or oxyhydroxide in the suspension liquid that step 3) obtains; Under the temperature that is not higher than 200 ° of C, continue stirring reaction and be no more than 24 hours; Filter then, remove the vitriol of solid product absorption again with water washing;
5) step 4) gained solid is heated at 200 ~ 500 ° of C behind preheating and drying, the lead-acid cell positive pole that promptly obtains having good electrochemical activity is with ultra-fine yellow lead oxide powder;
6) said negative pole powder is mixed in reaction kettle with a kind of reaction medium, a kind of morphology control agent and/or a kind of constitution controller; Stir under the temperature that is not higher than 200 ° of C, to react down and be no more than 24 hours; The suspension liquid that obtains is filtered, remove the vitriol of solid product with water washing;
7) solid that step 6) is obtained heats under the temperature that in air atmosphere, is not higher than 500 ° of C behind the preheating and drying; Perhaps; Also can the solid that step 6) obtains be dissolved in nitric acid or hot hydrochloric acid; Use the aqueous solution of alkali metal hydroxide or ammonia to handle then; Then under the condition that morphology control agent and/or constitution controller exist in an encloses container stirring reaction, its temperature of reaction is not higher than 300 ° of C, the time is no more than 24 hours; The lead-acid cell negative pole that can obtain having good electrochemical activity is with ultra-fine yellow lead oxide powder.
As preferably, the reaction medium in the said step 3) is the aqueous solution of pure water or acid and alkali substance.Said acid and alkali substance is sulfuric acid, hydrochloric acid, soluble carbon hydrochlorate, solubility oxyhydroxide or ammonia etc.Said reductive agent is can be with PbO
2Reductive material, especially sulphite, nitrite, organic alcohols, aldehydes and acids etc.
As preferably, the reaction medium in the said step 6) is to contain any soluble carbon hydrochlorate, particularly its sodium salt and ammonium salt; Or the aqueous solution of any solubility oxyhydroxide, particularly sodium hydroxide and ammoniacal liquor.
As preferably, described morphology control agent and constitution controller are any organism or inorganicss with this kind effect, and their guarantee that the yellow lead oxide of gained has definite pattern, structure and particle size.
Beneficial effect: the inventive method will be disassembled negative or positive electrode active material admixture that process obtains forms the nano-micro level with specific morphology and ad hoc structure through less chemical process PbO ultra-fine micropowder through a series of; This powder can be directly by the existing new lead-acid cell of explained hereafter; It is a kind of production technology that meets the recycling economy principle; This technology can reduce the Pollution risk that waste lead acid battery resource utilization process produces greatly, and it is low to have a production cost, the characteristics that economic benefit is high; Be suitable for existing lead-acid cell manufacturing enterprise and use, make the inexpensive lead-acid cell can be by lasting relieved use.
Embodiment
Below in conjunction with embodiment the present invention is described further:
Positive powder and the negative pole powder that is applicable to the isolating waste lead acid battery of gentle mechanical means of the present invention.Concrete steps are:
1), separates obtaining positive plate and negative plate, electrolytic solution sulfuric acid, plastic casing with waste lead acid battery gentle cutting from top.Handle positive plate and negative plate respectively through high velocity jet flushing, ultrasonic or mechanical impacting, obtain positive powder, negative pole powder, anodal LY grid, negative electrode lead alloy grid.
2) with the negative pole powder that obtains under the condition that pattern and constitution controller exist with carbonate or oxyhydroxide desulfurization; Then under 200 ° of C ~ 500 ° C in air heating make its partially oxidation and thermolysis, produce the negative pole powder of nano-micro level with good electrochemical activity.The contingent chemical reaction of this process has (with carbonate for sweetening agent time be example):
Sweetening process: PbSO
4+ CO
3 2-=PbCO
3+ SO
4 2-
Thermolysis/oxidising process: PbCO
3=PbO+CO
2
2Pb+O
2=2PbO
3) positive powder that obtains is reduced with the organic or inorganic reductive agent at 100 ° of C ~ 300 ° C under the condition of carbonate or oxyhydroxide, pattern and constitution controller existence.The solid matter that obtains after sulfate ion is removed in washing then, changes process furnace through desulfurization over to.In process furnace, this solid matter is dry at first at a lower temperature, is warming up to then in air, to heat under 200 ° of C ~ 500 ° C to make its thermolysis, produces the positive powder of the nano-micro level with good electrochemical activity.The contingent chemical reaction of this process has (being that reductive agent, sulfuric acid are that medium, carbonate are example during for sweetening agent with methyl alcohol):
Reduction process: 3PbO
2+ CH
3OH+3H
2SO
4=3PbSO
4+ CO
2+ 5H
2O
Sweetening process: PbSO
4+ CO
3 2-=PbCO
3+ SO
4 2-
Thermal decomposition process: PbCO
3=PbO+CO
2
Described carbonate can be any soluble carbon hydrochlorate, particularly its sodium salt and ammonium salt; Oxyhydroxide can be any solubility oxyhydroxide, particularly sodium hydroxide and ammoniacal liquor.
Described reductive agent can be any organic reducing substances, particularly methyl alcohol, formaldehyde and formic acid.
Described crystallization and morphology control agent can be any auxiliary agents that helps to form the plumbous oxide of specific crystal formation and pattern.
1. the treatment process of negative pole powder
Embodiment 1: use the sodium hydroxide desulfurization, calcination in air then
The sodium hydroxide solution that will in the concentration that contains little sodium chloride be 0.5 ~ 3.0mol/L from the negative pole powder that waste lead acid battery obtains is handled under ~ 100 ° of C conditions, makes PbSO in the negative pole powder
4All change into fine Pb (OH)
2
The negative pole powder places in the crucible after getting desulfurization, and ° C heats 1 ~ 4h 200 ° of C ~ 500 in the electric furnace then, can obtain the PbO micro mist that needs.
Embodiment 2: use the volatile salt desulfurization, calcination in air then
The sal volatile that will in the use concentration that contains Vinylpyrrolidone polymer be 0.5 ~ 3.0mol/L from the negative pole powder that waste lead acid battery obtains is handled under ~ 50 ° of C conditions, makes PbSO in the negative pole powder
4All change into fine PbCO
3
The negative pole powder places in the crucible after getting desulfurization, and 200 ° of C ~ 500 ° C heating 1 ~ 4h in electric furnace can obtain the PbO micro mist that needs then.
Embodiment 3: use the volatile salt desulfurization, be dissolved in hydrochloric acid then, precipitate with sodium hydroxide
The sal volatile that will in concentration be 0.5 ~ 3.0mol/L from the negative pole powder that waste lead acid battery obtains is handled under ~ 50 ° of C conditions, makes PbSO in the negative pole powder
4The PbCO that all changes into
3All sulfate radicals are removed in washing.
In a hydrothermal reaction kettle with the PbCO that obtains
3About 80 ° of C, be dissolved in hydrochloric acid, add ammoniacal liquor to solution then.The temperature of solution in the reaction kettle is increased to 180 ° of C, is incubated 0.5 ~ 4 hour, can obtain the PbO micro mist that needs.
2. the treatment process of positive powder
Embodiment 4: reduce in sulfuric acid medium with methyl alcohol, use the volatile salt desulfurization then
At first, will add from the positive powder that waste lead acid battery obtains and contain Vinylpyrrolidone polymer, excessive methanol and the vitriolic aqueous solution, sealed reactor, reaction is no more than 24 hours under 120 ° of C ~ 180 ° C stirs.Cooling reactor makes pressure be reduced to normal pressure, removes by filter liquid.Adding use concentration then is that 0.5 ~ 3.0mol/L carbonate (ammonium salt or sodium salt) solution is done the desulfurization processing, makes wherein PbSO
4All change into PbCO
3All vitriol is removed in washing.
The solid that obtains moves into crucible, and 200 ° of C ~ 500 ° C calcine 0.5 ~ 4h down and can obtain the ultra-fine lead oxide powder in retort furnace.
Embodiment 5: with containing the reduction of vitriolic methyl alcohol, use the volatile salt desulfurization then
At first, will add excessive methyl alcohol, add the sulfuric acid of capacity from the positive powder that waste lead acid battery obtains, sealed reactor, reaction is no more than 24 hours under 120 ° of C ~ 300 ° C stirs.Cooling reactor makes pressure be reduced to normal pressure, removes by filter all liquid.Adding concentration then is that 0.5 ~ 3.0mol/L carbonate (ammonium salt or sodium salt) solution is done the desulfurization processing, makes PbSO
4All change into PbCO
3All vitriol is removed in washing.
The solid that obtains moves into crucible, and 200 ° of C ~ 500 ° C calcine 0.5 ~ 4h down and can obtain the ultra-fine lead oxide powder in retort furnace.
Embodiment 6: reduce in alkaline medium with S-WAT, then thermolysis
At first, will add from the positive powder that waste lead acid battery obtains the aqueous solution of the excessive sodium hydrate that contains little sodium chloride, capacity S-WAT, sealed reactor, reaction is no more than 24 hours under 120 ° of C ~ 300 ° C stirs.Cooling reactor makes pressure be reduced to normal pressure, removes by filter liquid.Remove all vitriol with the water purification washing then.
The solid that obtains moves into crucible, and 200 ° of C ~ 500 ° C calcine 1 ~ 4h down and can obtain the ultra-fine lead oxide powder in retort furnace.
Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.The all available prior art of each integral part not clear and definite in the present embodiment realizes.
Claims (6)
1. the electrode active material with waste lead acid battery prepares the method for ultra-fine yellow lead oxide, and it is characterized in that: this method comprises the steps:
1) waste lead acid battery is cut from top, separate to obtain positive plate and negative plate, electrolytic solution sulfuric acid, plastic casing;
2) handle positive plate and negative plate respectively through current flushing, ultrasonic or mechanical impacting, obtain positive powder, negative pole powder, anodal LY grid, negative electrode lead alloy grid;
3) said positive powder is mixed in a closed reaction kettle with a kind of reaction medium and a kind of reductive agent, stir down being no more than that reaction is no more than 24 hours under 300 ° of C conditions;
4) aqueous solution of adding pattern and/or constitution controller, carbonate or oxyhydroxide in the suspension liquid that step 3) obtains; Under the temperature that is not higher than 200 ° of C, continue stirring reaction and be no more than 24 hours; Filter then, remove the vitriol of solid product absorption again with water washing;
5) step 4) gained solid is heated at 200 ~ 500 ° of C behind preheating and drying, the lead-acid cell positive pole that promptly obtains having good electrochemical activity is with ultra-fine yellow lead oxide powder;
6) said negative pole powder is mixed in reaction kettle with a kind of reaction medium, a kind of morphology control agent and/or a kind of constitution controller; Stir under the temperature that is not higher than 200 ° of C, to react down and be no more than 24 hours; The suspension liquid that obtains is filtered, remove the vitriol of solid product with water washing;
7) solid that step 6) is obtained heats under the temperature that in air atmosphere, is not higher than 500 ° of C behind the preheating and drying; Perhaps; Also can the solid that step 6) obtains be dissolved in nitric acid or hot hydrochloric acid; Use the aqueous solution of alkali metal hydroxide or ammonia to handle then; Then under the condition that morphology control agent and/or constitution controller exist in an encloses container stirring reaction, its temperature of reaction is not higher than 300 ° of C, the time is no more than 24 hours; The lead-acid cell negative pole that can obtain having good electrochemical activity is with ultra-fine yellow lead oxide powder.
2. the electrode active material with waste lead acid battery according to claim 1 prepares the method for ultra-fine yellow lead oxide, it is characterized in that: the reaction medium in the said step 3) is the aqueous solution of pure water or acid and alkali substance.
3. the electrode active material with waste lead acid battery according to claim 2 prepares the method for ultra-fine yellow lead oxide, it is characterized in that: said acid and alkali substance is sulfuric acid, hydrochloric acid, soluble carbon hydrochlorate, solubility oxyhydroxide or ammonia.
4. the electrode active material with waste lead acid battery according to claim 1 prepares the method for ultra-fine yellow lead oxide, it is characterized in that: the reductive agent in the said step 3) is sulphite, nitrite, organic alcohols, aldehydes and acids.
5. the electrode active material with waste lead acid battery according to claim 1 prepares the method for ultra-fine yellow lead oxide; It is characterized in that: the reaction medium in the said step 6) is to contain any soluble carbon hydrochlorate, or the aqueous solution of any solubility oxyhydroxide.
6. the electrode active material with waste lead acid battery according to claim 1 prepares the method for ultra-fine yellow lead oxide, it is characterized in that: described morphology control agent and constitution controller are organism or the inorganicss that the yellow lead oxide of any assurance gained has definite pattern, structure and particle size.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104393364A (en) * | 2014-11-13 | 2015-03-04 | 张家港智电芳华蓄电研究所有限公司 | Method for preparing PbO from waste lead-acid battery by using direct wet method |
| CN104619645A (en) * | 2014-02-21 | 2015-05-13 | 超威电源有限公司 | Method for recycling lead oxide-containing waste |
| CN104953192A (en) * | 2015-06-12 | 2015-09-30 | 河北师范大学 | Preparation method of Pb-containing lead-acid battery negative electrode additive |
| CN105441686A (en) * | 2016-01-06 | 2016-03-30 | 湘潭大学 | Reducing method for lead dioxide in waste lead plaster |
| CN106587140A (en) * | 2016-11-03 | 2017-04-26 | 华东师范大学 | Method for preparing nano lead oxide powder by using waste lead-containing soldering tins |
| CN106711531A (en) * | 2016-12-21 | 2017-05-24 | 东南大学 | Method for preparing basic lead sulfates from PbO and producing lead-acid battery from basic lead sulfates |
| 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 |
| US9828654B2 (en) | 2014-02-21 | 2017-11-28 | Chilwee Power Co. Ltd & Beijing University Of Chemical Technology | Method for directly recovering lead oxide used for a lead-acid battery cathode from waste lead paste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN103014347B (en) * | 2012-12-12 | 2014-12-03 | 北京化工大学 | Method for recycling waste lead-acid cells to directly produce lead oxide |
| CN104619645A (en) * | 2014-02-21 | 2015-05-13 | 超威电源有限公司 | Method for recycling lead oxide-containing waste |
| US9828654B2 (en) | 2014-02-21 | 2017-11-28 | Chilwee Power Co. Ltd & Beijing University Of Chemical Technology | Method for directly recovering lead oxide used for a lead-acid battery cathode from waste lead paste |
| CN104393364A (en) * | 2014-11-13 | 2015-03-04 | 张家港智电芳华蓄电研究所有限公司 | Method for preparing PbO from waste lead-acid battery by using direct wet method |
| CN104953192A (en) * | 2015-06-12 | 2015-09-30 | 河北师范大学 | Preparation method of Pb-containing lead-acid battery negative electrode additive |
| CN105441686A (en) * | 2016-01-06 | 2016-03-30 | 湘潭大学 | Reducing method for lead dioxide in waste lead plaster |
| CN106587140A (en) * | 2016-11-03 | 2017-04-26 | 华东师范大学 | Method for preparing nano lead oxide powder by using waste lead-containing soldering tins |
| CN106587140B (en) * | 2016-11-03 | 2017-11-24 | 华东师范大学 | A kind of method for preparing nano oxidized lead powder using waste and old leaded scolding tin |
| CN106711531A (en) * | 2016-12-21 | 2017-05-24 | 东南大学 | Method for preparing basic lead sulfates from PbO and producing lead-acid battery from basic lead sulfates |
| 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 |
| CN107164636B (en) * | 2017-05-27 | 2019-03-26 | 湘潭大学 | A kind of method that high-purity lead oxide is recycled in waste lead acid battery processing |
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|---|---|
| CN102747227B (en) | 2014-02-05 |
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