CN100583548C - Method of recycling waste lead acid battery lead by electrolyzing with acid-wet method - Google Patents
Method of recycling waste lead acid battery lead by electrolyzing with acid-wet method Download PDFInfo
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention relates to a method for recovering lead, in particular to a method for electrolyzing and recovering lead in a waste lead-acid accumulator by using an acid-mode wet method. The method comprises the following steps that: firstly, the waste lead-acid accumulator is treated with a pouring acid, a shell of the waste lead-acid accumulator is peeled off and separated to obtain a dilute sulphuric acid, waste plastic and a battery unit or a battery pack; secondly, the battery unit or the battery pack separated from the waste battery is positioned in an electrolytic cell; the lead is reduced by adopting a duplicate power-supply and multi-module electrolysis process; and a lead plate is formed on a slab lattice for recovering the lead. The lead recovery method eliminates the pollution of exhaust gas and waste slag containing the lead and SO2 in the prior pyrogenic lead-smelting process and overcomes the disadvantages of complex flow and low lead recovery coefficient in the prior wet lead smelting process.
Description
Technical field
The present invention relates to plumbous recovery method, relate in particular to and use acid wet method electrolysis to reclaim method plumbous in the waste and old lead acid accumulator, the lead electrolysis in acidic electrolysis bath that is about to the various valence states in the waste lead acid battery is converted into the method for the metallic lead that can directly utilize.It is applicable to that the cleaning of the lead of lead-acid battery reclaims and regeneration, and a kind of efficient wet that is suitable for suitability for industrialized production refines plumbous technology.
Background technology
Along with rapid development of science and technology, the high speed development of Domestic Automotive Industry particularly, automobile and electric motor car become people's indispensable vehicles of living already.Lead-acid battery is as automobile and the indispensable electric energy energy storage device of electric motor car, and its consumption figure and learies are along with the consumption of automobile increases rapidly.Consumption figure plumbous in the lead-acid battery of China in 2002 reaches 64.5 ten thousand tons, has increased more than 150% than 2000.2002-2006, battery of electric bicycle reach 20% rapid growth every year as a unexpected rival of lead-acid battery industry.2005, the recoverable amount of China's electric bicycle reached 8,000 ten thousand, and the lead-acid battery of scrapping its every year reaches ten thousand tons of 28-31, and wherein plumbous consumption figure reaches 190,000 tons.
At present reviver technology mainly contains two kinds of pyrogenic process and wet methods.The traditional pyrometallurgical smelting process such as reverberatory furnace, blast furnace and furnace cupola of the main at present employing of a lot of reviver enterprises produce the high temperature up to 1000-1200 ℃ in the smelting process, produce plumbous steam or waste gas such as lead fume dirt and sulfur dioxide simultaneously.This reviver technology that falls behind has relatively caused serious environmental to pollute and the wasting of resources, has improved simultaneously and has reclaimed plumbous cost.
According to investigations, the outstanding problem of China's waste lead accumulator regenerative lead factory existence is:
(1) lead recovery is low.At present, China's lead recovery is generally 80%-85%, and the rate of recovery far below external 95% has caused national every year nearly more than 20,000 tons of lead to be lost in smelting process.
(2) a large amount of lead dust, plumbous steams pollute.Owing to use pyrometallurgical smelting of lead, in using the reverberatory furnace smelting process, but 1 ton of lead-acid accumulator output of about every processing flue dust 70-80 kilogram contains have an appointment 60% lead, antimony, arsenic in these flue dust.Because most enterprises do not take pre-desulfurization measure substantially, also contain a large amount of sulfur dioxide in the flue gas during smelting of generation, these waste gas directly are discharged in the atmosphere without any processing of gathering dust.Next is flue dust suspended matter and heavy metal ion that smelting wastewater contains natural subsidence in the air, can cause the pollution to underground water and resident's drinking water.
(3) refine plumbous residue contamination.The nearly 20-30% of the slag rate of reverberatory furnace contains mineral matters such as the antimony of arsenic, 1-3.5% of lead, the 0.5-1% of 8-10% and silicon dioxide in the slag.Nuisance in these waste residues is deposited in the soil, and by food chain, progressively enrichment in crops causes the harm to human body.
Pyrometallurgical smelting of lead because wet method refining splicer skill is carried out, can not produce lead dust, plumbous steam, lead skim and sulfur dioxide pollution under moist environment relatively, helps the recovery and reuse of lead resource.More domestic and international in recent years enterprises and research unit take up to study the method for the lead in the wet method electrolytic recovery waste lead acid battery.For example, the Chinese patent publication number is the application for a patent for invention of CN 1808761 A, a kind of method plumbous in the wet method acid electroreduction scrap battery of using is disclosed, the plumbous mud that this method must will be taken out from refuse battery is pulverized levigate in pulverizer, adding lead monoxide powder and water mix makes slurry, be coated in then on the corrosion resistant plate, after the drying, this scribbled corrosion resistant plate electroreduction lead in electrolysis tank of plumbous mud.The complex disposal process of scrap lead before this method electrolysis, technological process is long, and the equipment investment expense is big, has not only increased the refinement cost, and brings very big corrosion to equipment.
Summary of the invention
The objective of the invention is to, refine the existing problem and shortage of plumbous technology at prior art pyrogenic process and wet method, provide a kind of novel simply directly will be from old and useless battery isolated battery unit or battery pack place electrolysis tank, adopt the method for duplicate supply multimode wet method electrolysis process reviver.This technology does not only consume chemical reagent and raw material, avoided the secondary pollution of extractive process, and realized that the grid in the waste lead acid battery, lead plaster, sulfuric acid, plastic casing etc. are classified and reclaimed and refine, obtain stereotype respectively, plastics and black sulfuric acid have been eliminated leaded and SO in the existing pyrometallurgical smelting of lead process
2Waste gas, the pollution of waste residue, overcome existing wet method refining splicer process flow complexity, defective that lead recovery is low.Use method of the present invention, flow process is simple, and the plumbous rate of recovery reaches more than 96%.The stereotype that utilizes this new technology to obtain can reach 99.95% with reviver purity further by having the electrorefining technology of ripe lead fluorosilicate now.
The invention provides method plumbous in a kind of acid wet method electrolytic recovery waste lead acid battery, it is characterized in that, will be from old and useless battery isolated battery unit or battery pack directly place electrolysis tank, adopt the reduction of duplicate supply multimode electrolysis process plumbous, on grid, form stereotype, to reclaim lead.
The method of lead in the acid wet method electrolytic recovery waste lead acid battery provided by the invention comprises step:
A. waste lead acid battery is fallen acid treatment;
B. cut open from through falling the shell of waste lead acid battery of acid treatment, obtain dilute sulfuric acid, waste plastics and battery unit or battery pack through separation;
C. will be from old and useless battery isolated battery unit or battery pack place electrolysis tank, use the reduction of duplicate supply multimode electrolysis process plumbous, on grid, form stereotype, to reclaim lead.
Described waste lead acid battery fall acid treatment and shell cut open from can end user's construction method or mechanical means carry out, obtain dilute sulfuric acid, waste plastics and battery unit or battery pack thus.The dilute sulfuric acid that obtains is through purifying, and after the filtration, the acid of most of process benefit is mixed with electrolyte again and uses, and fraction dilute sulfuric acid thin up is used for follow-up reviver process after the weight percent concentration of 0.1-20%.For valve-regulated full sealed lead-acid battery, can directly isolate battery pack and battery case without falling sour process.
The electrolysis tank that uses in this method is made by pure lead, corrosion-resistant lead alloy (as plumbous calcium, pb-ag alloy) or polyvinyl chloride (PVC) lining with lead material.And in electrolysis tank, injecting electrolyte, described electrolyte is the dilute sulfuric acid of 0.1-20 weight % concentration.In addition, in order to improve electrolytic efficiency, improve the cathodic process of electrode, can in electrolyte, suitably add some complexing agents, amine triacetic acid for example, natrium citricum, EDTA, sodium acetate or sodium glutamate etc., it is between the 0.03%-10% that the addition of these complexing agents generally is controlled at mass concentration.
The method of lead in the acid wet method electrolytic recovery waste lead acid battery of the present invention is primarily characterized in that and adopts duplicate supply multimode electrolysis process reduction lead.The anodal group of plumbous negative pole group (4) in all battery pack of soon taking out from old and useless battery and brown lead oxide (5) is connected in parallel with lead respectively and forms terminal (1) and terminal (2).This battery pack places lead to change in the electrolysis tank (7), and lead changes into electrolysis tank and connects terminal (3) with lead.The terminal (3) and the anodal terminal of organizing (2) of brown lead oxide that lead are changed into electrolysis tank (7) are connected on respectively on the positive pole and negative pole of power supply A, simultaneously the terminal (2) of the anodal group of brown lead oxide and the terminal (1) of plumbous negative pole group are connected on respectively on the positive pole and negative pole of power supply B, form duplicate supply multimode electrolysis mode.Toward the reduction electrolyte of electrolysis tank injection based on dilute sulfuric acid, and voltage and the output current of adjusting power supply A and B, the electrolysis temperature of control electrolysis tank is 10-50 ℃, electrolysis time is 5-45 hour.Bimodulus piece electrolytic process can be converted into metallic lead with the lead sulfate on brown lead oxide pole plate and the negative pole stereotype, brown lead oxide and other leadization thing, is deposited on and forms stereotype on the grid, isolates sulfuric acid simultaneously from electrolyte.
Through electrochemical reducting reaction obtain be deposited on the stereotype that forms on the grid repressed after, fusion under 350-450 ℃ of temperature in heating furnace, can obtain purity and be at least 96% regeneration lead pig or stereotype, preferably obtaining purity is regeneration lead pig or the stereotype of 97-99%.The regeneration lead pig or the stereotype that are obtained by the plumbous technology of the known lead fluorosilicate electrolytic refining of prior art, can obtain purity and be the electrolytic lead 99.95% or more, and metals such as a spot of antimony that contains in the recovery grid and tin.The electrolyte of above-mentioned said reviver process can be that the primary cell electrolyte dilution forms, and perhaps water cleans the acid waste liquid that contains that inside battery obtains, also can be the follow-up cleaning process of battery recycling stereotype produce contain acid waste liquid.Power supply A and B are common DC power supply, can be constant-current source or constant pressure source, also can be the Rectified alternating currents that rectification obtains.By regulating voltage and the output current of power supply A and B, in the 200-1000A scope, the Current Control of power supply B is in the 180-850A scope with the Current Control of described power supply A.
Experimental calculation shows that the rate of recovery of automobile lead-acid battery is generally 96.0-97.5% in batches, and the rate of recovery of electric motor car totally-enclosed battery reaches 96.1-98.6%.According to the situation of scrapping and the service time of lead-acid battery, the power consumption of producing reviver per ton is 570-930KWh.
In the implementation process, we are by the experiment of all kinds of lead-acid batteries of brands such as thousands of sails, Delphi, unification, day energy, super prestige, profit honor and blue sky, find that lead recovery method of the present invention can carry out direct reviver process to these batteries, obtain the regeneration stereotype.Show that method of the present invention is fit to the electric motor car sealed lead acid battery, also be fit to paste spread type even hauling type lead-acid battery.Wherein with blue sky 12V, the 10Ah battery of electric vehicle is an example, every total cell weight is 4.22kg, use method one step refining lead of the present invention to obtain the lead bullion plate, weigh to reclaiming lead, quality 2.94kg, the plumbous consumption rate that contrast experiment's electrogenesis in previous existence pond is average is through repeatedly testing the average recovery rate η (before the fusion)=96.9% that obtains.η (fusion of lead)=96.1%, refining plumbous rate (with the total restatement of battery) is 65.22%.Lead bullion after this fusion, content reaches 97.5-98.5%, can directly sell as product, perhaps obtains the electrolysis lead bullion through electrorefining.
Data information shows according to the relevent statistics, in the lead-acid battery that China scraps at present every year only one of battery of electric vehicle just reach 290,000 tons, the rate of recovery according to present pyrometallurgical smelting of lead technology 80% is calculated, approximately can reclaim 14.5 ten thousand tons of lead wherein, and the refining that causes tens thousand of tons plumbous waste residue, sulfur trioxide and low value-added gypsum by-product.If adopt new Wet technique of the present invention, not only reduce a large amount of investments in fixed assets and environmental improvement expense, and can directly reclaim 18.9 ten thousand tons of lead bullion wherein, by-product sulfuric acid can be used for producing gypsum or chemical fertilizer simultaneously.According to present 1.37 ten thousand yuan/ton lead bullion price, directly the economic benefit that produces reaches 6.03 hundred million yuan.
Description of drawings
Fig. 1 is a cell construction schematic diagram of the present invention.Wherein:
1. negative electrode lead group terminal, 2. brown lead oxide group terminal, 3. reduction electrolysis tank terminal,
4. plumbous negative pole, 5. brown lead oxide positive pole, 6. diaphragm plate, 7. reduction electrolysis tank.
Embodiment
To further the present invention be described below by embodiment.
Get the 12V of blue sky, 10 Tianjin Gao Ke company, 10Ah battery of electric vehicle, 42.6 kilograms of battery pack gross weights.10 batteries are put into grinding tool, cut the battery pack loam cake, take out battery pack by manipulator then, obtain 60 battery units by cutting machine.
This moment, the both positive and negative polarity with 60 battery units was connected with parallel connection with lead respectively, and this battery pack is placed on 17 * 200 * 7.5cm
3Internal layer be in the PVC plastic channel of 1.5mm stereotype.In electrolysis tank, inject the 12L running water then, plumbous electrolysis tank and brown lead oxide anode constituents are not connected on the positive pole and negative pole of power supply A, simultaneously anodal group of brown lead oxide and plumbous negative pole group are connected on respectively on the positive pole and negative pole of power supply B, form duplicate supply multimode electrolysis mode.By regulating output voltage and the output current of power supply A and B, the electric current of control power supply A and B is respectively 240A and 195A, keeps electrolyte temperature at 20-40 ℃, and continuous electrolysis 39 hours obtains the dilute sulfuric acid of 20-25% and the stereotype of regenerating.
Take out battery pack, behind clear water cleaning disacidify liquid, go out stereotype and dividing plate by mechanical separation.Then with lead grill in nitrogen or vacuum environment with behind 50-100 ℃ the temperature drying, obtain stereotype.Obtain in the above-mentioned cleaning process contain acid waste liquid can be directly as the electrolyte of next group reviver process.
After above-mentioned stereotype is repressed, after 350-450 ℃ of temperature fusion, obtain the lead pig of regenerating.The purity of this lead pig is 97-98%.Electrolytic refining process through common can obtain purity at the electrolytic lead more than 99.95%.The plumbous rate of recovery is 96.5%.
Embodiment 2
Get the 12V of 10 Baoding sail companies, 45Ah automobile batteries, 132 kilograms of battery pack gross weights.10 batteries are put into grinding tool, cut the battery pack loam cake, pour out electrolyte reclaim sulfuric acid in the acid storage then by the cutting machine unification.Clean inside battery with 60 premium on currency, to remove the residual acid solution of battery, this acid solution is in the electrolysis tank of going into lining with lead after the cleaning.Battery pack by manipulator takes out automobile batteries obtains 60 battery units.
This moment, the both positive and negative polarity with 60 battery units was connected with parallel way with the plumbous lead that connects row respectively, and this battery pack is put into 45 * 400 * 15cm
3Internal layer be in the PVC plastic channel of 2mm stereotype.In electrolysis tank, inject an amount of water then, do not have battery pack until the water surface.Plumbous electrolysis tank and brown lead oxide anode constituents are not connected on the positive pole and negative pole of power supply A, simultaneously anodal group of brown lead oxide and plumbous negative pole group are connected on respectively on the positive pole and negative pole of power supply B, form duplicate supply multimode electrolysis mode.By regulating output voltage and the output current of power supply A and B, the electric current of control power supply A and B is respectively 950A and 830A, keeps electrolyte temperature at 20-40 ℃, and continuous electrolysis 37 hours obtains the dilute sulfuric acid of 10-15% and the stereotype of regenerating.
Take out battery pack, behind clear water cleaning disacidify liquid, go out stereotype and plastic septum by mechanical separation.Then with lead grill in nitrogen or vacuum environment with behind 50-100 ℃ the temperature drying, obtain stereotype.Obtain in the above-mentioned cleaning process contain acid waste liquid can be directly as the electrolyte of next group reviver process.
Above-mentioned stereotype after 350-450 ℃ of temperature fusion, obtains the lead pig of regenerating after the compacting of hydraulic press static pressure.The purity of this lead pig is 97-98%.Electrolytic refining process through common can obtain purity at the electrolytic lead more than 99.95%, and the plumbous rate of recovery reaches 96.2%.
Get the 12V of 2 northeast storage battery companies, the 135Ah lorry is with waste lead acid battery (battery types please be described), about 92 kilograms of battery gross weight.2 batteries are put into grinding tool, cut the battery pack loam cake, pour out electrolyte reclaim sulfuric acid in the acid storage then by the cutting machine unification.Clean inside battery with 50 premium on currency, to remove the residual acid solution of battery, this acid solution is in the electrolysis tank of going into to serve as a contrast the pure lead of 3mm after the cleaning.Battery pack by manipulator takes out automobile batteries obtains 12 battery cells.
This moment, the both positive and negative polarity with 12 battery units was connected with parallel way with the plumbous lead that connects row respectively, and this battery pack is put into 50 * 140 * 15cm
3Internal layer be in the PVC plastic channel of 3mm stereotype.In electrolysis tank, inject an amount of water then, do not have battery pack 1cm until the water surface.Plumbous electrolysis tank and brown lead oxide anode constituents are not connected on the positive pole and negative pole of power supply A, simultaneously anodal group of brown lead oxide and plumbous negative pole group are connected on respectively on the positive pole and negative pole of power supply B, form duplicate supply multimode electrolysis mode.By regulating output voltage and the output current of power supply A and B, the electric current of control power supply A and B is respectively 510A and 450A, keeps the electrolyte temperature fluctuation at 20-45 ℃, and continuous electrolysis 32 hours obtains the dilute sulfuric acid of 10-15% and the stereotype of regenerating.
Take out battery pack, behind clear water cleaning disacidify liquid, go out stereotype and plastic septum by mechanical separation.Then with lead grill in nitrogen or vacuum environment with behind 50-100 ℃ the temperature drying, obtain stereotype.Obtain in the above-mentioned cleaning process contain acid waste liquid can be directly as the electrolyte of next group reviver process.
Above-mentioned stereotype after 350-450 ℃ of temperature fusion, obtains the lead pig of regenerating after the compacting of hydraulic press static pressure.The purity of this lead pig is 96.5-98%.Electrolytic refining process through common can obtain purity at the electrolytic lead more than 99.95%, and the plumbous rate of recovery is between 96.1-97.5%.
Though described the present invention in conjunction with specific embodiments at this; but be understood that the present invention is not limited to these execution modes disclosed herein; on the contrary, the scope of protection of present invention contains the various changes in the spirit and scope that are included in claims and is equal to replacement.
Claims (9)
1, the method for lead in the acid wet method electrolytic recovery waste lead acid battery is characterized in that comprising:
Will be from old and useless battery isolated battery unit or battery pack place electrolysis tank, adopt the plumbous method of duplicate supply multimode electrolysis process reduction, anodal group of all battery units that will take out from old and useless battery or the brown lead oxide in the battery pack and plumbous negative pole group are connected in parallel with lead respectively, plumbous electrolysis tank and brown lead oxide anode constituents are not connected on the positive pole and negative pole of power supply A, simultaneously anodal group of brown lead oxide and plumbous negative pole group are connected on respectively on the positive pole and negative pole of power supply B, form duplicate supply multimode electrolysis mode, by regulating voltage and the output current of power supply A and B, the electrolysis temperature and the electrolysis time of control electrolysis tank carry out electrolysis, with the lead sulfate on brown lead oxide pole plate and the stereotype, brown lead oxide and other leadization thing are converted into metallic lead, on grid, form stereotype, to reclaim lead.
2, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 1, it is characterized in that, battery unit that takes out from old and useless battery or battery pack are placing before electrolysis tank carries out duplicate supply multimode electrolysis process, earlier waste lead acid battery is fallen acid treatment, and cut open shell from described waste lead acid battery, obtain dilute sulfuric acid, waste plastics and battery unit or battery pack through separation.
3, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 1, wherein, by regulating voltage and the output current of power supply A and B, in the 200-1000A scope, the Current Control of power supply B is in the 180-850A scope with the Current Control of described power supply A.
4, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 2, wherein, the acid treatment and the cuing open from end user's construction method or mechanical means of shell of described waste lead acid battery are carried out.
5, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 1, wherein, described electrolysis tank is made by pure lead, corrosion-resistant lead alloy or polyvinyl chloride lining with lead material.
6, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 1 comprises that further inject electrolyte in electrolysis tank, described electrolyte is the dilute sulfuric acid of 0.1-20 weight % concentration.
7, according to method plumbous in any described acid wet method electrolytic recovery waste lead acid battery of claim 1-6, wherein, the electrolysis temperature of electrolysis tank is 10-50 ℃, and electrolysis time is 5-45 hour.
8, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 1, wherein, be deposited on the stereotype that forms on the grid repressed after, fusion under 350-450 ℃ of temperature, obtain purity and be at least 96% regeneration lead pig or stereotype, and the plumbous rate of recovery is more than 96%.
9, the method for lead in the acid wet method electrolytic recovery waste lead acid battery according to claim 8, wherein, the purity of described regeneration lead pig or stereotype is 97-99%, further uses the plumbous technology of known lead fluorosilicate electrolytic refining, can obtain purity and be the electrolytic lead more than 99.95%.
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| CN101613803B (en) * | 2009-07-28 | 2010-12-08 | 北京科技大学 | Method for recovering lead from lead paste of waste lead-acid battery |
| EP2323239A1 (en) * | 2009-11-13 | 2011-05-18 | Ascot S.R.L. | Integrated station for DC electric supply to geographically remote loads, for instance telecommunications antenna |
| CN102396099B (en) * | 2010-02-01 | 2014-07-16 | 深圳市雄韬电源科技股份有限公司 | Method for recycling negative electrode plate of waste lead-acid power battery |
| CN101824639B (en) * | 2010-04-30 | 2011-08-17 | 浙江汇同电源有限公司 | Anode of electrodeposition device for recovery of lead-acid battery and manufacturing method thereof |
| CN102618884B (en) * | 2012-03-16 | 2014-12-31 | 北京化工大学 | Lead regeneration method for recovering lead paste from waste lead acid storage battery by wet method |
| CN104183884A (en) * | 2013-07-31 | 2014-12-03 | 天能电池(芜湖)有限公司 | Lead acid storage battery waste acid recycling technology |
| CN103606685B (en) * | 2013-10-21 | 2015-07-08 | 安徽省华森电源有限公司 | Environment-friendly process for preparing high-energy storage battery plate by using secondary lead |
| US9751067B2 (en) | 2014-06-20 | 2017-09-05 | Johnson Controls Technology Company | Methods for purifying and recycling lead from spent lead-acid batteries |
| US9670565B2 (en) | 2014-06-20 | 2017-06-06 | Johnson Controls Technology Company | Systems and methods for the hydrometallurgical recovery of lead from spent lead-acid batteries and the preparation of lead oxide for use in new lead-acid batteries |
| US10062933B2 (en) | 2015-12-14 | 2018-08-28 | Johnson Controls Technology Company | Hydrometallurgical electrowinning of lead from spent lead-acid batteries |
| CN106207301A (en) * | 2016-08-11 | 2016-12-07 | 合肥国轩高科动力能源有限公司 | Method for electrolyzing and recycling negative electrode material and copper foil of waste lithium ion battery |
| CN107722662B (en) * | 2017-10-18 | 2020-07-24 | 界首市双特新材料科技有限公司 | Recovery processing technology of waste battery packaging material |
| CN110528026A (en) * | 2019-09-10 | 2019-12-03 | 沈阳鑫迪环境技术有限公司 | A kind of lead plaster acidity Solid phase electrolysis method |
| CN113106469A (en) * | 2021-03-05 | 2021-07-13 | 蚌埠睿德新能源科技有限公司 | Lead plaster desulfurization method for waste lead-acid storage battery |
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