CN101030663A - Method for recovering and regenerating refused battery critical material - Google Patents
Method for recovering and regenerating refused battery critical material Download PDFInfo
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- CN101030663A CN101030663A CNA2007100652096A CN200710065209A CN101030663A CN 101030663 A CN101030663 A CN 101030663A CN A2007100652096 A CNA2007100652096 A CN A2007100652096A CN 200710065209 A CN200710065209 A CN 200710065209A CN 101030663 A CN101030663 A CN 101030663A
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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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Abstract
The invention is concerned with the invalidation reason for capacity loss of used rechargeable batteries. It reaches the feasibility to resume the capability of filling and discharging of electricity content, voltage flat and reused life, and a new way to callback and rebirth the content and electrochemistry capability of anode and cathode of used battery and afford a effective method, i.e. nano-method. Take off active matter from the anode and cathode of used battery by vibration or peel-off with machine. Wash the pole with distilled water and carry with pump-filtration till the filtrate is neutral, dry in vacuum to rebirth the electrochemistry capability of pole. This invention reduces the pollution of used rechargeable batteries to environment and is suitable to low cost of rechargeable batteries and its key material at a certain extent with obvious effect and easy operation.
Description
Technical field
The present invention relates to the recovery and the cycling and reutilization technical field of positive and negative electrode material in the waste secondary battery.
Background technology
Along with China's rapid economy development, resources effective utilization rationally and environmental improvement are extremely urgent.China is the production and consumption big country of primary cell, secondary cell, and the growth at full speed of various portable type electronic products forms huge Battery Market.From China's energy strategy security standpoint, the motor vehicle particularly development of hybrid vehicle has been listed country's related industry planning the Eleventh Five-Year Plan period in.The share in the shared market of electrokinetic cell progressively promotes, and shortage of resources of Yin Faing and environmental problem are serious day by day thus.Therefore, carry out recovery, regeneration and the recycling of old and useless battery, particularly the relevant above-mentioned research at electrokinetic cell has urgency more.Simultaneously, waste battery causes serious heavy metal environmental pollution and comprehensive anti-pollution and recycling waste to list major fields and preferential theme thereof in the environmental area in.At present, China's old and useless battery rate of recovery less than 2% is far below the recovery utilization rate of developed country 50%.Particularly the populous and living standards of the people of China improves constantly, the MH-Ni battery will be widely used and develop, and simultaneously its environment and resource problem of bringing will day by day highlight, and the recycling of old and useless battery becomes people at present than one of question of common concern.
With regard to secondary cell, be of the pollution of toxic heavy metal elements such as strictness control Pb and Cd to environment, developed country such as America and Europe and Japan has successively set up the retrieval management rules of relevant waste lead acid battery and Ni/Cd battery, and the regeneration of waste nickel hydrogen battery, lithium ion battery is studied as the important techniques brainstorm subject.Thereby when realizing the environmental protection target, also reclaimed various valuable metals, obtained good economic benefit and social benefit.
For old and useless battery, mainly adopt pyrogenic process and wet method to reclaim its noble metal at present.After old and useless battery carried out category filter, fragmentation, put again in people's baking furnace 600～800 ℃ of following roastings,, again the roasting residue is put into rotary kiln 1100～1300 ℃ of following roastings with extracting mercury after the condensation of gas of discharging, from flue gas, reclaim zinc oxide, from residue, reclaim manganese and iron.It is at high temperature to make the metal in the used dry batteries and the process of compound oxidation, reduction, decomposition, volatilization and condensation thereof that used dry batteries is handled in pyrometallurgy.Pyrogenic process divides two kinds in normal pressure and vacuum again, and normal pressure metallurgy method All Jobs all carries out in atmosphere, and the vacuum rule is to carry out under airtight subnormal ambient.Most scholars think that pyrometallurgy is the best approach of handling used dry batteries, reclaim the most effective to the processing of mercury.Traditional normal pressure metallurgical method mainly contains two kinds: the one, under lower temperature, heat used dry batteries, and make the mercury volatilization earlier, under higher temperature, reclaim zinc and other heavy metal then; The 2nd, with used dry batteries roasting at high temperature, make the volatilization of wherein volatile metal and oxide thereof, residue is as metallurgical intermediate product or otherwise processed.
Hydrometallurgy process is to control the stability of material in solution by creating conditions.For example: leaching process is exactly by adding certain dissolution with solvents waste material, metal ion being stabilized in the solution.Deposition process then requires to create conditions and makes metal ion unstable in solution.In hydrometallurgy, solvent extraction is the method for a kind of separation, enrichment or purified metal, its essence be to make metal ion or its compound by the aqueous solution change over to the not miscible liquid organic facies of water among.The collection that obtains is thus closed liquid and is then stripped, and makes the metal that is extracted change water over to by organic facies again.Organic facies is returned extraction process and is recycled after regeneration.According to the composition and the character of stoste, it is the solution extraction key of success that choose reasonable is used extractant and diluent.PingweiZhang (Hydrometallurgy, 1998, (50): 61-75) wait the people to utilize valuable metal in the hydrometallurgic recovery waste nickel hydrogen battery, proposed the recovery battery waste and mainly contained 5 unit operations steps and form, and the optimum condition that draws leaching is: 3mol/LHCl, 95 ℃, solid-to-liquid ratio is 1: 9, processing time 9h, with this understanding, can leach＞96% nickel 99% rare earth and 100% cobalt.(US 5858061,1999-01-12) wait the people to use H earlier for Klaus Kleinsorgen
2SO
4Dissolving Ni-MH battery waste material, then digestion liquid is carried out solvent extraction, select and the two-phase volume ratio by control pH value, solvent, rare earth element, iron, aluminium etc. will be separated out with the form of precipitation, then there are nickel and the cobalt identical in the liquid phase with ratio in the waste material, by with one-step electrolysis the intermediate product of handling being made the intermediate alloy that can utilize again, rare earth element last and that be settled out is reprocessed into mishmetal through electric power metallurgy and is used for making new hydrogen bearing alloy then.Up to now, though both at home and abroad the recovery and the regeneration techniques of waste secondary battery launched a series of research work, and obtained certain progress, but still deposit a lot of technical bottlenecks.
The present invention is primarily aimed at the failure cause of old and useless battery, study its charge/discharge capacity, voltage platform, the feasibility of performance recoveries such as cycle life, just explored old and useless battery, negative material capacity and chemical property reclaim the new way with regeneration, a kind of comparatively effective method---nanometer facture is proposed, inefficacy secondary battery anode and cathode material is taken off active material by methods such as machinery concussions, wash with distilled water, suction filtration to filtrate is neutral, vacuum drying, can reach the purpose of electrode material chemical property regeneration after treatment, thereby realized the circular regeneration of old and useless battery electrode material to a certain extent, effect is obvious and simple.The present invention can reduce the pollution that waste secondary battery brings to environment, will help the cost degradation of secondary cell.This method is simple, effect is obvious, and can not cause any secondary pollution to environment.
Summary of the invention
The purpose of this invention is to provide a kind of method that is used for the positive and negative material recovery regeneration of waste secondary battery, can overcome above-mentioned defective.It is characterized in that: inefficacy secondary cell positive and negative electrode material is taken off active material by methods such as ultrasonic concussion or mechanical agitation from collector, with distilled water washing, suction filtration to filtrate is neutral, vacuum drying, carry out to reach the purpose of electrode material chemical property regeneration after nanometer is handled through mechanical ball milling or chemical method, thereby realized the cycling and reutilization of battery material to a certain extent.The condition that need to prove the required control of this method comprises: extraneous factors such as high-temperature process temperature, ball milling time, acid treatment.
Concrete implementation step of the present invention is, at normal temperatures, is the inefficacy Ni-MH battery below 80% of former nominal capacity with doing for 1000 weeks through charge and discharge circulation life and capacity attenuation, is used for battery material regeneration tests example of the present invention.Choosing certain high-temperature process temperature, ultrasonic wave time, ball milling time respectively carries out nanometer to battery material and handles.Material processed is carried out the check and analysis of chemical property and positive and negative electrode material aspect thereof after finishing to battery material.Through the Electrochemical Detection excellent performance, method of testing is through the positive and negative electrode after the said method regeneration: the 0.1C 12h that charges, shelve 30min, and 0.2C is discharged to the regulation electrode potential, 100mV just very wherein, negative pole is-740mV (vs.Hg/HgO/6M KOH).This positive and negative electrode material properties test result such as Fig. 2, shown in Figure 3.
In sum, a kind of method---nanometer facture that is used for old and useless battery material recovery regeneration provided by the invention has realized the chemical property circular regeneration of old and useless battery electrode material to a certain extent, and effect is obvious and simple.The present invention can reduce the pollution that waste secondary battery brings to environment, will help the cost degradation of secondary cell, and compared with prior art, production cost is low, economic benefit is high, and method is easy, easy operating.
Description of drawings
The flow chart of Fig. 1-waste secondary battery material recovery regeneration
Discharge performance comparison curves before and after Fig. 2-hydrogen storing alloy powder regeneration
Discharge performance comparison curves before and after Fig. 3-nickel hydroxide positive plate powder regeneration
Embodiment
Embodiment 1:
To make 1000 all charge and discharge circulation lifes and consistency Ni-MH battery preferably, and be used for nanometer of the present invention and handle the experiment of waste nickel hydrogen battery negative material.Battery is carried out machine cuts and dissection, take out negative plate, through methods such as ultrasonic oscillation or mechanical agitation negative electrode active material is taken off from nickel foam or nickel plating perforated steel ribbon collector, with distilled water washing, suction filtration to filtrate is neutral, and dries under the condition that 80 ℃ of vacuum degrees of temperature are 0.05Mpa.Through salt acid treatment active material-alloyed powder, behind mechanical ball milling or the chemical treatment 20h to granularity be nanoscale, behind the additives such as additional nickel powder, be pressed into circular electrode, 0.1C charge 12 hours, be-740mV (vs.Hg/HgO/6M KOH) that Fig. 2 is the discharge performance comparison curves before and after the hydrogen storing alloy powder regeneration 0.2C be discharged to electrode potential.Reclaim hydrogen storing alloy powder with this method, its chemical property is significantly improved, and can be used as cell negative electrode material once more.
Embodiment 2:
To make 1000 all charge and discharge circulation lifes and consistency Ni-MH battery preferably, and be used for nanometer of the present invention and handle the experiment of waste nickel hydrogen battery positive electrode.Battery is carried out machine cuts and dissection, take out positive plate, through methods such as ultrasonic oscillation or mechanical agitation positive active material is taken off from the nickel foam collector, be neutral with distilled water washing, suction filtration to filtrate, and under the condition that 80 ℃ of temperature vacuum degrees are 0.05Mpa, dry.Active material behind mechanical ball milling 20h to granularity be nanoscale, after replenishing additives such as nickel, cobalt powder, be pressed into circular electrode, 0.1C charge 12 hours, 0.2C be discharged to electrode potential is 100mV (vs.Hg/HgO/6M KOH), and Fig. 3 is the discharge performance comparison curves before and after the regeneration of nickel hydroxide positive plate powder.Reclaim positive powder with this method, its chemical property is significantly improved, and can be used as cell positive material once more.
Embodiment 3:
To make 1000 all charge and discharge circulation lifes and consistency Ni-MH battery preferably, and be used for nanometer of the present invention and handle the experiment of waste nickel hydrogen battery negative material.Battery is carried out machine cuts and dissection, take out negative plate, through the ultrasonic oscillation method negative electrode active material is taken off from nickel foam or nickel plating perforated steel ribbon collector, be neutral with distilled water washing, suction filtration to filtrate, and under the condition that 40 ℃ of temperature vacuum degrees are 0.08Mpa, dry.After acetic acid is handled active material-alloyed powder mechanical ball milling 12h to granularity be nanoscale, be pressed into circular electrode, 0.1C charging 12 hours, 0.2C is discharged to electrode potential and is-740mV (vs.Hg/HgO/6M KOH).Reclaim hydrogen storing alloy powder with this method, its discharge capacity and voltage obviously improve, and can be used as cell negative electrode material once more.
Embodiment 4:
To make 1000 all charge and discharge circulation lifes and consistency Ni-MH battery preferably, and be used for nanometer of the present invention and handle the experiment of waste nickel hydrogen battery positive electrode.Battery is carried out machine cuts and dissects back taking-up positive plate, through the ultrasonic oscillation method positive active material is taken off from the nickel foam collector, with distilled water washing, suction filtration to filtrate is neutral, and dries under the condition that 40 ℃ of temperature vacuum degrees are 0.08Mpa.Handle active material through mechanical ball milling 12h to granularity be nanoscale, replenish the cobalt oxide powder additive after, be pressed into circular electrode, 0.1C charging 12 hours, it is 100mV (vs.Hg/HgO/6M KOH) that 0.2C is discharged to electrode potential.Reclaim positive powder with this method, its chemical property is significantly improved, and can be used as cell positive material once more.
Embodiment 5:
To make 1000 all charge and discharge circulation lifes and consistency Ni-MH battery preferably, and be used for nanometer of the present invention and handle the experiment of waste nickel hydrogen battery negative material.Battery is carried out machine cuts and dissection, take out negative plate, through the mechanical agitation method negative electrode active material is taken off from nickel foam or nickel plating perforated steel ribbon collector, be neutral with distilled water washing, suction filtration to filtrate, and under the condition of 40 ℃ of vacuum degree 0.08Mpa of temperature, dry.Through amion acetic acid handle active material-alloyed powder through mechanical ball milling or chemical treatment 25h to granularity be nanoscale, then alloyed powder is carried out being pressed into circular electrode after silver-plated surface is modified, 0.1C charge 12 hours, 0.2C be discharged to electrode potential be-740mV (vs.Hg/HgO/6M KOH), reclaim hydrogen storing alloy powder with this method, its Stability Analysis of Structures and chemical property are significantly improved, and can be used as cell negative electrode material once more.
Embodiment 6:
To do 500 all charge and discharge circulation lifes and consistency lithium ion battery preferably, and be used for nanometer of the present invention and handle the waste lithium ion cell anode material experiment.Battery is carried out machine cuts dissection and taking-up positive plate in the water, through peeling off positive active material cobalt acid lithium is taken off from aluminum foil current collector, with distilled water washing, suction filtration to filtrate is neutral, and is that high-temperature roasting removes conductive agents such as carbon elimination under 800 ℃ of conditions through temperature in air.With active material cobalt acid lithium mechanical ball milling 20h to granularity be nano-scale particle, the positive electrode of regeneration is prepared into positive pole, lithium metal is a negative pole, forms button cell.0.1C charge to 4.2V, 0.2C is discharged to 3V.The positive electrode that reclaims with this method has identical structure and similar charge-discharge performance with raw material.
Claims (6)
1. this method is characterised in that: but the waste secondary battery positive and negative electrode material that will lose efficacy takes off active material by methods such as machinery concussion are peelable, with distilled water washing, suction filtration to filtrate is neutral, vacuum drying, through the nanometer facture, can reach the purpose of electrode material chemical property regeneration, thereby realize that to a certain extent waste secondary battery electrode material capacity and chemical property reclaim and regeneration.It is characterized in that finishing through following steps:
1) at room temperature the waste secondary battery shell is separated and cut open, take out positive and negative plate;
2) inefficacy secondary cell pole piece being taken off the positive and negative electrode active material by methods such as ultrasonic oscillation or mechanical agitation from collector, is neutral with distilled water washing, suction filtration to filtrate, and vacuum drying or high-temperature process are to remove binding agent and carbonaceous conductive agent etc.; Use the acid treatment active material, to remove oxide on surface or hydroxide;
3) by certain hour mechanical ball milling or chemical method, with the positive and negative electrode material nanoization, and suitably replenish necessary additive or carry out surface treatment, make chemical property regeneration such as electrode material capacity;
2. according to the method for the regeneration of the waste secondary battery electrode material described in the claim 1, it is characterized in that described secondary cell is mainly lead-acid battery, nickel-cadmium cell, Ni-MH battery, lithium ion battery;
3. according to the method for the regeneration of the waste secondary battery electrode material described in the claim 1, it is characterized in that described high-temperature process temperature is between 60-900 ℃;
4. according to the method for the waste secondary battery electrode material described in the claim 1 regeneration, it is characterized in that described vacuum drying temperature between 30-80 ℃, vacuum degree is under the condition of 0.1-0.01Mpa;
5. according to the method for the regeneration of the waste secondary battery electrode material described in the claim 1, it is characterized in that described acid treatment comprises acetic acid, oxalic acid, formic acid, amion acetic acid, hydrochloric acid or sulfuric acid;
6. according to the method for the regeneration of the waste secondary battery electrode material described in the claim 1, it is characterized in that described additional necessary additive or surface treatment comprise surface treatments such as adding conductive agent, copper or silver.Processing time is 0.5h～40h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100652096A CN101030663A (en) | 2007-04-06 | 2007-04-06 | Method for recovering and regenerating refused battery critical material |
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| CNA2007100652096A CN101030663A (en) | 2007-04-06 | 2007-04-06 | Method for recovering and regenerating refused battery critical material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184340A (en) * | 2011-12-31 | 2013-07-03 | 深圳市雄韬电源科技股份有限公司 | Method for recovering lead plaster of negative pole of disused lead acid storage battery and application of recovered lead plaster |
| CN104183882A (en) * | 2013-05-27 | 2014-12-03 | 湖南邦普循环科技有限公司 | Separation method for current collectors and active materials in lithium ion battery positive and negative pole pieces |
| CN105375011A (en) * | 2015-11-25 | 2016-03-02 | 百顺松涛（天津）动力电池科技发展有限公司 | Solution for problem of jellylike sizing agent after material mixing of ternary cathode materials |
| CN106935924A (en) * | 2017-04-07 | 2017-07-07 | 山东理工大学 | The circulation utilization method of valuable metal in waste and old ni-mh power battery cathode plate |
| CN108336440A (en) * | 2018-01-05 | 2018-07-27 | 深圳市比克电池有限公司 | A kind of waste and old lithium ion battery collector recovery method |
| WO2018192120A1 (en) * | 2017-04-18 | 2018-10-25 | 中科过程（北京）科技有限公司 | Method for efficiently separating metal current collector of positive electrode material of waste lithium ion battery |
| CN108760586A (en) * | 2018-05-23 | 2018-11-06 | 广州能源检测研究院 | A kind of method that overlay material particle size is distributed in detection lithium battery pole slice |
| CN109923729A (en) * | 2017-07-27 | 2019-06-21 | 株式会社Lg化学 | The method of redgenerated cell |
| CN111628234A (en) * | 2020-05-27 | 2020-09-04 | 云南省能源研究院有限公司 | Waste battery recovery system and recovery method thereof |
| CN111684089A (en) * | 2017-11-28 | 2020-09-18 | 尼拉国际股份公司 | Grinding of recovered negative electrode material |
-
2007
- 2007-04-06 CN CNA2007100652096A patent/CN101030663A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184340A (en) * | 2011-12-31 | 2013-07-03 | 深圳市雄韬电源科技股份有限公司 | Method for recovering lead plaster of negative pole of disused lead acid storage battery and application of recovered lead plaster |
| CN103184340B (en) * | 2011-12-31 | 2014-10-29 | 深圳市雄韬电源科技股份有限公司 | Method for recovering lead plaster of negative pole of disused lead acid storage battery and application of recovered lead plaster |
| CN104183882A (en) * | 2013-05-27 | 2014-12-03 | 湖南邦普循环科技有限公司 | Separation method for current collectors and active materials in lithium ion battery positive and negative pole pieces |
| CN105375011A (en) * | 2015-11-25 | 2016-03-02 | 百顺松涛（天津）动力电池科技发展有限公司 | Solution for problem of jellylike sizing agent after material mixing of ternary cathode materials |
| CN106935924A (en) * | 2017-04-07 | 2017-07-07 | 山东理工大学 | The circulation utilization method of valuable metal in waste and old ni-mh power battery cathode plate |
| WO2018192120A1 (en) * | 2017-04-18 | 2018-10-25 | 中科过程（北京）科技有限公司 | Method for efficiently separating metal current collector of positive electrode material of waste lithium ion battery |
| GB2577194A (en) * | 2017-04-18 | 2020-03-18 | Sino Science Process Beijing Science&Technology Co Ltd | Method for efficiently separating metal current collector of positive electrode material of waste lithium ion battery |
| GB2577194B (en) * | 2017-04-18 | 2022-11-23 | Sino Science Process Beijing Science&Technology Co Ltd | Method for efficiently separating metal current collector and cathode material of waste lithium ion battery |
| CN109923729A (en) * | 2017-07-27 | 2019-06-21 | 株式会社Lg化学 | The method of redgenerated cell |
| US11387499B2 (en) | 2017-07-27 | 2022-07-12 | Lg Energy Solution, Ltd. | Method for regenerating cell |
| CN111684089A (en) * | 2017-11-28 | 2020-09-18 | 尼拉国际股份公司 | Grinding of recovered negative electrode material |
| CN108336440A (en) * | 2018-01-05 | 2018-07-27 | 深圳市比克电池有限公司 | A kind of waste and old lithium ion battery collector recovery method |
| CN108336440B (en) * | 2018-01-05 | 2020-04-07 | 深圳市比克电池有限公司 | Method for recovering waste lithium ion battery current collector |
| CN108760586A (en) * | 2018-05-23 | 2018-11-06 | 广州能源检测研究院 | A kind of method that overlay material particle size is distributed in detection lithium battery pole slice |
| CN111628234A (en) * | 2020-05-27 | 2020-09-04 | 云南省能源研究院有限公司 | Waste battery recovery system and recovery method thereof |
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