CN100449011C - Method for recovering valuable metal in invalid lithium ion battery - Google Patents
Method for recovering valuable metal in invalid lithium ion battery Download PDFInfo
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- CN100449011C CN100449011C CNB2007101078376A CN200710107837A CN100449011C CN 100449011 C CN100449011 C CN 100449011C CN B2007101078376 A CNB2007101078376 A CN B2007101078376A CN 200710107837 A CN200710107837 A CN 200710107837A CN 100449011 C CN100449011 C CN 100449011C
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Abstract
A method for recovering valuable metals in a failure lithium ion battery relates to a method for recovering and treating the failure battery, in particular to a method for recovering, treating and utilizing the valuable metals in the failure lithium ion battery. The method is characterized by comprising the following steps in sequence: a. perforating the failed lithium ion battery shell for decompression; b. placing the perforated failure lithium ion battery into electrolyte for discharge treatment; c. roasting the lithium ion battery subjected to discharge treatment; d. crushing the roasted lithium ion battery; e. carrying out magnetic separation on the crushed lithium ion battery to separate out magnetic substances and non-magnetic substances; f. grading the granularity of the magnetic substance; g. and (4) grading the nonmagnetic substance by particle size. The method has the advantages of simple process, short flow and low cost; valuable metals can be recovered to the maximum extent, the recovery rates of cobalt, copper, nickel and iron are all more than 96 percent, and the economic benefit is remarkable; acid and organic solvent are not used in the process, the flue gas is easy to treat during roasting, and no secondary pollution to the environment is caused.
Description
Technical field
The recovery method of valuable metal in the disabled lithium ion cell, the recovery and treatment method, particularly disabled lithium ion cell that relates to a kind of dead battery recycles, utilizes the method for valuable metal.
Background technology
Lithium ion battery has that specific energy is big, self-discharge is little, long service life, advantage such as low in the pollution of the environment, is the main supporting power supply of notebook computer, mobile phone, digital camera, video camera products.Because the fast development in the last few years of these products, the market share of lithium ion battery is increasing, and volume of production and marketing increases fast.Be 2～3 years the work-ing life of lithium ion battery, can predict in the recent period the peak period that lithium ion battery is scrapped to occur.
Lithium ion battery generally is made up of five basic elements of character, comprises positive electrode material, negative material, ionogen, barrier film and shell.Present commercial lithium ion cell positive is by about 88% positive active material cobalt acid lithium (LiCoO
2), behind 7%～8% the acetylene black conductive agent, 3%～4% organic binder bond uniform mixing, coat on the aluminum foil current collector of thick about 20 μ m.Negative pole by about 90% negative electrode active material carbon materials, 4%～5% acetylene black conductive agent, 6%～7% tackiness agent uniform mixing after, coat on the Copper Foil collector of thick about 15 μ m.Electrolytic solution is LiPF
6Organic solution, organic solvent are carbonates.The tackiness agent main component is a polyvinylidene difluoride (PVDF) (PVDF) etc.Diaphragm material is porous polyethylene or polypropylene.Shell is materials such as stainless steel, nickel-plated steel, aluminium, and shape has cylinder shape and square.Also have elements such as insulation spacer, rupture disk, wear ring in addition.
Cobalt belongs to scarce resource, cobalt raw material costliness, production cost height.It is low that copper and mickel equally also faces ore grade, exploits and select the big problem of smelting difficulty.Lithium ion battery contains metals such as a large amount of cobalts, copper, if arbitrarily abandon, can waste a large amount of non-ferrous metal secondary resources, also can cause environmental pollution.The content of cobalt metal, copper is far above nature primary ore grade in the lithium ion battery, and the cost of recycling is low than raw ore exploitation processing cost, is good non-ferrous metal secondary resource, is easy to realize resource circulation utilization.
The fast development of lithium ion battery relatively, the research and development of disabled lithium ion cell treatment process then seem and relatively lag behind.People have begun to pay attention to the research to " mineral products " resource circulation utilization of this high value of disabled lithium ion cell in the recent period, and disabled lithium ion cell recycling technology is one of research focus of metal current recycle.At present, the disabled lithium ion cell Processing Technology also is in the laboratory study stage basically, Processing Technology Research deficiency, the report that does not have heavy industrialization to use at present.
In the patent documentation of disclosed waste and old lithium ion battery recycling, application number is the Chinese patent of CN200310103584, disclosed is to adopt the refuse battery roasting, screening produces the fine powder body of containing metal and metal oxide, through steps such as corrosion, filtration, extraction and electrolysis, prepare the method for highly purified cobalt and nickel metal; In the method, what adopt after the roasting is wet treatment method, complex process, long flow path.
The patent No. is the Chinese patent of CN200410019541.5, and disclosed is a kind of employing mechanical means or ultrasonication anode material for lithium-ion batteries, through pyroprocessing, replenishes necessary lithium compound, makes the method for positive electrode material regeneration; This method does not disclose carries out effectively reclaiming to other materials in the battery comprehensively.
Application number is the Chinese patent of CN200410019958, has disclosed a kind of hydrometallurgical processes that adopts and has reclaimed the method for preparing the cobalt oxide nano-powder from used Li ion cell; Application number is the Chinese patent of CN200410051921, and disclosed is a kind of that lithium ion battery is broken apart, behind the sour molten Battery Pole Core, reclaims the method for cobalt with the ammonium oxalate precipitation; Application number is the Chinese patent of CN200510018601, and disclosed is a kind of with after the lithium ion battery physical removal, and the calcining positive electrode material produces Co (OH) with hydrometallurgical process
2Precipitation, thereby the method for recovery cobalt; Application number is the Chinese patent of CN200510015078, and disclosed is a kind of with the cobalt acid lithium in the chemical precipitation method separating Li ionization cell, and roasting prepares the method for cobalt acid powder for lithium then; In above-mentioned technology, the wet process of employing exists complex process, cost is higher, waste water and dregs must carry out environmental protection treatment problem; And because the inside lithium ion cell structure is tight, the singularity of complicated component, the leaching yield that directly leaches metal with wet processing is not high, and to battery pretreated having relatively high expectations in early stage.
Application number is the Chinese patent of CN200610037681, discloses a kind of physical method of using the each several part in the waste and old lithium ion battery is separated, and obtains the method for pure electrode materials.Because the inside lithium ion cell structure is tight, separating difficulty is big, and physical method is difficult to reach the ideal effect.
In prior art, particularly adopt in the processing method that the refuse battery roasting is handled again, because positive electrode material, negative material and ionogen etc. in the disabled lithium ion cell are enclosed in the firm housing, and remaining capacity is still arranged in the battery, can be short-circuited during roasting and explosion generation danger.
Summary of the invention
The present invention seeks to the deficiency that exists in the above-mentioned prior art, provide that a kind of technology is simple, flow process is short, it is comprehensive to reclaim valuable metal, and can effectively solve the recovery method that roasting process produces valuable metal in the high disabled lithium ion cell of explosion problem, safety performance.
Purpose of the present invention is achieved through the following technical solutions.
The recovery method of valuable metal in the disabled lithium ion cell is characterized in that its technological process may further comprise the steps successively:
A. decompress(ion) is carried out in perforation on the disabled lithium ion cell shell;
B. the disabled lithium ion cell after will boring a hole is put into electrolytic solution and is carried out discharge process;
C. will carry out calcination process through the lithium ion battery of discharge process;
D. the lithium ion battery after the roasting is carried out fragmentation;
E. the lithium ion battery after the fragmentation is carried out magnetic separation, isolate magnetic thing and nonmagnetics;
F. the magnetic thing is carried out size classification;
G. nonmagnetics is carried out size classification.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention when it is characterized in that decompress(ion) is carried out in perforation on the disabled lithium ion cell shell, is to adopt the machinery awl to bore a hole on housing, and pore quantity is 1～10, bore dia 1～5mm.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention is characterized in that the electrolytic solution of the disabled lithium ion cell discharge usefulness after its perforation is to be selected from NaCl, NaOH, Na
2SO
4A kind of is electrolytical solution, and the weight percent concentration of electrolytic solution is 0.2%～5%.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention is characterized in that the lithium ion battery through discharge process is under 400 ℃～1000 ℃ temperature, calcination process 2～6 hours.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention is characterized in that it being that the lithium ion battery after the roasting is crushed to granularity is 0.5～5mm.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention is characterized in that lithium ion battery after the fragmentation carries out magnetic separation and isolates magnetic thing and nonmagnetics under the magneticstrength of 1000～10000Gs.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention, it is characterized in that it being that the magnetic thing is carried out size classification, obtain based on metallic iron and nickel, granularity is the coarse particles magnetic thing of 1-5mm and is the fine particle magnetic thing less than 1mm based on CoO, granularity.
The recovery method of valuable metal in the disabled lithium ion cell of the present invention, it is characterized in that it being that nonmagnetics is carried out size classification, obtain being the coarse particles nonmagnetics of 1-5mm and being fine particle nonmagnetics less than 1mm based on graphite, granularity based on metallic copper, granularity.
Method of the present invention, the employing disabled lithium ion cell is a raw material, owing in the disabled lithium ion cell remaining capacity is arranged still, the safety when guaranteeing roasting is at first carried out discharge stabilization to battery and is handled.With behind the battery machine bore spine perforation decompress(ion), be immersed at normal temperatures and carry out discharge process in the electrolyte solution earlier, removed the part organic electrolyte simultaneously.To discharge pretreated lithium ion battery at the roasting kiln roasting, and the temperature of roasting is between 400 ℃～1000 ℃.If organic electrolyte and binding agent in the too low battery of temperature are difficult to remove fully, material meeting sintering in the too high battery of temperature, low-melting metal can melt, and all can influence the effect of follow-up fragmentation and magnetic separation.Roasting process is 2～6 hours, removed the organic substance in the battery in the process fully, and metal is retained in also wherein all, and variation has taken place the thing that contains cobalt mutually.CoO is an antiferromagnetic substance, and its Neel temperature is 17 ℃, and CoO is a paramagnetism when this temperature, and susceptibility reaches maximum value.Therefore CoO is easy to be subjected to the effect in magnetic field at normal temperature, thereby separates with other non-magnetic substance.Roasting product is carried out magnetic separation after crusher in crushing, sub-elect magnetic thing and nonmagnetics.Magnetic thing and nonmagnetics are carried out size classification respectively, and coarse grain magnetic produce product are the secondary resources based on iron content and nickel, and particulate magnetic produce product are the higher-grade cobalt concentrate based on CoO, and CoO content is greater than 60%; The coarse grain nonmagnetics is the secondary resource based on copper, and the particulate nonmagnetics is the product based on graphite.Therefore, the valuable metal in the lithium ion battery obtains Separation and Recovery, and the rate of recovery of cobalt, copper, nickel, iron has realized the recycle of metals resources all greater than 96%.
The present invention is raw material with the disabled lithium ion cell, by steps such as roasting, magnetic separation and classifications, reclaims valuable metal wherein, realizes the recycle of cobalt metal, copper, nickel and iron.The present invention has the following advantages: (1) technology is simple, flow process is short, cost is low; (2) can at utmost reclaim valuable metal, the rate of recovery of cobalt, copper, nickel, iron is all greater than 96%, remarkable in economical benefits; (3) do not use acid and organic solvent in the process, flue gas is handled easily during roasting, no environment secondary pollution.
Description of drawings
Fig. 1 process flow sheet of the present invention.
Embodiment
The recovery method of valuable metal in the disabled lithium ion cell is through following steps: under (1) normal temperature the disabled lithium ion cell shell bored a hole with mechanical bore spine and carry out decompress(ion); Pore quantity is 1～10, bore dia 1～5mm; (2) lithium ion battery after will boring a hole is put into electrolytic solution and is carried out discharge process, blasts in heat-processed to prevent battery, removes the organic electrolyte in the part battery simultaneously; Electrolytic solution is NaCl, NaOH, the Na that selects for use ionogen soluble in water
2SO
4Solution, electrolyte weight percentage concentration are 0.2%～5%.(3) will carry out calcination process through the lithium ion battery of discharge process,, obtain suitable roasting product to remove organic substance fully; Its maturing temperature is 400 ℃～1000 ℃, and the time is 2～6 hours.(4) lithium ion battery after the roasting is carried out fragmentation; Because fragmentation is relatively easy after the roasting, described disintegrating apparatus can be selected jaw crusher, roller crusher etc. for use, and crushing granularity requirement is 0.5～5mm.(5) product after the fragmentation is carried out magnetic separation, separate magnetic thing and nonmagnetics; The magneticstrength of magnetic separation is 1000～10000Gs; Can select permanent magnetic separator, electromagnetic separator etc. for use.(6) the magnetic thing is carried out size classification; Obtain based on metallic iron and nickel, granularity be the coarse particles magnetic thing of 1-5mm and granularity for less than 1mm, based on the fine particle magnetic thing of CoO.(7) non-magnetic material is carried out classification, obtain based on metallic copper, granularity be the coarse particles nonmagnetics of 1-5mm and granularity for less than 1mm, based on the fine particle nonmagnetics of graphite.Product can be used as resource circulation utilization.
Embodiment 1:
The IRC18650 type notebook computer lithium ion battery of getting 4 joint inefficacies is a raw material, battery gross weight 184.25 grams, and main metal ingredient such as following table 1 in the battery:
Major metal composition in the lithium ion battery of table 1 embodiment 1
| Element | Co | Cu | Ni | Fe | Zn | Al | Mg | Li |
| Battery content (%) | 18.68 | 7.44 | 1.69 | 18.73 | 0.11 | 3.97 | 0.02 | 2.27 |
Battery after bore spine is worn 1 Φ 3mm hole in 0.2%NaOH electrolytic solution discharge process, with the battery after the discharge process with resistance furnace 680 ℃ of roastings 3 hours, organism is removed fully, obtain 153.38 the gram roasting products.The battery crusher in crushing of roasting after magnetic separation under the 2000Gs magneticstrength, obtains magnetic thing 104.11 grams and nonmagnetics 45.06 grams through permanent magnetic separator, and both obtain four kinds of products respectively after size classification.Product is through sampling analysis, and Chemical Composition is as follows respectively:
The coarse grain magnetic produce product major metal composition of table 2 embodiment 1:
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 2.02 | 1.55 | 7.07 | 78.02 | 5.49 | 0.83 |
Coarse grain magnetic produce product weigh 43.17 grams, and the rate of recovery of metallic iron reaches 97.59%, and nickel reaches 98.07%.
The particulate magnetic produce product major metal composition of table 3 embodiment 1:
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 54.89 | 0.32 | 0.13 | 0.71 | 6.16 | 5.61 |
Particulate magnetic produce product weigh 61.04 grams, and the rate of recovery of cobalt reaches 97.37%, and cobalt is mainly concentrated and is recovered in this product.Product detects through XRD, and cobalt exists with the CoO form.The CoO granularity is less than 1mm, and content is 69.8%, is high-grade cobalt metallurgical raw material.
The coarse grain nonmagnetics product major metal composition of table 4 embodiment 1:
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 0.71 | 42.12 | 0.088 | 0.058 | 12.73 | 0.84 |
Coarse grain nonmagnetics product weighs 29.46 grams, and the rate of recovery of metallic copper reaches 97.64%, is high-grade copper raw material.
The particulate nonmagnetics product major metal composition of table 5 embodiment 1:
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 3.39 | 4.23 | 0.052 | 0.084 | 3.23 | 2.32 |
Particulate nonmagnetics product 15.44 grams, this product can be recycled separately based on graphite.
Embodiment 2:
The rectangular lithium ion battery supporting with mobile phone is raw material, gets 4 batteries, weighs 109.57 grams, and main metal ingredient such as following table 6 in the battery do not contain Fe in the battery:
Major metal composition in the lithium ion battery of table 6 embodiment 2
| Element | Co | Cu | Ni | Fe | Al | Li |
| Battery content (%) | 19.90 | 10.03 | 0.72 | - | 6.22 | 2.27 |
Battery after bore spine is worn 5 Φ 1mm holes at 5%NaCl solution discharge 3h, 400 ℃ of roasting 6h, organism is removed fully, obtains 75.72 gram product of roastings.The battery crusher in crushing of roasting after magnetic separation under the 10000Gs magneticstrength, obtains magnetic thing 39.52 grams and nonmagnetics 36.18 grams through magnetic separator, and both obtain four kinds of products respectively after size classification.Product is through sampling analysis, and Chemical Composition is as follows respectively:
The coarse grain magnetic produce product major metal composition of table 7 embodiment 2
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 2.95 | 3.47 | 20.14 | - | 7.03 | 4.32 |
Coarse grain magnetic produce product weigh 3.81 grams, and the metallic nickel rate of recovery reaches 97.30%.
The particulate magnetic produce product major metal composition of table 8 embodiment 2
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 58.84 | 0.58 | 0.04 | - | 6.10 | 4.75 |
Particulate magnetic produce product weigh 35.6 grams, and the rate of recovery of cobalt reaches 96.07%.Product detects through XRD, and cobalt exists with the CoO form.The CoO granularity is less than 1mm, and content is 74.8%, is high-grade cobalt metallurgical raw material, is fit to further hydrometallurgy or pyrometallurgy and handles.
The coarse grain nonmagnetics product major metal composition of table 9 embodiment 2
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 0.78 | 66.49 | 0.08 | - | 17.53 | 1.85 |
Coarse grain nonmagnetics product weighs 15.90 grams, and the rate of recovery of metallic copper reaches 96.2%, is high-grade copper raw material.
The particulate nonmagnetics product major metal composition of table 10 embodiment 2
| Element | Co | Cu | Ni | Fe | Al | Li |
| Content (%) | 2.26 | 3.09 | 0.04 | 5.43 | 2.55 |
Particulate nonmagnetics product 20.25 gram, this product be based on graphite, also recyclable utilization.
This flow process reclaims the valuable metal in the lithium ion battery, and technology is simple, easy to operate, can make the valuable metal in the lithium ion battery obtain the very recycling of high level.
Claims (8)
1. the recovery method of valuable metal in the disabled lithium ion cell is characterized in that its technological process may further comprise the steps successively:
A. decompress(ion) is carried out in perforation on the disabled lithium ion cell shell;
B. the disabled lithium ion cell after will boring a hole is put into electrolytic solution and is carried out discharge process;
C. will carry out calcination process through the lithium ion battery of discharge process;
D. the lithium ion battery after the roasting is carried out fragmentation;
E. the lithium ion battery after the fragmentation is carried out magnetic separation, isolate magnetic thing and nonmagnetics;
F. the magnetic thing is carried out size classification;
G. nonmagnetics is carried out size classification.
2. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1, when it is characterized in that decompress(ion) is carried out in perforation on the disabled lithium ion cell shell, be to adopt the machinery awl to bore a hole on housing, pore quantity is 1～10, bore dia 1～5mm.
3. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1 is characterized in that the electrolytic solution of the disabled lithium ion cell discharge usefulness after its perforation is to be selected from NaCl, NaOH, Na
2SO
4A kind of is electrolytical solution, and the weight percent concentration of electrolytic solution is 0.2%～5%.
4. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1 is characterized in that the lithium ion battery through discharge process is under 400 ℃～1000 ℃ temperature, calcination process 2～6 hours.
5. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1 is characterized in that it being that the lithium ion battery after the roasting is crushed to granularity is 0.5～5mm.
6. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1 is characterized in that lithium ion battery after the fragmentation carries out magnetic separation and isolates magnetic thing and nonmagnetics under the magneticstrength of 1000～10000Gs.
7. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1, it is characterized in that it being that the magnetic thing is carried out size classification, obtain based on metallic iron and nickel, granularity is the coarse particles magnetic thing of 1-5mm and is the fine particle magnetic thing less than 1mm based on CoO, granularity.
8. the recovery method of valuable metal in the disabled lithium ion cell according to claim 1, it is characterized in that it being that nonmagnetics is carried out size classification, obtain being the coarse particles nonmagnetics of 1-5mm and being fine particle nonmagnetics less than 1mm based on graphite, granularity based on metallic copper, granularity.
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| CNB2007101078376A CN100449011C (en) | 2007-05-18 | 2007-05-18 | Method for recovering valuable metal in invalid lithium ion battery |
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| CNB2007101078376A CN100449011C (en) | 2007-05-18 | 2007-05-18 | Method for recovering valuable metal in invalid lithium ion battery |
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| CN100449011C true CN100449011C (en) | 2009-01-07 |
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| CN101519726B (en) * | 2009-04-16 | 2011-01-05 | 北京矿冶研究总院 | Method for directly roasting and treating waste lithium ion battery and recycling valuable metal |
| CN102029283B (en) * | 2010-02-05 | 2012-07-25 | 伟翔环保科技发展(上海)有限公司 | Recycling separation system of lithium battery component materials |
| CN102009054A (en) * | 2010-10-18 | 2011-04-13 | 华东交通大学 | Novel process for efficiently crushing waste lithium ion battery |
| JP5651462B2 (en) * | 2010-12-27 | 2015-01-14 | Ｄｏｗａエコシステム株式会社 | Method of recovering valuable material from lithium ion secondary battery and recovered material containing valuable material |
| CN102324592A (en) * | 2011-07-27 | 2012-01-18 | 上海交通大学 | Method for recovering cadmium, ferrum, nickel and cobalt from used nickel-cadmium battery |
| CN103427096A (en) * | 2012-05-14 | 2013-12-04 | 深圳市艾博尔新能源有限公司 | Disposal method and apparatus of waste lithium battery |
| CN102856610A (en) * | 2012-08-28 | 2013-01-02 | 奇瑞汽车股份有限公司 | Pretreatment method for recycling scrap lithium ion battery |
| CN103682510B (en) * | 2013-12-03 | 2015-11-18 | 广东电网公司电力科学研究院 | For electrolyte and the charging method of waste lithium cell electric discharge |
| CN104593606B (en) * | 2015-01-14 | 2016-08-17 | 上海交通大学 | Waste and old cobalt acid lithium ion battery defective positive and negative pole material method of resource |
| CN105671316A (en) * | 2016-03-18 | 2016-06-15 | 江西理工大学 | Method for recovering valuable metals from waste lithium-ion power batteries |
| CN106058358A (en) * | 2016-08-17 | 2016-10-26 | 合肥国轩高科动力能源有限公司 | Discharge method of improving discharge degree of waste lithium ion battery |
| CN107492695A (en) * | 2017-07-17 | 2017-12-19 | 中航锂电（洛阳）有限公司 | The separation method of positive/negative plate in a kind of lithium ion battery removal process |
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| KR20210124305A (en) * | 2019-02-08 | 2021-10-14 | 블루 솔루션즈 | Method for Extracting Lithium from Electric Batteries Containing Solid Metal Lithium |
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| CN110760685A (en) * | 2019-12-06 | 2020-02-07 | 江西理工大学 | Method for recovering retired lithium ion battery anode material |
| JP7355713B2 (en) * | 2020-07-16 | 2023-10-03 | 株式会社神戸製鋼所 | Pretreatment method for recovering valuable elements from secondary batteries and method for recovering valuable elements from secondary batteries |
| CN112103588B (en) * | 2020-09-03 | 2022-04-05 | 江西省中子能源有限公司 | Lithium ion battery recovery processing method |
| CN113083848A (en) * | 2021-03-10 | 2021-07-09 | 深圳清研装备科技有限公司 | Sorting and recycling method for positive and negative electrode materials of waste lithium iron phosphate batteries |
| CN113151670B (en) * | 2021-04-28 | 2023-06-13 | 四川省有色冶金研究院有限公司 | Method for recycling invalid lithium battery |
| CN115637329B (en) * | 2022-12-23 | 2023-03-31 | 湖南金阳烯碳新材料股份有限公司 | Recovery process of lithium ion battery negative electrode material |
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