CN110592384A - Novel process for simultaneously recovering valuable metal and iron from mixed type waste lithium ion battery - Google Patents

Novel process for simultaneously recovering valuable metal and iron from mixed type waste lithium ion battery Download PDF

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CN110592384A
CN110592384A CN201910994322.5A CN201910994322A CN110592384A CN 110592384 A CN110592384 A CN 110592384A CN 201910994322 A CN201910994322 A CN 201910994322A CN 110592384 A CN110592384 A CN 110592384A
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leaching
iron
waste lithium
acid
lithium ion
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CN110592384B (en
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陈湘萍
李佳竺
李静
何志强
何路凤
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/005—Preliminary treatment of scrap
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00—Obtaining manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • 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
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

A novel process for simultaneously recovering valuable metals and iron from mixed waste lithium ion batteries comprises the following steps; s1, preprocessing: carrying out pretreatment procedures such as discharging, disassembling and stripping on the waste lithium battery; s2, leaching: leaching the stripped anode material of the waste lithium ion battery to obtain leached materialThe liquid contains Mn2+、Ni2+、Co2+、Li+The main metal in the leaching residue is iron; s3, adjusting the proportion of metal ions in the leaching solution, and then precipitating, grinding and calcining the metal ions to obtain LiNi1/3Co1/3Mn1/3O2A material; s4, FePO obtained in step S24Adding lithium source into the residue to prepare LiFePO4A material. The invention has the advantages of high selectivity, wide application range and high recovery rate.

Description

Novel process for simultaneously recovering valuable metal and iron from mixed type waste lithium ion battery
Technical Field
The invention relates to the technical field of waste lithium batteries, in particular to a novel process for simultaneously recovering valuable metals and iron from mixed type waste lithium ion batteries.
Background
In recent years, as the output of electronic devices and mobile devices such as vehicles is increasing, the demand for lithium batteries is also increasing, and the service life of lithium ion batteries is limited, so that the number of waste lithium batteries is rapidly increasing. China is a large population country and is one of the main bodies of battery production and consumption in the world without any doubt, and according to statistics, due to the development of the electric vehicle industry, the total amount of the waste lithium ion batteries in the world is estimated to exceed 250 hundred million and the weight of the waste lithium ion batteries reaches 50 million tons in 2020.
The lithium ion battery contains various metal substances such as cobalt, lithium, nickel, manganese and the like, wherein the cobalt content is more as high as 5-20%, and far exceeds the metal content in average ore. Therefore, if the discarded lithium batteries are discarded without being treated, not only a great deal of valuable metals are wasted, but also potential hazards (such as heavy metals, harmful electrolytic pollution liquid and the like) can be caused to the ecological environment and human health. If the valuable metals in the waste lithium batteries can be efficiently and environmentally recovered, a large amount of valuable metals can be recovered, considerable economic and resource benefits are generated, and potential hazards to the ecological environment and human health can be reduced or avoided.
At present, a great deal of research is carried out on the recovery of waste lithium batteries by a plurality of researchers at home and abroad, and the recovery method of the waste lithium battery anode material powder obtained after pretreatment mainly comprises a pyrogenic method, a wet method, a bioleaching method and the like. But the pyrogenic process has high energy consumption and long bioleaching period, and is difficult to meet industrial application. The wet leaching method has high efficiency, large treatment capacity and high resource recovery rate. At present, the wet leaching mainly takes inorganic acid and reducing agent as main components. But ammonia system leaching can cause ammonia nitrogen pollution and increase subsequent treatment cost.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a novel process for simultaneously recovering valuable metals and iron from mixed waste lithium ion batteries, and the novel process has the advantages of high selectivity, wide application range and high recovery rate.
In order to achieve the purpose, the invention adopts the technical scheme that:
a novel process for simultaneously recovering valuable metals and iron from mixed waste lithium ion batteries comprises the following steps;
s1, preprocessing: carrying out pretreatment procedures such as discharging, disassembling and stripping on the waste lithium battery;
s2, leaching: leaching the stripped anode material of the waste lithium ion battery to obtain a leaching solution containing Mn2+、Ni2+、Co2+、Li+The main metal in the leaching residue is iron;
s3, adjusting the proportion of metal ions in the leaching solution to be that the metal ions are precipitated, ground and calcined to obtain LiNi1/3Co1/3Mn1/3O2A material;
s4, FePO obtained in step S24Adding lithium source into the residue to prepare LiFePO4A material.
In the leaching process of S2, sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, citric acid or oxalic acid is used as leaching acid, hydrogen peroxide, sodium thiosulfate, ascorbic acid or sucrose is used as a reducing agent, and the waste lithium ion battery anode material is leached under the conditions that the temperature is 20-80 ℃, the time is 10-80 min, the liquid-solid ratio of the leaching acid to the anode material is 5-60 mL/g, the acid concentration is 0.5-5 mol/L, and the dosage concentration of the reducing agent is 1-10%.
And adding Mn, Ni, Co and Li salts into the S3 to adjust the metal ion ratio to Li to Ni to Co to Mn to be 3 to 1, then precipitating the metal ions, recycling the acid used for leaching, and calcining at 500-1000 ℃.
And adding a lithium source into the S4, adjusting the ratio of iron to lithium to be 1:1, and calcining at 500-1000 ℃.
The invention has the beneficial effects that:
the battery takes waste lithium batteries as raw materials, anode powder is taken as the raw materials after pretreatment for leaching, the leaching is carried out and then filtration is carried out, the leaching solution contains four metals of Mn, Ni, Co and Li, and the leaching residue is a compound of iron. Regulating the ratio of metal ions in the leaching solution, adding precipitated metal ions, reusing the obtained acid in the leaching step, calcining the precipitated powder, and grinding to synthesize LiNi1/3Co1/3Mn1/3O2A material. Leached residue FePO4Adding a lithium source, fully mixing, calcining and grinding to obtain LiFePO4A material.
Compared with the prior art, the invention intensively discusses the waste cathode material (namely LiCoO) from the most complicated waste LIBs at present2，LiMn2O4，LiFePO4，LiNixCoyMnzO2) The different metals are recovered by selective leaching, coprecipitation and material preparation. For the recovery of different metals which will eventually stabilize as LiFePO4And LiNi1/3Co1/3Mn1/3O2The new cathode material of (1). Such a recovery process may provide an alternative to different metal recoveries, with an emphasis on a balance between efficiency, selectivity, simplicity and applicability.
Description of the drawings:
fig. 1 is a schematic diagram of the electrochemical performance of the waste LIB regenerated cathode material of the present invention.
FIG. 2 is a schematic flow chart of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
The novel process for simultaneously recovering valuable metals and iron from the mixed waste lithium ion battery comprises the following steps:
1kg of waste lithium battery is taken and subjected to pretreatment procedures such as discharging, disassembling and stripping to obtain 420g of cathode material, wherein the detailed percentages of Co, Li, Mn, Ni and Fe are as follows: 17.2%, 5.4%, 16.1%, 6.5% and 8.6%.
And leaching the anode material at 40 ℃ for 40min, wherein the liquid-solid ratio is 30mL/g, the acid concentration is 2mol/L, and the dosage of the reducing agent is 4%. And filtering after leaching to obtain a mixed solution of Co, Li, Mn and Ni and iron compound residues. Regulating the content of metal ions in the leaching solution, then precipitating the metal ions, recycling the acid, then calcining the precipitate at 600 ℃, and grinding to obtain the synthetic LiNi1/3Co1/3Mn1/3O2A material. Adding a lithium source into the iron compound residue obtained after leaching, fully mixing, calcining at 550 ℃, and grinding to obtain LiFePO4A material.
Example 2
The novel process for simultaneously recovering valuable metals and iron from the mixed waste lithium ion battery comprises the following steps:
taking 3kg of waste lithium battery, and carrying out pretreatment procedures such as discharging, disassembling, stripping and the like to obtain 1.26kg of the cathode material, wherein the detailed percentages of Co, Li, Mn, Ni and Fe are as follows: 17.2%, 5.4%, 16.1%, 6.5% and 8.6%.
And leaching the anode material at 50 ℃ for 80min, wherein the liquid-solid ratio is 30mL/g, the acid concentration is 1mol/L, and the dosage of the reducing agent is 2%. And filtering after leaching to obtain a mixed solution of Co, Li, Mn and Ni and iron compound residues. Regulating the content of metal ions in the leaching solution, then precipitating the metal ions, recycling the acid, then calcining the precipitate at 900 ℃, and grinding to obtain the synthetic LiNi1/3Co1/3Mn1/3O2A material. FePO obtained after leaching4Adding a lithium source into the residue, fully mixing, calcining at 800 ℃, and grinding to obtain LiFePO4A material.
Example 3
The novel process for simultaneously recovering valuable metals and iron from the mixed waste lithium ion battery comprises the following steps:
taking 0.5kg of waste lithium battery, and carrying out pretreatment procedures such as discharging, disassembling, stripping and the like to obtain 210g of the cathode material, wherein the detailed percentages of Co, Li, Mn, Ni and Fe are as follows: 17.2%, 5.4%, 16.1%, 6.5% and 8.6%.
And leaching the anode material at 80 ℃ for 50min, wherein the liquid-solid ratio is 30mL/g, the acid concentration is 6mol/L, and the dosage of the reducing agent is 8%. And filtering after leaching to obtain a mixed solution of Co, Li, Mn and Ni and iron compound residues. Regulating the content of metal ions in the leaching solution, then precipitating the metal ions, recycling the acid, then calcining the precipitate at 800 ℃, and grinding to obtain the synthetic LiNi1/3Co1/3Mn1/3O2A material. Adding a lithium source into the iron compound residue obtained after leaching, fully mixing, calcining at 700 ℃, and grinding to obtain LiFePO4A material.
As shown in fig. 1: electrochemical performance of the waste LIB regenerated cathode material. Re-NCM: (A) electrochemical performance and discharge curve of the initial charge of the regenerated NCM cathode material at different calcination temperatures of 700 ℃, 800 ℃ and 900 ℃ (a)1) Rate capability (A)2) And cycle performance (A)3) (ii) a Re-LFP: (B) electrochemical performance curves for initial charging and discharging of the regenerated NCM cathode material at different calcination temperatures at 600 ℃, 700 ℃ and 800 ℃ (B)1) Rate capability (B)2) And cycle performance (B)3)。
As shown in fig. 2: comprises the following steps;
s1, preprocessing: carrying out pretreatment procedures such as discharging, disassembling and stripping on the waste lithium battery;
s2, leaching: leaching the stripped anode material of the waste lithium ion battery to obtain a leaching solution containing Mn2+、Ni2+、Co2+、Li+The main metal in the leaching residue is iron;
s3, adjusting the proportion of metal ions in the leaching solution to be that the metal ions are precipitated, ground and calcined to obtain LiNi1/3Co1/3Mn1/3O2A material;
s4, obtained step S2FePO of4Adding lithium source into the residue to prepare LiFePO4A material.

Claims (4)

1. A novel process for simultaneously recovering valuable metals and iron from mixed waste lithium ion batteries is characterized by comprising the following steps;
s1, preprocessing: carrying out pretreatment procedures such as discharging, disassembling and stripping on the waste lithium battery;
s2, leaching: leaching the stripped anode material of the waste lithium ion battery to obtain a leaching solution containing Mn2+、Ni2+、Co2+、Li+The main metal in the leaching residue is iron;
s3, adjusting the proportion of metal ions in the leaching solution, and then precipitating, grinding and calcining the metal ions to obtain LiNi1/3Co1/ 3Mn1/3O2A material;
s4, FePO obtained in step S24Adding lithium source into the residue to prepare LiFePO4A material.
2. The novel process for simultaneously recovering valuable metals and iron from mixed type waste lithium ion batteries according to claim 1, characterized in that in the leaching process of S2, sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, citric acid or oxalic acid is used as leaching acid, hydrogen peroxide, sodium thiosulfate, ascorbic acid or sucrose is used as a reducing agent, and the waste lithium ion battery anode material is leached under the conditions that the temperature is 20-80 ℃, the time is 10-80 min, the liquid-solid ratio of the leaching acid to the anode material is 5-60 mL/g, the acid concentration is 0.5-5 mol/L, and the reducing agent dosage concentration is 1-10%.
3. The novel process for simultaneously recovering valuable metals and iron from mixed waste lithium ion batteries according to claim 1 is characterized in that Mn, Ni, Co and Li salts are added into S3 to adjust the metal ion ratio to be Li: Ni: Co: Mn: 3:1:1:1, the metal ions are precipitated, acid used for leaching can be recycled, and the process is calcined at 500-1000 ℃.
4. The novel process for simultaneously recovering valuable metals and iron from mixed type waste lithium ion batteries according to claim 1, characterized in that S4 is added with a lithium source, the ratio of iron to lithium is adjusted to 1:1, and the calcination is carried out at 500-1000 ℃.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111987381A (en) * 2020-08-25 2020-11-24 长沙矿冶研究院有限责任公司 Method for synchronously defluorinating valuable metals leached from waste lithium ion batteries
CN112374553A (en) * 2020-11-13 2021-02-19 东北大学 Method for recycling and regenerating retired lithium ion battery anode material
CN113046559A (en) * 2021-03-05 2021-06-29 华东理工大学 Method for recovering lithium, cobalt, nickel and manganese from retired lithium ion battery anode material
CN113353909A (en) * 2021-05-31 2021-09-07 蜂巢能源科技有限公司 Method for preparing lithium iron phosphate cathode material by utilizing recovered lithium
CN113943867A (en) * 2021-10-22 2022-01-18 江门市恒创睿能环保科技有限公司 Method for leaching cobalt and lithium from waste lithium cobalt oxide battery
CN114291854A (en) * 2021-12-30 2022-04-08 中南大学 Treatment method for recycling waste battery anode material

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CN106654205A (en) * 2016-12-19 2017-05-10 天齐锂业股份有限公司 Method for preparing ternary cathode material precursor by using waste lithium battery material

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111987381A (en) * 2020-08-25 2020-11-24 长沙矿冶研究院有限责任公司 Method for synchronously defluorinating valuable metals leached from waste lithium ion batteries
CN112374553A (en) * 2020-11-13 2021-02-19 东北大学 Method for recycling and regenerating retired lithium ion battery anode material
CN113046559A (en) * 2021-03-05 2021-06-29 华东理工大学 Method for recovering lithium, cobalt, nickel and manganese from retired lithium ion battery anode material
CN113046559B (en) * 2021-03-05 2022-03-01 华东理工大学 Method for recovering lithium, cobalt, nickel and manganese from retired lithium ion battery anode material
CN113353909A (en) * 2021-05-31 2021-09-07 蜂巢能源科技有限公司 Method for preparing lithium iron phosphate cathode material by utilizing recovered lithium
CN113353909B (en) * 2021-05-31 2024-03-26 蜂巢能源科技有限公司 Method for preparing lithium iron phosphate positive electrode material by utilizing recovered lithium
CN113943867A (en) * 2021-10-22 2022-01-18 江门市恒创睿能环保科技有限公司 Method for leaching cobalt and lithium from waste lithium cobalt oxide battery
CN114291854A (en) * 2021-12-30 2022-04-08 中南大学 Treatment method for recycling waste battery anode material

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