CN112626344A - Method for recovering Li and Co in lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid - Google Patents
Method for recovering Li and Co in lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid Download PDFInfo
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- CN112626344A CN112626344A CN202011484797.9A CN202011484797A CN112626344A CN 112626344 A CN112626344 A CN 112626344A CN 202011484797 A CN202011484797 A CN 202011484797A CN 112626344 A CN112626344 A CN 112626344A
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- Prior art keywords
- polyethylene glycol
- dicarboxylic acid
- lithium
- glycol dicarboxylic
- positive electrode
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Classifications
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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
- 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
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention relates to a method for recovering Li and Co in a lithium battery anode material by using polyethylene glycol dicarboxylic acid, which specifically comprises the following steps: mixing polyethylene glycol dicarboxylic acid with a lithium ion battery anode material, heating for a complex reaction, adding a cobalt precipitator and a lithium precipitator after the reaction is completed, and performing solid-liquid separation to obtain a solid containing Li and Co. The method uses the polyethylene glycol dicarboxylic acid as a metal recycling agent to extract metal elements such as Li, Co and the like, has mild reaction conditions, does not involve high temperature and high pressure, has short time consumption and high metal recycling rate, does not introduce other toxic and harmful substances, can recycle the polyethylene glycol dicarboxylic acid, is green and environment-friendly, has simple and easily controlled operation and low cost, and can be suitable for large-scale production operation.
Description
Technical Field
The invention belongs to the technical field of processing non-ore raw materials (such as waste materials) to produce non-ferrous metals or compounds thereof, and relates to a method for recovering Li and Co in a lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid.
Background
In recent years, lithium ion batteries have been widely used in the fields of electrochemical power sources, mobile electronic devices, electric vehicles, and the like because of their high energy density and power density. Typical lithium ion battery electrodes comprise a lithium metal oxide positive electrode material and a graphite negative electrode material, with the mainstream positive active material being LiCoO2And doping Ni, Mn, Al and other ions can reduce the cost of the anode material of the lithium ion battery to a certain extent. The mass percentage of Li and Co in the waste lithium ion battery can reach 10-30%, and the recovery of the two metals in the lithium ion battery is particularly important in recent years with the continuous rising of the price of Co raw materials.
The recovery process of metal elements in lithium ion batteries in the current market is mainly divided into three types: hydrometallurgical, pyrometallurgical and biodegradable techniques. The hydrometallurgical recovery is high, however, many complicated pretreatments are involved, the mineral acids used are highly corrosive, require complicated post-separation procedures and release large amounts of Cl2、SOx、NOxGas harmful to air is obtained; organic acid in the thermal metallurgy method can not be used independently generally, and can play a role only by adding a proper amount of reducing aid, so that the thermal metallurgy method has high dependence on raw materials; but the biodegradation technology has low recovery rate and more complex process. Therefore, the development of the technology for recovering the metal in the lithium ion battery electrode material, which is environment-friendly, efficient, simple to operate and easy to control, has important significance in the scientific research community and the industrial community.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for recovering Li and Co in a lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid, aiming at the defects in the prior art, and the method has the advantages of low cost, environmental friendliness, safety, reliability and simplicity in operation.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the method for recovering Li and Co in the lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid comprises the following steps: mixing polyethylene glycol dicarboxylic acid with a lithium ion battery anode material, heating for a complex reaction, adding a cobalt precipitator and a lithium precipitator after the reaction is completed, and performing solid-liquid separation to obtain a solid containing Li and Co.
According to the scheme, the polymerization degree of the polyethylene glycol dicarboxylic acid is 200-1000.
According to the scheme, the active ingredient in the lithium ion battery positive electrode material is LiCoO2，LiNi0.5Mn0.3Co0.2O2，LiNi0.6Mn0.2Co0.2O2，LiNi0.8Mn0.1Co0.1O2The mass ratio of active ingredients to polyethylene glycol dicarboxylic acid in the lithium ion battery anode material is 0.01-0.02: 1.
according to the scheme, the temperature of the complex reaction is 100-150 ℃, and the time of the complex reaction is 30-300 min. Under the condition of low reaction temperature, the reaction time needs to be prolonged for ensuring the complete reaction, otherwise, the reaction time is short when the reaction temperature is high.
The preferable complexing reaction temperature is 120-150 ℃, and the complexing time is 3-5 h.
According to the scheme, the cobalt precipitator is oxalate. Preferably sodium oxalate or potassium oxalate, and the cobalt precipitator is added in excess according to the theoretical dosage of the reaction with lithium cobaltate in the lithium ion battery anode material, wherein the dosage is 1.2-1.4 times of the theoretical dosage.
According to the scheme, the lithium precipitator is carbonate or phosphate. Preferably sodium carbonate or sodium phosphate, and the lithium precipitator is added in excess according to the theoretical dosage of reaction with lithium cobaltate in the lithium ion battery anode material, wherein the dosage is 1.2-1.4 times of the theoretical dosage.
The lithium ion battery anode material is mainly composed of lithium cobaltate as an active material, and polyethylene glycol dicarboxylic acid with a proper polymerization degree can reduce and complex trivalent cobalt ions and lithium ions in the lithium cobaltate into the polyethylene glycol dicarboxylic acid at a lower temperature in a shorter time, and the reaction is complete, and the recovery efficiency is high when the polyethylene glycol dicarboxylic acid is matched with a precipitator. The solid product containing Li and Co recovered by the method can be directly utilized or can be purified and utilized.
The invention has the beneficial effects that: the method uses polyethylene glycol dicarboxylic acid as a metal recycling agent, and uses hydroxyl, carboxyl, carbonyl and ether bonds contained in the polyethylene glycol dicarboxylic acid as active centers to perform complexation with Li and Co metal atoms in an electrode material of a lithium ion battery, so that the anode material of the lithium ion battery is decomposed, and metal elements such as Li, Co and the like in the anode material are extracted.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described in detail with reference to the following examples.
In the embodiment of the invention, the concentration of metal ions is tested by adopting an ICP-OES (inductively coupled plasma emission spectrometer), and the model is Agilent 730.
Example 1
A method for recovering Li and Co in a lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid specifically comprises the following steps: polyethylene glycol dicarboxylic acid (polymerization degree of 250) and lithium ion battery positive electrode material (obtained by disassembling battery and recycling, and active ingredient is LiCoO)2) Mixing, wherein the mass ratio of the active ingredients of the lithium ion battery positive electrode material to the polyethylene glycol dicarboxylic acid is 0.02: 1, heating to 150 ℃ for complex reaction, stirring at 600 revolutions per minute for 5 minutes, digesting part of complex reactants after the reaction is finished, and testing the content of metal ions in the reactants by ICP-OES, wherein the results show that the recovery rate of Li ions is 43 percent and the recovery rate of Co ions is 27 percent. Then, the rest of the complex reactant is added with excessive cobalt precipitator (sodium oxalate, the adding amount is 1.2 times of the theoretical dosage) and then added with lithium for precipitationPrecipitating agent (sodium carbonate, the addition amount is 1.2 times of theoretical dosage), precipitating Co and Li, and performing solid-liquid separation to obtain solid containing Li and Co.
Example 2
Li and Co were recovered from a positive electrode material for a lithium battery by a method similar to that of example 1, except that the time of the complexation reaction was 15 minutes, the recovery rate of Li ions was 71.1% and the recovery rate of Co ions was 64.4% as measured after the complexation reaction.
Example 3
Li and Co in the positive electrode material of a lithium battery were recovered by a method similar to that of example 1, except that the time of the complexation reaction was 30 minutes, the recovery rate of Li ions was 91.4% and the recovery rate of Co ions was 92.4% as measured after the complexation reaction.
Example 4
Li and Co in the positive electrode material of a lithium battery were recovered by a method similar to that of example 1, except that the time of the complexation reaction was 45 minutes, the recovery rate of Li ions was 92.7% and the recovery rate of Co ions was 99.9% as measured after the complexation reaction.
Example 5
Li and Co were recovered from the positive electrode material for lithium batteries by a method similar to that of example 1, except that the time of the complexation reaction was 60 minutes, the recovery rate of Li ions after the complexation reaction was 99.9%, and the recovery rate of Co ions was 93.0%.
Example 6
Li and Co in the positive electrode material of the lithium battery were recovered by a method similar to that of example 1, except that the time of the complexation reaction was 120 minutes, and the recovery rate of Li ions after the complexation reaction was found to be nearly 97.9%, and the recovery rate of Co ions was found to be nearly 100%.
Example 7
The method similar to example 1 is adopted to recover Li and Co in the lithium battery anode material, except that the complexation reaction time is 180 minutes, the reaction is complete (lithium cobaltate is black powder, polyethylene glycol dicarboxylic acid is transparent liquid, and the reaction can be roughly judged to be complete if the black powder in the system completely disappears), the recovery rate of Li ions is close to 100% after complexation reaction, and the recovery rate of Co ions is close to 100%.
Example 8
Polyethylene glycol dicarboxylic acid (polymerization degree of 250) and lithium ion battery positive electrode material (obtained by disassembling battery and recycling, and active ingredient is LiCoO)2) Mixing, wherein the mass ratio of the active ingredients of the lithium ion battery positive electrode material to the polyethylene glycol dicarboxylic acid is 0.02: 1, heating to 100 ℃ for complex reaction, stirring at 600 revolutions per minute for 300 minutes, taking a small amount of complex reactant after the reaction is finished for digestion treatment, and testing by ICP-OES, wherein the results show that the recovery rates of Li ions and Co ions are 39.6% and 55.3% respectively. And then adding excessive cobalt precipitator (sodium oxalate, the adding amount is 1.2 times of the theoretical amount) and lithium precipitator (sodium carbonate, the adding amount is 1.2 times of the theoretical amount) into the residual complex reactant, precipitating Co and Li, and carrying out solid-liquid separation to obtain a solid containing Li and Co.
Example 9
Polyethylene glycol dicarboxylic acid (polymerization degree of 250) and lithium ion battery positive electrode material (obtained by disassembling battery and recycling, and active ingredient is LiCoO)2) Mixing, wherein the mass ratio of the active ingredients of the lithium ion battery positive electrode material to the polyethylene glycol dicarboxylic acid is 0.02: 1, heating to 120 ℃ for complex reaction, stirring at 600 revolutions per minute for 300 minutes, taking a small amount of complex reactant after the reaction is finished for digestion treatment, and testing by ICP-OES, wherein the results show that the recovery rates of Li ions and Co ions are 99.4% and 96.8% respectively. And then adding excessive cobalt precipitator (sodium oxalate, the adding amount is 1.2 times of the theoretical amount) and lithium precipitator (sodium carbonate, the adding amount is 1.2 times of the theoretical amount) into the residual complex reactant, precipitating Co and Li, and carrying out solid-liquid separation to obtain a solid containing Li and Co.
Example 10
Polyethylene glycol dicarboxylic acid (polymerization degree of 600) and lithium ion battery positive electrode material (obtained by disassembling battery and recycling, and active ingredient is LiCoO2) Mixing, wherein the mass ratio of the active ingredients of the lithium ion battery positive electrode material to the polyethylene glycol dicarboxylic acid is 0.02: 1, heating to 150 ℃ for complex reaction, stirring at 600 revolutions per minute for 300 minutes, and taking a small amount of complex reactant after the reaction is finishedDigestion treatment and ICP-OES test show that the recovery rates of Li ions and Co ions are 71.9% and 63.8%, respectively, and then excess cobalt precipitator (sodium oxalate, the addition amount is 1.2 times of the theoretical amount) and lithium precipitator (sodium carbonate, the addition amount is 1.2 times of the theoretical amount) are added into the residual complex reactant, Co and Li are precipitated, and solid-liquid separation is carried out to obtain solid containing Li and Co.
Claims (9)
1. A method for recovering Li and Co in a lithium battery positive electrode material by using polyethylene glycol dicarboxylic acid is characterized by comprising the following steps: mixing polyethylene glycol dicarboxylic acid with a lithium ion battery anode material, heating for a complex reaction, adding a cobalt precipitator and a lithium precipitator after the reaction is completed, and performing solid-liquid separation to obtain a solid containing Li and Co.
2. The method for recovering Li and Co in the lithium battery cathode material by using polyethylene glycol dicarboxylic acid as claimed in claim 1, wherein the polymerization degree of the polyethylene glycol dicarboxylic acid is 200-1000.
3. The method for recovering Li and Co in a positive electrode material of a lithium battery using polyethylene glycol dicarboxylic acid according to claim 1, wherein the active ingredient in the positive electrode material of the lithium ion battery is LiCoO2，LiNi0.5Mn0.3Co0.2O2，LiNi0.6Mn0.2Co0.2O2，LiNi0.8Mn0.1Co0.1O2The mass ratio of active ingredients to polyethylene glycol dicarboxylic acid in the lithium ion battery anode material is 0.01-0.02: 1.
4. the method as claimed in claim 1, wherein the temperature of the complexation reaction is 100-150 ℃ and the time of the complexation reaction is 30-300 min.
5. The method for recovering Li and Co in the lithium battery anode material by using the polyethylene glycol dicarboxylic acid as claimed in claim 4, wherein the temperature of the complexation reaction is 120-150 ℃, and the complexation time is 3-5 h.
6. The method for recovering Li and Co in a positive electrode material of a lithium battery using polyethylene glycol dicarboxylic acid according to claim 1, wherein the cobalt precipitant is oxalate.
7. The method for recovering Li and Co in the positive electrode material of the lithium battery by using the polyethylene glycol dicarboxylic acid as claimed in claim 6, wherein the cobalt precipitant is sodium oxalate or potassium oxalate, and the cobalt precipitant is added in excess according to a theoretical amount of the lithium cobaltate in the positive electrode material of the lithium battery, and the amount of the cobalt precipitant is 1.2-1.4 times of the theoretical amount.
8. The method for recovering Li and Co in a positive electrode material for a lithium battery using polyethylene glycol dicarboxylic acid according to claim 1, wherein the lithium precipitant is carbonate or phosphate.
9. The method for recovering Li and Co in the positive electrode material of the lithium battery by using the polyethylene glycol dicarboxylic acid according to claim 8, wherein the lithium precipitant is sodium carbonate or sodium phosphate, and the lithium precipitant is added in an excess amount of 1.2 to 1.4 times of a theoretical amount of the lithium cobaltate in the positive electrode material of the lithium ion battery according to the theoretical amount of the lithium cobaltate in the reaction.
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Cited By (2)
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| CN114421045A (en) * | 2022-03-10 | 2022-04-29 | 西安西热锅炉环保工程有限公司 | Method for closed-loop recovery of retired power battery by using low-viscosity green solvent |
| CN115196689A (en) * | 2022-08-22 | 2022-10-18 | 武汉旭清工程技术有限公司 | Compound solvent for producing cobaltosic oxide from cobalt-containing positive electrode material of waste lithium battery and using method |
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Application publication date: 20210409 |