CN111924816A - Method for recovering electrolyte of waste lithium ion battery - Google Patents

Method for recovering electrolyte of waste lithium ion battery Download PDF

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Publication number
CN111924816A
CN111924816A CN202010629017.9A CN202010629017A CN111924816A CN 111924816 A CN111924816 A CN 111924816A CN 202010629017 A CN202010629017 A CN 202010629017A CN 111924816 A CN111924816 A CN 111924816A
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filtrate
filter residue
electrolyte
carbonate
filtering
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徐浩
史靖辉
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Qujing Huaxiang Technology Co ltd
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Qujing Huaxiang Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/37—Phosphates of heavy metals
    • C01B25/375—Phosphates of heavy metals of iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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
    • 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 provides a method for recovering electrolyte of a waste lithium ion battery, which comprises the following steps: (1) obtaining electrolyte of a waste lithium ion battery, adding an extracting agent into the electrolyte for extraction, adding a calcium compound into the obtained lower-layer liquid, stirring, and filtering to obtain a first filtrate and a first filter residue; washing the first filter residue with water for multiple times to obtain a second filtrate and a second filter residue; (2) adding EDTA to the first filtrate to remove calcium, filtering to obtain a third filtrate, adjusting the pH of the third filtrate to 1-2, adding an iron source, heating at 60-90 ℃ for 1-4h, and filtering to obtain a third filter residue and a fourth filtrate; washing the third filter residue for multiple times to obtain high-purity iron phosphate; (3) mixing the second filtrate and the fourth filtrate, adding carbonate, heating to 80-100 ℃, heating, and filtering to obtain fourth filter residue; and washing the fourth filter residue for multiple times to obtain high-purity lithium carbonate. The method is simple, reasonable and easy to operate, and environment-friendly.

Description

Method for recovering electrolyte of waste lithium ion battery
Technical Field
The invention relates to the technical field of comprehensive utilization of waste resources, in particular to a method for recovering electrolyte of a waste lithium ion battery.
Background
Lithium ion batteries using lithium iron phosphate, ternary positive electrode materials (such as nickel cobalt lithium manganate) and the like as positive electrode materials are widely used as power batteries of electric tools such as electric vehicles and the like, and accordingly, the number of waste lithium ion batteries is increasing. Therefore, the method has double meanings of economic value and social benefit for effectively recycling and reusing the waste lithium ion battery.
At present, the method for recycling the waste lithium ion battery mainly aims at the anode material, and the recycling of the electrolyte is less. Among them, lithium hexafluorophosphate is an important component of the current lithium ion battery electrolyte, and accounts for about 43% of the total cost of the electrolyte. Therefore, the method is particularly important for recovering the waste lithium ion battery electrolyte containing lithium hexafluorophosphate.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for recovering electrolyte of waste lithium ion batteries, wherein high-purity iron phosphate and lithium carbonate products can be obtained from the electrolyte of the waste lithium ion batteries through simple process treatment.
Specifically, the invention provides a method for recovering electrolyte of a waste lithium ion battery, which comprises the following steps:
(1) obtaining electrolyte from a waste lithium ion battery, adding an extracting agent into the electrolyte for extraction to remove organic matters, collecting lower-layer liquid, adding a calcium compound into the lower-layer liquid, stirring, and filtering to obtain first filtrate and first filter residue; washing the first filter residue for multiple times to obtain a second filtrate and a second filter residue;
(2) adding EDTA to the first filtrate to remove calcium, filtering to obtain a third filtrate, adjusting the pH of the third filtrate to 1-2, adding an iron source, heating to react at 60-90 ℃ for 1-4h, and filtering to obtain a third filter residue and a fourth filtrate; washing the third filter residue for multiple times to obtain high-purity iron phosphate;
(3) mixing the second filtrate and the fourth filtrate, adding carbonate, heating to 80-100 ℃, and filtering to obtain fourth filter residue; and washing the fourth filter residue for multiple times to obtain high-purity lithium carbonate.
In the step (1), the obtaining of the electrolyte from the waste lithium ion battery includes: and disassembling the waste lithium ion battery, separating the positive plate, the negative plate and the diaphragm, and placing the battery in a centrifuge for centrifugation to obtain the electrolyte. Optionally, the rotation speed of the centrifugation is 1000-. For example, 1200-1800 rpm.
The electrolyte of the waste lithium ion battery contains lithium hexafluorophosphate. Optionally, the waste lithium ion battery includes a waste lithium iron phosphate battery, a waste ternary material battery, and the like.
The electrolyte of the waste lithium ion battery mainly comprises lithium hexafluorophosphate, an organic solvent (such as Dimethoxyethane (DME), Propylene Carbonate (PC), Ethylene Carbonate (EC), diethyl carbonate (DEC) and the like), and additives can be added. In the step (1), the extractant is added to the electrolyte mainly for removing organic matters such as DME, PC, EC, DEC and the like in the electrolyte and making lithium hexafluorophosphate (LiPF) as a main component as much as possible6) And remains in the lower liquid layer after extraction. Optionally, the extractant comprises at least one of benzene, gasoline, diethyl ether, carbon tetrachloride, and ethyl acetate.
In the step (1) of the present application, a calcium compound is added to the lower layer liquid (i.e., the electrolyte solution from which the organic matter has been removed), mainly for the purpose of making F in the electrolyte solution-React with calcium ions to generate CaF2Precipitation, avoidance of F-Flows into the ecological environment. Alternatively, the calcium compound may be at least one of calcium oxide and calcium hydroxide. Further, when the calcium compound is added, water is also added. Optionally, the calcium compound is added with stirring for 0.5-1.5 h. The rotational speed of the stirring can be 60-300 revolutions per minute.
In the step (1), F in the electrolyte can be tested firstly-And PF6 -And then calculating the amount of the calcium compound. Optionally, the calcium compound and F in the electrolyte-In a molar ratio of 1:1, the calcium compound and the PF in the electrolyte6 -The molar ratio of (1) to (6.0-6.2). Controlling the amount of the calcium compound in the above range can ensure F in the electrolyte-Is sufficiently precipitated without causing phosphoric acid in the electrolyteAnd (3) converting the roots into calcium phosphate, and matching with calcium removal treatment of the obtained first filtrate and heating treatment after adding carbonate in the step (3), so that no calcium carbonate is generated in the obtained fourth filter residue, and the purity of lithium carbonate is high.
In the step (1), after adding a calcium compound and stirring, the first filtrate obtained contains Ca2+、Li+、PO4 3-And trace amount of Al3+、Cu2+. Wherein, the fine scraps of the positive electrode current collector aluminum and the negative electrode current collector copper brought by disassembling the waste battery may be converted into Al under the action of HF generated by hydrolysis of lithium hexafluorophosphate3+、Cu2+. The first filter residue mainly comprises CaF2And small amount of adsorbed Li+、Al3+、Cu2+. Washing the first filter residue with water to obtain second filter residue CaF with extremely high purification2The second filtrate contains Li+And a very small amount of Al3+、Cu2+。
In the step (2), the pH is adjusted to 1-2, and the heating reaction after the iron source is added is to accelerate the formation of iron phosphate precipitate. Alternatively, in the step (2), the temperature of the heating reaction may be 60 to 80 ℃ and 70 to 90 ℃. Alternatively, the temperature of the heating reaction is 65 to 85 ℃, preferably 70 to 80 ℃. The heating reaction time can be 1-3h, 2-4h or 1-2 h.
Optionally, in the step (2), the iron source may be at least one selected from iron sulfate, iron nitrate, iron oxide red, iron chloride, and iron carbonate.
In step (2), after calcium is removed from the first filtrate, the third filtrate contains Li+、PO4 3-And trace amount of Al3+、Cu2+. The third filter residue is mainly ferric phosphate precipitate and a small amount of Li adsorbed by the ferric phosphate precipitate+、Al3+、Cu2+The fourth filtrate mainly contains Li+And trace amount of Al3+、Cu2+。
Optionally, in the step (2), the ratio of the number of moles of EDTA to the number of moles of calcium ions in the first filtrate is 4: 1.
Alternatively, in the step (3), the carbonate may be at least one selected from sodium carbonate, potassium carbonate, and ammonium carbonate. Preferably, the carbonate is ammonium carbonate.
Optionally, in the step (3), the temperature increase rate in the heating treatment is 0.5 to 2 ℃/min.
Optionally, in the step (3), the time of the heat treatment is 1-2 h.
In the step (3), carbonate is added into the combined filtrate of the second filtrate and the fourth filtrate, and then the mixture is heated at 80-100 ℃, so that most impurity ions (such as Al) can be ensured3+、Cu2+Etc.) remain in solution, yielding a fourth residue of higher purity (lithium carbonate). And if heating is firstly carried out and then carbonate is added, the lithium carbonate can quickly generate a precipitate, and most impurity ions in the solution are coated in the precipitate, so that the purity of the obtained lithium carbonate filter residue is low.
In the step (3), the fourth filter residue is washed, so that a very small amount of Al adsorbed by the lithium carbonate can be obtained3+、Cu2+Etc. and Na introduced by using sodium carbonate and potassium carbonate+、K+And the like.
In the invention, the first filter residue, the third filter residue and the fourth filter residue are washed by using the shearing emulsifying pump, so that better impurity removal and purification effects can be realized, namely impurity ions adsorbed on the surfaces of the corresponding filter residues or coated in the filter residues can be well removed. The method has the advantages that the shearing emulsifying pump is adopted for washing, impurities in the water-containing slurry of each filter residue can be fully released, the method has the characteristics of large treatment capacity, no dispersed shearing dead angle, mass and automatic production and suitability for industrial production.
Specifically, the water washing with the shear emulsification pump comprises: placing the slurry of each filter residue and water into a feeding pipe of a shearing emulsification pump, and sucking the mixed slurry into a working cavity for homogenization treatment under the pressure difference between the feeding pipe and the working cavity where a rotor of the shearing emulsification pump is located, wherein the rotating speed of the rotor of the shearing emulsification pump is 1000-2935rpm, and the pressure difference is 0.1-0.2 MPa. Optionally, the rotor speed of the shear emulsification pump is 1500-2900rpm, preferably 2000-2900 rpm. Wherein, the pressure of a working cavity where a rotor of the shearing emulsifying pump is positioned is less than the pressure in the feeding pipe.
The recovery method provided by the invention has a simple process, can convert the waste lithium ion battery electrolyte into high-purity ferric phosphate and lithium carbonate products through the design of the steps of ring-to-ring buckling, and solves the problems of high recovery difficulty, high danger in the recovery process, high recovery cost and the like of the conventional waste lithium ion battery electrolyte. The method is reasonable and easy to implement, low in cost, environment-friendly and capable of being applied industrially.
Detailed Description
The following are exemplary embodiments of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations are also regarded as the protection scope of the present invention.
The present invention will be further illustrated by the following specific examples.
Example 1
A method for recovering electrolyte of a waste lithium iron phosphate battery comprises the following steps:
(1) removing the shell of the waste lithium iron phosphate battery, disassembling and separating out a positive plate, a negative plate and a diaphragm, and placing the positive plate, the negative plate and the diaphragm in a centrifuge for centrifugation to obtain electrolyte through separation; extracting 150mL of the above electrolyte with 50mL of benzene to remove organic substances, collecting the lower liquid layer, and measuring F-The molar number of (2) is 0.013mol, PF6 -The mole number of the (2) is 0.071 mol; then adding 30g of calcium oxide and water into the lower-layer liquid, stirring for 0.5h, and filtering to obtain a first filtrate and first filter residue; washing the first filter residue with water for 3 times by using a shearing emulsifying pump to obtain a second filtrate and a second filter residue;
(2) adding EDTA (ethylene diamine tetraacetic acid) into the first filtrate obtained in the step (1) to remove calcium, filtering to obtain a third filtrate, adjusting the pH of the third filtrate to 2 by using nitric acid, adding 50g of ferric nitrate, heating and reacting at 70 ℃ for 3 hours, and filtering to obtain a third filter residue and a fourth filtrate; washing the third filter residue (with the impurity ion content of 221ppm) for 3 times by using a shearing emulsion pump to obtain high-purity iron phosphate (with the purity as high as 99.15% and the impurity ion content of only 25 ppm);
(3) mixing the second filtrate and the fourth filtrate, adding 15g of sodium carbonate into the mixed filtrate, heating to 100 ℃ at the heating rate of 1 ℃/min for heating treatment for 1h, and filtering to obtain fourth filter residue; and washing the fourth filter residue (with the impurity ion content of 138ppm) with water for 3 times by using a shearing emulsifying pump to obtain high-purity lithium carbonate (with the purity as high as 98.83% and the impurity ion content of only 41 ppm).
Example 2
A method for recovering electrolyte of a waste lithium iron phosphate battery comprises the following steps:
(1) removing the shell of the waste lithium iron phosphate battery, disassembling and separating out a positive plate, a negative plate and a diaphragm, placing the positive plate, the negative plate and the diaphragm in a centrifuge for centrifugation, and separating to obtain electrolyte; extracting 200mL of above electrolyte with 60mL of diethyl ether to remove organic substances, collecting the lower layer liquid after extraction, and measuring F-Is 0.015mol, PF6 -The mole number of (3) is 0.073 mol; then adding 40g of calcium oxide and water into the lower layer liquid, stirring for 0.8h, and filtering to obtain a first filtrate and a first filter residue; washing the first filter residue with water for 3 times by using a shearing emulsifying pump to obtain a second filtrate and a second filter residue;
(2) adding EDTA (ethylene diamine tetraacetic acid) into the first filtrate obtained in the step (1) to remove calcium, filtering to obtain a third filtrate, adjusting the pH of the third filtrate to 1 by using hydrochloric acid, adding 60g of ferric chloride, heating and reacting at 80 ℃ for 2.5h, and filtering to obtain a third filter residue and a fourth filtrate; washing the third filter residue with 3 times of water by using a shearing emulsifying pump to obtain high-purity iron phosphate (the purity is as high as 98.85%, and the content of impurity ions is only 50 ppm);
(3) combining the second filtrate and the fourth filtrate, adding 23g of sodium carbonate into the combined filtrate, heating to 90 ℃ at the heating rate of 0.5 ℃/min for heating treatment for 1.5h, and filtering to obtain fourth filter residue; and washing the fourth filter residue for 3 times by using a shearing emulsifying pump to obtain high-purity lithium carbonate (the purity is as high as 98.74%, and the content of impurity ions is only 61 ppm).
Example 3
A method for recovering electrolyte of a waste lithium iron phosphate battery comprises the following steps:
(1) removing the shell of the waste lithium iron phosphate battery, disassembling and separating out a positive plate, a negative plate and a diaphragm, placing the positive plate, the negative plate and the diaphragm in a centrifuge for centrifugation, and separating to obtain electrolyte; extracting 100mL of the above electrolyte with 30mL of ethyl acetate to remove organic substances, collecting the lower liquid layer, and measuring F-Is 0.011mol, PF6 -The mole number of (3) is 0.068 mol; then adding 25g of calcium oxide and water into the lower layer liquid, stirring for 1h, and filtering to obtain a first filtrate and a first filter residue; washing the first filter residue with water for 3 times by using a shearing emulsifying pump to obtain a second filtrate and a second filter residue;
(2) adding EDTA (ethylene diamine tetraacetic acid) into the first filtrate obtained in the step (1) to remove calcium, filtering to obtain a third filtrate, adjusting the pH of the third filtrate to 1.5 by using sulfuric acid, adding 3g of iron oxide red, heating to react at 75 ℃ for 3h, and filtering to obtain a third filter residue and a fourth filtrate; washing the third filter residue with 3 times of water by using a shearing emulsifying pump to obtain high-purity iron phosphate (the purity is as high as 98.91%, and the content of impurity ions is only 36 ppm);
(3) mixing the second filtrate and the fourth filtrate, adding 15g of sodium carbonate into the mixed filtrate, heating to 80 ℃ at the heating rate of 0.5 ℃/min for heating treatment for 2h, and filtering to obtain fourth filter residue; and washing the fourth filter residue for 3 times by using a shearing emulsifying pump to obtain high-purity lithium carbonate (the purity is as high as 98.78%, and the content of impurity ions is only 45 ppm).
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A method for recovering electrolyte of a waste lithium ion battery is characterized by comprising the following steps:
(1) obtaining electrolyte from a waste lithium ion battery, adding an extracting agent into the electrolyte for extraction to remove organic matters, collecting lower-layer liquid, adding a calcium compound into the lower-layer liquid, stirring, and filtering to obtain first filtrate and first filter residue; washing the first filter residue for multiple times to obtain a second filtrate and a second filter residue;
(2) adding EDTA to the first filtrate to remove calcium, filtering to obtain a third filtrate, adjusting the pH of the third filtrate to 1-2, adding an iron source, heating to react at 60-90 ℃ for 1-4h, and filtering to obtain a third filter residue and a fourth filtrate; washing the third filter residue for multiple times to obtain high-purity iron phosphate;
(3) mixing the second filtrate and the fourth filtrate, adding carbonate, heating to 80-100 ℃, and filtering to obtain fourth filter residue; and washing the fourth filter residue for multiple times to obtain high-purity lithium carbonate.
2. The recycling method according to claim 1, wherein in the step (1), the obtaining of the electrolyte from the lithium ion battery comprises: and disassembling the waste lithium ion battery, separating the positive plate, the negative plate and the diaphragm, and placing the battery in a centrifuge for centrifugation to obtain the electrolyte.
3. The recovery process of claim 1, wherein in step (1), the extractant comprises at least one of benzene, gasoline, diethyl ether, carbon tetrachloride, and ethyl acetate.
4. The recycling method according to claim 1, wherein in the step (1), the calcium compound may be at least one of calcium oxide and calcium hydroxide.
5. A recycling method according to claim 4, wherein in the step (1), the calcium compound and F in the electrolyte-In a molar ratio of 1:1, the calcium compound and the PF in the electrolyte6 -The molar ratio of (1) to (6.0-6.2).
6. The recycling method according to claim 1, wherein in the step (2), the iron source is at least one selected from the group consisting of iron sulfate, iron nitrate, iron oxide red, iron chloride, and iron carbonate.
7. The recycling method according to claim 1, wherein in the step (3), the carbonate may be at least one selected from the group consisting of sodium carbonate, potassium carbonate, and ammonium carbonate.
8. The recovery method according to claim 1, wherein in the step (3), the temperature increase rate in the heat treatment is 0.5 to 2 ℃/min.
9. The recovery method of any one of claims 1-8, wherein the water washing of the first, third and fourth filter cake is performed with a shear emulsification pump.
10. The recycling method according to claim 9, wherein the water washing with the shear emulsification pump comprises: placing the slurry of each filter residue and water into a feeding pipe of a shearing emulsification pump, and sucking the mixed slurry into a working cavity for homogenization treatment under the pressure difference between the feeding pipe and the working cavity where a rotor of the shearing emulsification pump is located, wherein the rotating speed of the rotor of the shearing emulsification pump is 1000-2935rpm, and the pressure difference is 0.1-0.2 MPa.
CN202010629017.9A 2020-07-02 2020-07-02 Method for recovering electrolyte of waste lithium ion battery Pending CN111924816A (en)

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CN114759286A (en) * 2022-05-30 2022-07-15 清华大学深圳国际研究生院 Method for recovering waste electrolyte of lithium ion battery
WO2024021232A1 (en) * 2022-07-28 2024-02-01 广东邦普循环科技有限公司 Method for underwater crushing and electrolyte solution recycling of waste lithium ion battery

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