CN110743528B - Method for preparing water decomposition catalyst by using waste battery - Google Patents
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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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
- 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
A method for preparing a water decomposition catalyst by using waste batteries comprises the following steps: disassembling the waste battery, and disassembling a positive electrode, a negative electrode and a diaphragm from the waste battery; separating out the positive active material on the positive current collector to obtain positive active material particles; adding positive active material particles into a strong acid solution for reaction and dissolution, then adding an alkaline solution to make the solution neutral, and then adding buffer salt into the solution to prepare a catalyst precursor solution; the catalyst is prepared by an electrodeposition method in an electrolytic cell containing a catalyst precursor solution. The method of the invention uses the anode material in the waste battery to prepare the water decomposition catalyst, has simple process, short recovery period and low cost, and the obtained product has high added value.
Description
Technical Field
The invention belongs to the technical field of recycling of waste lithium batteries, and particularly relates to a method for preparing a water decomposition catalyst by using a positive electrode material of a waste battery.
Background
In recent years, new energy automobiles in China are developed rapidly under the promotion of national policies. The sales volume of new energy automobiles in China in the last half of 2019 reaches 61.7 thousands, and the new energy automobiles are the first to live in the world. The service life of the new energy automobile is about 8 years, and at present, part of new energy automobiles face the problem of scrapping treatment. By 2020, new energy automobiles in China enter a scrapping peak period, and the scrapping amount at the time is more than 20 thousands of automobiles. If the waste water cannot be recycled, the waste water not only causes huge pollution to the environment, but also causes a large amount of resource loss.
The recovery of the lithium battery is a major subject of the recovery and utilization of new energy automobiles, and aiming at the recovery and the utilization of the lithium battery, the commonly used treatment means is to separate the active materials of the positive electrode sheet and the negative electrode sheet of the battery by an ultrasonic stripping method or a mechanical crushing method, then dissolve the active material of the positive electrode into an acid solution, neutralize the solution, then precipitate metal elements, and finally prepare the positive electrode material or the raw material again by a high-temperature sintering method. However, the anode material or raw material prepared from the material recovered by the process has the problems of incapability of ensuring the purity, uncontrollable structure of the material, long preparation period of the material, high cost and the like. How to fully utilize the waste batteries and prepare products with higher added value, lower preparation cost and simpler process is an urgent problem to be solved for recycling the waste lithium ion batteries.
Disclosure of Invention
The invention aims to provide a method for preparing a water-splitting catalyst by using waste batteries, which is used for preparing the water-splitting catalyst with high added value by recovering metal elements in the waste batteries.
In order to achieve the purpose, the invention adopts the following technical solutions:
A method for preparing a water decomposition catalyst by using waste batteries comprises the following steps:
disassembling the waste battery, and disassembling a positive electrode, a negative electrode and a diaphragm from the waste battery;
separating out the positive active material on the positive current collector to obtain positive active material particles;
adding positive active material particles into a strong acid solution for reaction and dissolution, then adding an alkaline solution to make the solution neutral, and then adding buffer salt into the solution to prepare a catalyst precursor solution;
the catalyst is prepared by an electrodeposition method in an electrolytic cell containing a catalyst precursor solution.
Further, performing electrodeposition on the catalyst by adopting a cyclic voltammetry method, performing electrodeposition by taking a conductive current collector as a working electrode, a glassy carbon electrode as a counter electrode and Ag/AgCl as a reference electrode, and washing and drying a film deposited on the conductive current collector to obtain the water decomposition catalyst.
Further, the conductive current collector is a metal simple substance current collector, a metal compound current collector, an alloy current collector, a carbon current collector or conductive glass.
Furthermore, the scanning voltage range of the electrodeposition is 3.0 to-2.0 vs. NHE, the scanning speed is 1 to 1000mV/s, and the scanning times are 1 to 1000 weeks.
Furthermore, when the waste battery is disassembled, the waste battery is completely discharged, then the waste battery is subjected to shell breaking, and the anode, the cathode and the diaphragm are disassembled.
Furthermore, during discharging, the waste battery is discharged to the lower limit voltage, and then the resistance wire is used for short-circuiting the positive electrode and the negative electrode of the battery, so that the battery is completely discharged.
Further, when the positive active material is separated, the anode obtained by splitting is crushed, anode fragments are dispersed in an organic solvent, so that the positive active material is separated from the current collector and is dispersed in an organic solution, and then screening is carried out, so that current collector fragments, a conductive agent and positive active material particles are obtained.
Furthermore, ultrasonic dispersion is carried out for 1-12 hours at the temperature of 60-95 ℃ during dispersion.
Further, the organic solvent for dispersion is one or a mixture of more of N, N-dimethylformamide, alcohol, acetonitrile, N-methylpyrrolidone, ether solvents and lipid solvents.
Further, the buffer salt is NaH 2 PO 3 /Na 2 HPO 3 NaH in catalyst precursor solution 2 PO 3 /Na 2 HPO 3 The concentration of (B) is 1 mM-1000 mM.
According to the technical scheme, the method utilizes the anode material in the waste battery to prepare the water decomposition catalyst, and compared with the conventional waste battery recovery process, the method has the following advantages that:
1. The process is simple: in the process of preparing the water decomposition catalyst by using the metal elements of the waste lithium ion battery positive plate, a metal element precipitation separation process and a high-temperature sintering process are not required, so that the recovery process is greatly simplified, the process time is shortened, and the problems of complex process and long recovery period of the existing waste battery recovery technology are solved;
2. the cost is low: the process for preparing the catalyst by electrodeposition only needs a small amount of electric energy, and has simple equipment and low cost;
3. high added value: according to the invention, the metal in the anode plate of the waste lithium ion battery is prepared into the water decomposition catalyst by an electrochemical deposition method, and the obtained product has high added value.
Drawings
In order to illustrate the embodiments of the present invention more clearly, the drawings that are needed in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained by those skilled in the art without inventive effort.
FIG. 1 is a scanning electron micrograph of a catalyst obtained in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a catalyst obtained in example 2 of the present invention;
FIG. 3 is a scanning electron micrograph of a catalyst obtained in example 3 of the present invention;
FIG. 4 is a graph comparing the electrocatalytic water splitting performance of the catalysts of examples 1, 2, 3 of the present invention and comparative example.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Detailed Description
In order to make the aforementioned and other objects, features and advantages of the invention more apparent, embodiments of the invention are described in detail below.
The invention relates to a method for preparing a water decomposition catalyst by using a positive electrode material in a waste battery, wherein the waste battery can be a waste ternary battery, a waste lithium cobaltate, a waste lithium iron phosphate battery and the like, and the type of the battery can be a liquid lithium ion battery, a lithium sulfur battery, a solid battery and the like. The method comprises the following steps:
disassembling the battery; after the waste battery is completely discharged, the battery is broken, and the anode, the cathode and the diaphragm are separated and collected. When discharging, the waste battery can be discharged to the lower limit voltage, and then the resistance wire is used for short-circuiting the positive electrode and the negative electrode of the battery, so that the electricity in the battery is completely discharged. The resistance of the resistance wire can be 0.01-10000 m omega.
Separating the positive electrode active material; and crushing the split positive pole piece, dispersing the positive pole pieces into an organic solvent, separating the positive active material from the current collector and dispersing the positive active material in the organic solvent, and then screening to obtain current collector pieces, a conductive agent and positive active material particles. In order to enhance the dispersion effect, the ultrasonic dispersion can be carried out for 1-12 hours at the temperature of 60-95 ℃ during dispersion. The organic solvent for dispersion may be one or more of N, N-dimethylformamide, alcohol, acetonitrile, N-methylpyrrolidone, ether solvent, lipid solvent, etc. The screened positive active material can be one or a mixture of a ternary material, lithium cobaltate, lithium manganate and lithium iron phosphate.
Preparing a catalyst precursor solution; adding the separated positive active material particles into a strong acid solution for reaction and dissolution, adding an alkaline solution for synthesis after the reaction is finished to make the solution finally neutral, and then adding buffer salt into the solution to prepare the catalyst precursor solution. The strong acid in the step can be one or a mixture of sulfuric acid, nitric acid, hydrochloric acid and perchloric acid, and the alkaline solution can be NaOH solution. The buffer salt can be NaH 2 PO 3 /Na 2 HPO 3 Buffer bag, NaH 2 PO 3 /Na 2 HPO 3 The buffer bag contains NaH 2 PO 3 And Na 2 HPO 3 Adding NaH to 2 PO 3 /Na 2 HPO 3 Adding the mixture into the solution,NaH in the prepared catalyst precursor solution 2 PO 3 /Na 2 HPO 3 The concentration of (B) is 1 mM-1000 mM.
Preparing a catalyst; the method comprises the steps of preparing a catalyst by adopting an electrodeposition method, performing electrodeposition on the catalyst by adopting a cyclic voltammetry method, preparing the catalyst by performing electrodeposition in an electrolytic cell containing a catalyst precursor solution by taking a conductive current collector as a working electrode, a glassy carbon electrode as a counter electrode and Ag/AgCl (saturated potassium chloride-containing internal solution) as a reference electrode, depositing a layer of film, namely the water-decomposing catalyst, on the current collector to obtain the water-decomposing catalyst, washing the water-decomposing catalyst by using deionized water for several times, and performing vacuum drying to obtain the water-decomposing catalyst. The conductive current collector in the step can be made of metal simple substances, metal compound materials, alloy materials, carbon materials, conductive glass and other materials. The scanning voltage range of the electrodeposition is 3.0 to-2.0 vs. NHE, the scanning speed is 1 to 1000mV/s, and the scanning times are 1 to 1000 weeks. Preferably, the scanning voltage range is 1.2 to-0.8 vs. NHE, and the scanning speed is 5 to 100 mV/s.
The present invention will be further illustrated by the following specific examples and comparative examples. The reagents, materials and instruments used in the following description are all conventional reagents, conventional materials and conventional instruments, which are commercially available, and the reagents may be synthesized by a conventional synthesis method, if not specifically described.
Example 1
Firstly, discharging the waste ternary lithium ion battery to a lower limit voltage of 2.7V by using the waste ternary lithium ion battery as a raw material, then short-circuiting the positive electrode and the negative electrode of the waste battery by using a resistance wire with a resistance of 30m omega to enable the battery to be completely discharged, then mechanically breaking the shell of the battery, and separating and separately collecting the positive electrode, the negative electrode and the diaphragm.
And step two, mechanically crushing the positive plate, dispersing the obtained positive fragments into N, N-dimethylformamide, performing ultrasound treatment at the temperature of 70 ℃ for 2 hours to separate the positive active material from the current collector and disperse the positive active material in an organic solvent, then screening to obtain current collector fragments, a conductive agent and positive active material particles, and washing the positive active material particles with water for three times.
Step three, slowly adding the separated positive active material particles into a 1M concentrated sulfuric acid solution for reaction and dissolution, neutralizing with a 0.1M sodium hydroxide solution after the reaction is finished to finally make the solution neutral, and then adding NaH into the solution 2 PO 3 /Na 2 HPO 3 Preparing a catalyst precursor solution, and adding NaH into the prepared precursor solution 2 PO 3 /Na 2 HPO 3 The concentration of (3) is 0.1M.
And step four, performing electrodeposition in an electrolytic cell containing precursor solution to prepare the catalyst by taking conductive glass (FTO) as a working electrode, a glassy carbon electrode as a counter electrode and Ag/AgCl (saturated potassium chloride-containing internal solution) as a reference electrode. Carrying out electro-deposition on the catalyst by adopting cyclic voltammetry, wherein the scanning voltage range is 1.2-0.8 vs. NHE, the scanning speed is 20mV/s, the scanning period is 12 weeks, a layer of film, namely the water decomposition catalyst, is obtained by deposition on conductive glass, then the water decomposition catalyst is washed by deionized water for three times, and the water decomposition catalyst C1 is obtained by vacuum drying for 2 hours at the temperature of 100 ℃. FIG. 1 is an SEM photograph of water-splitting catalyst C1 prepared in example 1, and it can be seen from FIG. 1 that a layer of particulate catalyst is deposited on the surface of the FTO.
Example 2
This example is different from example 1 in that it uses a waste lithium cobalt oxide battery as a raw material to prepare a water-splitting catalyst, and the other steps are the same as example 1, and the obtained water-splitting catalyst is designated as C2. FIG. 2 is an SEM photograph of water-splitting catalyst C2 prepared in example 2, and it can be seen from FIG. 2 that a layer of particulate catalyst is deposited on the surface of the FTO.
Example 3
This example is different from example 1 in that it uses waste lithium iron phosphate batteries as raw materials to prepare a water-splitting catalyst, and the other steps are the same as those of example 1, and the obtained water-splitting catalyst is designated as C3. FIG. 3 is an SEM photograph of water-splitting catalyst C3 prepared in example 3, and from FIG. 3 it can be seen that a layer of bulk catalyst was deposited on the surface of the FTO.
The water-splitting catalysts obtained in examples 1, 2 and 3 were subjected to a catalytic performance test, and a blank FTO (conductive glass) was used as a comparative example, which was designated as D1. During testing, a catalyst, Ag/AgCl (saturated potassium chloride-containing internal solution) and a glassy carbon electrode are respectively used as a working electrode, a reference electrode and a counter electrode, and electrocatalytic reaction is carried out for 3 hours under the potential of 1.1V vs. The comparison of the obtained electrocatalytic water splitting performance is shown in FIG. 4, and it can be seen from FIG. 4 that the catalysts C1, C2 and C3 prepared in examples 1, 2 and 3 all have better water splitting catalytic activity, and among them, the catalyst performance of C1 is the best. The water decomposition catalyst is prepared by using the anode material of the waste battery, and the metal element precipitation separation and high-temperature sintering are not needed in the whole process, so that the recovery process is greatly simplified, the recovery cost is reduced, and the additional value of the product is improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for preparing a water decomposition catalyst by using waste batteries is characterized by comprising the following steps:
disassembling the waste battery, and disassembling a positive electrode, a negative electrode and a diaphragm from the waste battery;
separating out the positive active material on the positive current collector to obtain positive active material particles;
adding positive active material particles into a strong acid solution for reaction and dissolution, then adding an alkaline solution to make the solution neutral, and then adding buffer salt into the solution to prepare a catalyst precursor solution;
the catalyst is prepared in an electrolytic cell containing a catalyst precursor solution by adopting an electrodeposition method, wherein the scanning voltage range of electrodeposition is 1.2-0.8 vs. NHE, and the scanning speed is 5-100 mV/s.
2. The method for preparing a water-splitting catalyst using waste batteries according to claim 1, wherein: performing electrodeposition on the catalyst by adopting a cyclic voltammetry method, performing electrodeposition by taking a conductive current collector as a working electrode, a glassy carbon electrode as a counter electrode and Ag/AgCl as a reference electrode, and washing and drying a film deposited on the conductive current collector to obtain the water decomposition catalyst.
3. The method for preparing a water-splitting catalyst using waste batteries according to claim 2, wherein: the conductive current collector is a metal simple substance current collector or a metal compound current collector or an alloy current collector or a carbon current collector or conductive glass.
4. The method for preparing a water-splitting catalyst using the waste battery as set forth in claim 1, wherein: when the waste batteries are disassembled, the waste batteries are completely discharged, then the shells of the waste batteries are broken, and the positive electrode, the negative electrode and the diaphragm are disassembled.
5. The method for preparing a water-splitting catalyst using waste batteries according to claim 4, wherein: when discharging, the waste battery is discharged to the lower limit voltage, and then the resistance wire is used for short-circuiting the positive electrode and the negative electrode of the battery, so that the battery is completely discharged.
6. The method for preparing a water-splitting catalyst using the waste battery as set forth in claim 1, wherein: when the positive active material is separated, the anode obtained by splitting is crushed, the anode fragments are dispersed in an organic solvent, so that the positive active material is separated from the current collector and is dispersed in the organic solvent, and then screening is carried out, so that the current collector fragments, the conductive agent and the positive active material particles are obtained.
7. The method for preparing a water-splitting catalyst using waste batteries according to claim 6, wherein: ultrasonic dispersion is carried out for 1-12 hours at the temperature of 60-95 ℃ during dispersion.
8. The method for preparing a water-splitting catalyst using the waste batteries according to claim 6 or 7, wherein: the organic solvent for dispersion is one or more of N, N-dimethylformamide, alcohol, acetonitrile, N-methylpyrrolidone, ether solvent and lipid solvent.
9. The method for preparing a water-splitting catalyst using the waste battery as set forth in claim 1, wherein: the buffer salt is NaH 2 PO 3 /Na 2 HPO 3 NaH in catalyst precursor solution 2 PO 3 /Na 2 HPO 3 The concentration of (B) is 1 mM-1000 mM.
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| CN113355690B (en) * | 2020-03-03 | 2022-05-06 | 天津大学 | Method for preparing efficient water electrolysis catalyst on large scale by using waste lithium ion battery anode material |
| CN113611876A (en) * | 2021-08-05 | 2021-11-05 | 哈尔滨工业大学 | Method for recycling anode material of waste lithium ion battery as electrocatalyst |
| CN113707893B (en) * | 2021-08-16 | 2022-08-12 | 广西师范大学 | Carbon-based electrocatalyst prepared from waste lithium iron phosphate battery positive electrode material and preparation method and application thereof |
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