CN112151902B - Method for quickly separating electrode material from current collector and utilizing electrode material and current collector in high-value mode - Google Patents
Method for quickly separating electrode material from current collector and utilizing electrode material and current collector in high-value mode Download PDFInfo
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- CN112151902B CN112151902B CN202010843790.5A CN202010843790A CN112151902B CN 112151902 B CN112151902 B CN 112151902B CN 202010843790 A CN202010843790 A CN 202010843790A CN 112151902 B CN112151902 B CN 112151902B
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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
The invention discloses a method for quickly separating an electrode material from a current collector and a device for quickly separating the electrode material from the current collectorA method of upscaling utilization, the method comprising the steps of: removing an electrode plate from a waste battery, wherein the electrode plate comprises an electrode material and a nickel-based current collector fixedly connected with the electrode material through a binder; putting the electrode plate into a heating furnace, introducing carbon monoxide gas into the heating furnace, heating to a preset temperature, and reacting a nickel-based current collector in the electrode plate with the carbon monoxide gas to generate gaseous Ni (CO)4(ii) a For the gaseous Ni (CO)4Carrying out heat treatment, and decomposing to obtain nickel powder and carbon monoxide; and calcining the residual electrode material and the binder in the heating furnace, removing the binder and recovering the electrode material. The invention can realize the rapid separation of the electrode material and the current collector, and because the interface separation process is relatively mild, strong acid and strong alkali damage is not adopted, the structure damage of the recovered electrode material is less, and the physical method recycling can be facilitated.
Description
Technical Field
The invention relates to the technical field of battery recovery, in particular to a method for quickly separating and utilizing an electrode material and a current collector in a high-value mode.
Background
In recent years, lithium ion batteries have been widely used in various fields, and their usage has been steadily increasing not only in the 3C field but also in the electric automobile field. With the great increase of the capacity of lithium batteries, the production of a large amount of waste lithium batteries causes serious environmental pollution. Therefore, the method has important significance for recycling the waste lithium battery, has huge economic value, and can relieve potential environmental crisis.
The industry is still in the exploration and development stage of the recovery technology of the waste batteries, and all the technologies need to be mature and improved. The battery active material is used as an important component of a lithium battery and is adhered to a current collector through an organic binder such as PVDF (polyvinylidene fluoride), and the current collector is usually made of an aluminum foil or a nickel-based material. In the process of recycling the waste batteries, the binding force between the electrode material and the current collector is quite firm, so that the direct mechanical separation is difficult to achieve, and the efficient separation and sorting of the electrode material and the current collector becomes a technical problem to be solved urgently in the current waste battery recycling industry application.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, an object of the present invention is to provide a method for rapid separation and high-value utilization of an electrode material and a current collector, which aims to solve the problem that the prior art cannot rapidly and efficiently separate the electrode material and a nickel-based current collector in a waste battery.
The technical scheme of the invention is as follows:
a method for rapid separation and high-value utilization of an electrode material and a current collector comprises the following steps:
removing an electrode plate from a waste battery, wherein the electrode plate comprises an electrode material and a nickel-based current collector fixedly connected with the electrode material through a binder;
putting the electrode plate into a heating furnace, introducing carbon monoxide gas into the heating furnace, heating to a preset temperature, and reacting a nickel-based current collector in the electrode plate with the carbon monoxide gas to generate gaseous Ni (CO)4；
Recovering said gaseous Ni (CO)4Separating the electrode material from the nickel-based current collector;
for the recovered gaseous Ni (CO)4Carrying out heat treatment, and decomposing to obtain nickel powder and carbon monoxide;
and calcining the residual electrode material and the binder in the heating furnace, removing the binder and recovering the electrode material.
The electrode plate is a positive plate, the positive plate comprises a positive material and a positive nickel-based current collector fixedly connected with the positive material through a binder, and the positive nickel-based current collector material is one of pure nickel, nickel alloy or nickel-plated material which is treated by a passivating agent.
The electrode plate is a negative plate, the negative plate comprises a negative material and a negative nickel-based current collector fixedly connected with the negative material through a binder, and the negative nickel-based current collector material is one of pure nickel, nickel alloy or nickel-plated material.
The method for rapid separation and high-value utilization of the electrode material and the current collector comprises the step of carrying out high-speed separation on the electrode material and the current collector, wherein the passivating agent is one or more of chromate, potassium permanganate, titanium salt, phosphate, molybdate, silicate and silane.
The method for quickly separating the electrode material from the current collector and utilizing the electrode material in a high-value mode, wherein in the step of introducing carbon monoxide gas into the heating furnace and heating to the preset temperature, the preset temperature is 50-70 ℃.
The electrode material and the current collector are quickly separated and the value of the electrode material and the current collector are utilized in a high-value way, wherein the recovered gaseous Ni (CO) is used4In the step of performing the heat treatment, the heat treatment temperature is 230-350 ℃.
The method for rapid separation and high-value utilization of the electrode material and the current collector comprises the step of calcining at the temperature of 600-700 ℃.
Has the advantages that: the invention provides a method for quickly separating and utilizing high value of an electrode material and a current collector, which utilizes the low-temperature volatilization and decomposition characteristics of nickel tetracarbonyl, decomposes an electrode material of a waste battery and a nickel-based current collector interface by adopting CO at a low temperature (50-70 ℃) to separate the nickel-based current collector from the electrode material by volatilizing the nickel tetracarbonyl, and then decomposes the nickel tetracarbonyl into high-purity nickel powder and carbon monoxide at a relatively higher temperature (230-. The invention can realize the rapid separation of the electrode material of the waste battery and the current collector, and the structure of the recovered electrode material is less damaged because the interface separation process is relatively mild and does not adopt strong acid and strong alkali, thereby being beneficial to the regeneration and the utilization of a physical method; the carbon monoxide medium can be recycled, and the current collector can be prepared into high-purity nickel powder, so that the added value is high and the cost is low.
Drawings
Fig. 1 is a flowchart illustrating a method for rapid separation and high-value utilization of an electrode material and a current collector according to a preferred embodiment of the present invention.
Fig. 2 is an SEM image of the positive electrode material of example 1 after being peeled and sintered at 600 ℃.
Fig. 3 is an XRD pattern of the positive electrode material of example 1 after being peeled and sintered at 600 ℃.
Detailed Description
The present invention provides a method for rapid separation and high-value utilization of an electrode material and a current collector, and the present invention is further described in detail below in order to make the purpose, technical scheme and effect of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The current concept of separating electrode materials and current collectors in waste batteries generally includes: removing the binder at high temperature, dissolving the binder in organic solution, dissolving the current collector in alkali solution, and the like. The disadvantage of removing the binder at high temperature is that the temperature is high, the energy consumption is high, and the waste generated by burning the binder needs to be added with an additional recovery device; in the method for dissolving the binder by the organic solution, the viscosity of the organic solvent is high, so that the subsequent electrode materials cannot be sieved easily after dissolution; the problems of long time consumption, large liquid consumption, large amount of waste gas generated in the dissolving process and the like exist in the alkali liquor dissolving process.
Based on the problems in the prior art, the present embodiment provides a method for quickly separating and utilizing an electrode material and a current collector in a high-value manner, as shown in fig. 1, which includes the steps of:
s10, removing an electrode plate from the waste battery, wherein the electrode plate comprises an electrode material and a nickel-based current collector fixedly connected with the electrode material through a binder;
s20, after the electrode plate is placed in a heating furnace, introducing carbon monoxide gas into the heating furnace and heating to a preset temperature to enable the nickel-based current collector and the nickel-based current collector in the electrode plate to be connected with each otherThe carbon monoxide gas reacts to produce gaseous Ni (CO)4；
S30, recovering the gaseous Ni (CO)4Separating the electrode material from the nickel-based current collector;
s40, recovering the gaseous Ni (CO)4Carrying out heat treatment, and decomposing to obtain nickel powder and carbon monoxide;
and S50, calcining the residual electrode material and the binder in the heating furnace, removing the binder, and recovering the electrode material.
In the embodiment, the electrode plate has certain porosity, CO gas can reach the interface of the nickel-based current collector through the electrode plate under the action of airflow, and the nickel-based current collector and the CO gas can react to generate gaseous nickel tetracarbonyl (Ni (CO))4) And volatilizing to realize the rapid damage of the contact interface of the electrode material and the nickel-based current collector, so that the electrode material directly falls off from the nickel-based current collector and is separated. Along with the extension of the reaction time, the CO gas can further react with the nickel-based current collector, so that the nickel-based current collector can completely generate nickel tetracarbonyl gas which is completely separated from the electrode material, the volatilized nickel tetracarbonyl is collected, and the nickel tetracarbonyl is heated to a specific temperature by a heating furnace such as a tubular furnace, and the Ni (CO)4 gas is decomposed to obtain high-purity nickel powder and carbon monoxide. The carbon monoxide is recycled, and the high-purity nickel powder can be used for regenerating nickel foil or sold outside. The invention can realize the rapid separation of the electrode material of the waste battery and the current collector, and the structure of the recovered electrode material is less damaged because the interface separation process is relatively mild and does not adopt strong acid and strong alkali, thereby being beneficial to the physical method for recycling.
The method for separating the nickel-based current collector from the positive electrode material has the advantages that the contact interface of the nickel-based current collector and the electrode material is directly damaged from the inside of the electrode plate, the electrode material and the nickel-based current collector can be sufficiently separated, the separation method of the embodiment is simple, the nickel foil is dissolved by strong acid and strong base in the traditional lithium battery recovery process to be separated from the positive electrode material, obviously, the embodiment reduces the steps of raw and auxiliary materials and the process flow, saves the cost, improves the efficiency, and can further refine the nickel-based current collector to obtain high-purity nickel powder. In the embodiment, organic solvents such as NMP, DMAC, DMF and the like are not adopted, so that the pollution to the environment and the high cost of the recovery process caused by the introduction of a large amount of organic solvents are reduced, the recovery process of the whole waste lithium battery current collector is simplified, the high value of the recovered product is realized, and the recovery rate of the nickel-based current collector by the separation method can reach more than 99%. The embodiment also solves the problem of recycling lithium battery resources, relieves worries for the development of electric automobiles, does not produce secondary pollution of waste acid or waste alkali, and has wide application prospect.
In some specific embodiments, the waste lithium battery may be a waste lithium battery, the waste lithium battery is disassembled after discharging, electrode plates therein are taken out, and are respectively cleaned by an organic solvent or deionized water to remove electrolytes, the positive electrode plate and the negative electrode plate are cut into small pieces and are respectively placed into a heating furnace, carbon monoxide gas is introduced into the heating furnace, the flow rate of CO is controlled, a certain temperature and pressure are maintained, and under the condition, nickel in the nickel-based current collector reacts with CO to generate gaseous ni (CO)4Keeping the reaction for a period of time, wherein the residual black powder substances in the quartz boat are respectively battery anode material and cathode material active substances; respectively calcining the black powder substances, and removing the organic binder to obtain pure recovered cathode powder and graphite powder; collecting Ni (CO)4Heating the gas to a certain temperature, and decomposing to obtain high-purity nickel powder and regenerated carbon monoxide.
In some embodiments, the electrode sheet is a positive electrode sheet, the positive electrode sheet includes a positive electrode material and a positive electrode nickel-based current collector fixedly connected to the positive electrode material by a binder, and the positive electrode nickel-based current collector material is one of pure nickel, a nickel alloy or a nickel-plated material treated by a passivation solution, but is not limited thereto. By way of example, the passivating agent is one or more of a chromium salt, potassium permanganate, a titanium salt, a phosphate, a molybdate, a silicate, and a silane, but is not limited thereto.
In other embodiments, the electrode sheet is a negative electrode sheet, the negative electrode sheet includes a negative electrode material and a negative electrode nickel-based current collector fixedly connected to the negative electrode material by a binder, and the negative electrode nickel-based current collector material is one of pure nickel, a nickel alloy, or a nickel-plated material, but is not limited thereto.
In some embodiments, the step of introducing carbon monoxide gas into the heating furnace and heating to a predetermined temperature is performed at 50 to 70 ℃. In this temperature range, the reaction efficiency of the carbon monoxide gas and the nickel-based current collector is the highest, and Ni (CO) can be generated rapidly and efficiently4Gas, thereby effectively separating the electrode material from the nickel-based current collector.
In some specific embodiments, the gas pressure in the furnace is less than or equal to 50kPa, and the reaction time of the carbon monoxide gas and the nickel-based current collector is 8-12h to ensure effective separation of the electrode material and the nickel-based current collector. By way of example, carbon monoxide gas is introduced into the heating furnace and heated to 50 ℃ under the condition of 50kPa, and the carbon monoxide gas is reacted with the nickel-based current collector for 10 hours, so that the nickel-based current collector is completely reacted to generate gaseous Ni (CO)4。
In some embodiments, the gaseous Ni (CO) to be recovered4Is passed into a tube furnace and heated to 230-350 ℃, and the gaseous Ni (CO)4Decomposing to obtain high-purity nickel and carbon monoxide.
In some embodiments, after introducing carbon monoxide gas into the heating furnace and maintaining the reaction for a period of time, the remaining black powder material in the quartz boat is the electrode material and adhesive of the waste battery, and the electrode material can be positive electrode material powder or negative electrode material powder, PVDF, conductive carbon, etc. And calcining the residual electrode material and the binder in the heating furnace at the calcining temperature of 600-700 ℃, and removing the binder to obtain the recovered and relatively pure battery electrode material.
The following is a further explanation of the method for rapid separation and high-value utilization of electrode material and current collector according to the present invention through specific embodiments:
example 1
Assembling a lithium battery (power on) NCM523 by using the passivated nickel foil as a positive current collector and the pure nickel foil as a negative current collector;
carrying out a charge-discharge experiment on the lithium battery to obtain a waste lithium battery;
disassembling the waste lithium battery after discharging, taking out electrode plates in the waste lithium battery, and respectively cleaning a positive plate and a negative plate by using deionized water;
cutting the positive plate and the negative plate into small pieces of 5mm multiplied by 5mm, respectively placing the small pieces into a quartz boat and placing the quartz boat and the quartz boat into a tube furnace;
introducing carbon monoxide gas into the tubular furnace, controlling the flow rate of CO, keeping the temperature at 50 ℃ and the pressure at 50kPa, and reacting nickel in the nickel-based current collector with CO to generate gaseous Ni (CO)4 under the condition;
keeping the reaction for 10 hours, wherein the residual black powder substances in the quartz boat are respectively battery anode material and cathode material active substances;
placing the powder into an alumina crucible and placing the powder into a muffle furnace, keeping the temperature at 600 ℃, and calcining for 8 hours; obtaining pure NCM523 material and graphite powder;
heating the collected Ni (CO)4 gas to 260 ℃, and decomposing the gas to obtain high-purity nickel powder and regenerated carbon monoxide.
Fig. 2 is an SEM image of the recovered NCM523 ternary cathode material.
Fig. 3 is an XRD pattern of the recovered NCM523 ternary cathode material, from which it can be seen that the cathode waste has an α -NaFeO2 type layered structure and no impurity phase exists.
Example 2
Assembling a lithium battery (power on) NCM622 by using the passivated nickel foil as a positive current collector and the pure nickel foil as a negative current collector;
carrying out a charge-discharge experiment on the lithium battery to obtain a waste lithium battery;
disassembling the waste lithium battery after discharging, taking out electrode plates in the waste lithium battery, and respectively cleaning a positive plate and a negative plate by using deionized water;
cutting the positive plate and the negative plate into small pieces of 5mm multiplied by 5mm, respectively placing the small pieces into a quartz boat and placing the quartz boat and the quartz boat into a tube furnace;
introducing carbon monoxide gas into the tubular furnace, controlling the flow rate of CO, keeping the temperature at 60 ℃ and the pressure at 50kPa, and reacting nickel in the nickel-based current collector with CO to generate gaseous Ni (CO)4 under the condition;
keeping the reaction for 10 hours, wherein the residual black powder substances in the quartz boat are respectively battery anode material and cathode material active substances;
placing the powder into an alumina crucible and placing the powder into a muffle furnace, keeping the temperature at 600 ℃, and calcining for 8 hours; obtaining pure NCM622 material and graphite powder;
heating the collected Ni (CO)4 gas to 280 ℃, and decomposing the gas to obtain high-purity nickel powder and regenerated carbon monoxide.
Example 3
Assembling a lithium cobalt oxide battery (power on) by using the passivated nickel foil as a positive current collector and the pure nickel foil as a negative current collector;
carrying out a charge-discharge experiment on the lithium battery to obtain a waste lithium battery;
disassembling the waste lithium battery after discharging, taking out electrode plates in the waste lithium battery, and respectively cleaning a positive plate and a negative plate by using deionized water;
cutting the positive plate and the negative plate into small pieces of 5mm multiplied by 5mm, respectively placing the small pieces into a quartz boat and placing the quartz boat and the quartz boat into a tube furnace;
introducing carbon monoxide gas into the tubular furnace, controlling the flow rate of CO, keeping the temperature at 65 ℃ and the pressure at 50kPa, and reacting nickel in the nickel-based current collector with CO to generate gaseous Ni (CO)4 under the condition;
keeping the reaction for 10 hours, wherein the residual black powder substances in the quartz boat are respectively battery anode material and cathode material active substances;
placing the powder into an alumina crucible and placing the powder into a muffle furnace, keeping the temperature at 600 ℃, and calcining for 8 hours; obtaining pure lithium cobaltate material and graphite powder;
heating the collected Ni (CO)4 gas to 300 ℃, and decomposing the gas to obtain high-purity nickel powder and regenerated carbon monoxide.
In summary, the invention provides a method for rapid separation and high-value utilization of an electrode material and a current collector, which utilizes the low-temperature volatilization and decomposition characteristics of nickel tetracarbonyl, adopts CO to decompose the interface between the electrode material and the nickel-based current collector of a waste battery at a low temperature (50-70 ℃) so that the nickel-based current collector volatilizes nickel tetracarbonyl and is separated from the electrode material, and then decomposes the nickel tetracarbonyl into high-purity nickel powder and carbon monoxide at a relatively high temperature (230-. The invention can realize the rapid separation of the electrode material of the waste battery and the current collector, and the structure of the recovered electrode material is less damaged because the interface separation process is relatively mild and does not adopt strong acid and strong alkali, thereby being beneficial to the regeneration and the utilization of a physical method; the carbon monoxide medium can be recycled, and the current collector can be prepared into high-purity nickel powder, so that the added value is high and the cost is low.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (3)
1. A method for rapid separation and high-value utilization of an electrode material and a current collector is characterized by comprising the following steps:
removing an electrode plate from a waste battery, wherein the electrode plate comprises an electrode material and a nickel-based current collector fixedly connected with the electrode material through a binder;
putting the electrode plate into a heating furnace, introducing carbon monoxide gas into the heating furnace, heating to a preset temperature, and reacting a nickel-based current collector in the electrode plate with the carbon monoxide gas to generate gaseous Ni (CO)4Wherein the preset temperature is 50-70 ℃, and the reaction time of the carbon monoxide gas and the nickel-based current collector is 8-12 h;
recovering said gaseous Ni (CO)4Separating the electrode material from the nickel-based current collector;
for the recovered gaseous Ni (CO)4Carrying out heat treatment, and decomposing to obtain nickel powder and carbon monoxide, wherein the heat treatment temperature is 230-350 ℃;
calcining the residual electrode material and the binder in the heating furnace, removing the binder, and recovering the electrode material;
wherein the gas pressure in the heating furnace is less than or equal to 50 kPa;
the electrode plate is a positive plate or a negative plate, the positive plate comprises a positive material and a positive nickel-based current collector fixedly connected with the positive material through a binder, and the positive nickel-based current collector material is one of pure nickel, nickel alloy or nickel-plated material processed by a passivating agent;
the negative plate comprises a negative material and a negative nickel-based current collector fixedly connected with the negative material through a binder, wherein the negative nickel-based current collector material is one of pure nickel, nickel alloy or nickel-plated material.
2. The method for rapid separation and high-value utilization of the electrode material and the current collector according to claim 1, wherein the passivating agent is one or more of chromium salt, potassium permanganate, titanium salt, phosphate, molybdate, silicate and silane.
3. The method as claimed in claim 1, wherein the temperature of the calcination process is 600-700 ℃.
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