CN115377544A - Method for recovering lithium iron phosphate positive electrode material and separating current collector - Google Patents

Method for recovering lithium iron phosphate positive electrode material and separating current collector Download PDF

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Publication number
CN115377544A
CN115377544A CN202211101225.7A CN202211101225A CN115377544A CN 115377544 A CN115377544 A CN 115377544A CN 202211101225 A CN202211101225 A CN 202211101225A CN 115377544 A CN115377544 A CN 115377544A
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China
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current collector
positive electrode
iron phosphate
mixed
lithium iron
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Inventor
崔大祥
王金
张芳
卢玉英
葛美英
惠荣敏
焦靖华
张放为
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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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
    • 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
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Secondary Cells (AREA)
  • Primary Cells (AREA)

Abstract

The invention discloses a method for recovering a lithium iron phosphate positive electrode material and separating a current collector, which comprises the steps of crushing a positive electrode plate containing lithium iron phosphate in a powerful crusher to obtain a mixed material; placing the mixed material in a muffle furnace for pretreatment, carbonizing and gasifying the adhesive and the conductive agent in the positive electrode material, oxidizing a current collector, and then washing to remove residual carbon in the material; and (2) putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment material into the mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 0.3-2.5mol/L, and filtering to respectively obtain the anode material and the current collector containing material. The method can realize the separation and recovery of the anode material and the current collector, and further dissociate the adhesive macromolecular chains and the carbon conductive agent in the anode material film to separate the anode material, so that the anode material can be smoothly recycled.

Description

Method for recovering lithium iron phosphate positive electrode material and separating current collector
Technical Field
The invention relates to the field of lithium batteries, relates to a method for recovering a lithium iron phosphate positive electrode material and separating a current collector, and particularly relates to a method for recovering a positive electrode and separating a current collector from a waste lithium ion battery positive electrode.
Background
Due to the rapid development of technology in the past decade, lithium Ion Batteries (LIBs) have been vigorously developed in various fields. However, due to the limited operational life, more and more retired spent batteries face a severe accumulation. According to statistical results, the global lithium ion battery yield is over 5.8 hundred million as early as 2000, and reaches 30 hundred million by 2010. The yield of lithium batteries produced in China only reaches 78.42 hundred million by 2016. By 2020, there will be a large number of scrapped lithium ion batteries worldwide, the total number of which will reach 250 hundred million and the weight will be as high as 50 million tons. The waste lithium ion batteries contain a large amount of heavy metal components including lithium, nickel, cobalt, manganese and other elements, and if the elements are not well recovered, large-area pollution can be caused. Therefore, the recovery of the waste lithium ion battery is very important. The waste lithium ion battery is recycled, so that a large amount of metals can be recycled, the production cost is reduced, the pollution to the environment can be reduced, and meanwhile, the efficient recycling of battery materials plays a crucial role in the sustainable development of the battery industry. At present, the development trend of waste lithium ion battery recovery is gradually changed from the optimization of the traditional metallurgical process to the development of a more diversified and environment-friendly mode, the sustainability of the recovery process becomes an important evaluation factor, and the recovery and reutilization of the waste lithium ion battery to reduce the cost and realize sustainable production are very important.
The anode material is used as a key raw material of the battery core, directly determines the safety and development of the battery, and occupies the highest proportion of the material cost of the lithium ion battery. If the scrapped lithium ion batteries are directly discarded without being recycled, on one hand, the content of precious metal resources in the retired lithium ion batteries is far higher than that of natural ores, so that the metal elements in the retired lithium ion batteries are recycled, and the method is an important way for relieving the current situation of resource exhaustion and developing the recycling economy of the lithium ion batteries; on the other hand, the accumulation of a large amount of waste lithium ion batteries can cause potential pollution to the ecosystem. The recycling of the waste batteries can greatly reduce the negative impact on the environment. In addition, the potential safety hazards of ignition and explosion caused by the waste lithium ion batteries are not inconstant. Therefore, the resource recycling of the waste lithium batteries is urgent. The economic value of the waste lithium ion battery is furthest exerted, the negative influence of the waste lithium ion battery is reduced, and the stable and healthy development of the lithium ion battery industry can be guaranteed.
The positive electrode binder is generally polyvinylidene fluoride (PVDF), and because of strong binding effect, the positive electrode material is difficult to be completely separated from the aluminum foil by the common method. Therefore, the separation of the positive electrode material from the current collector aluminum foil becomes a key problem in the pretreatment process for lithium battery recycling. At present, in the method for recycling the anode material of the waste lithium ion battery, the separation of the anode material and the current collector, and the removal of the electrolyte and the binder component are very important links in the recycling. One type of method is as follows: the method comprises the steps of disassembling and stripping waste lithium iron phosphate batteries, calcining the collected positive pole pieces at high temperature, decomposing and losing the binder to separate positive active substances from current collector aluminum foils, and then screening to obtain lithium iron phosphate active substance powder. The treatment methods disclosed by the patent publications can destroy the original structure of the active material in the anode reclaimed material, have high energy consumption, generate carbon-containing gas in the process of removing carbon and a binder, increase the greenhouse effect to a certain extent and pollute the environment. Another type of method is: directly immersing the anode plate separated from the waste lithium ion battery into a sodium hydroxide solution, carrying out alkaline leaching to remove aluminum, and drying the aluminum-removed material obtained by filtering to obtain the anode active material. The method enables the filtrate to contain sodium aluminate, and increases the process for secondary recovery of aluminum metal.
Disclosure of Invention
The invention aims to provide a method for recovering a positive electrode material from a waste lithium battery positive electrode, which can dissolve an adhesive to realize the separation of the positive electrode material and a current collector to obtain a positive electrode material film and further dissociate adhesive macromolecular chains in the positive electrode material film to separate the positive electrode material, thereby smoothly obtaining the positive electrode material for recycling.
The purpose of the invention is realized by the following scheme: a method for recovering a lithium iron phosphate positive electrode material and a current collector comprises the following steps:
a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) The mixed material is placed in a muffle furnace for pretreatment, so that the adhesive and the conductive agent in the positive electrode material are carbonized and gasified, the current collector is oxidized, and then washing treatment is carried out to remove residual carbon in the material;
(c) And (2) putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment material into the mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 0.3-2.5mol/L, and filtering to respectively obtain the anode material and the current collector containing material.
The power of the strong force pulverizer in the step (a) is 350-1100W.
In the step (b), the oxidation temperature is 150-400 ℃, the temperature rise rate is 3-8 ℃/min, and the heat preservation time is 2-5h.
The strong base in step (c) is sodium hydroxide, potassium hydroxide or lithium hydroxide.
The mass ratio of the mixed positive electrode material to the strong base in the step (c) is (0.5-15): 1.15.
placing the cathode material film in the strong alkali mixed solution in the step (c), and when freezing/pyrolysis is repeatedly carried out, stirring the mixed solution, heating to 40-80 ℃, and then cooling to a temperature below a freezing point for freezing; and then heating and raising the temperature for continuous reaction, cooling to below a freezing point after stirring, freezing, and repeatedly dissolving a current collector in the positive electrode material.
The temperature range for cooling to below freezing point for freezing is-40 to-10 ℃, and the temperature range for melting and unfreezing the solution when the temperature is raised to above freezing point is 5 to 20 ℃.
The invention has the beneficial effects that the method is different from the prior method of crushing or calcining the whole battery or the positive pole piece, and the like, the method obtains the mixed material by crushing through a crusher; then carbonizing, washing to separate the adhesive and the conductive agent in the anode material, and primarily purifying the recovered anode material; preferably, the above materials are placed in a strong alkaline solution, freezing/dissolving is repeatedly performed to dissolve the metal oxide (mainly, the current collector) in the pretreatment material in the mixed solution, and the purified positive electrode material and the current collector-containing material are obtained by filtration, respectively. The key point of the method is that the carbonization treatment and the alkali treatment: the adhesive and the conductive agent in the pole piece can be easily removed by carbonization treatment, and the structure of the material can not be influenced. The current collector and the impurity metal salt are further separated by alkali treatment, and when the concentration of the alkali is higher, the longer the treatment time is, the better the effect is.
Drawings
FIG. 1 is a flow chart of the method of the present invention;
fig. 2 is an XRD spectrum of the lithium iron phosphate as the cathode material recovered in example 1 of the present invention.
Detailed Description
For further explanation of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings.
In the early treatment, the waste lithium ion battery is subjected to discharge treatment, and a positive pole piece, a negative pole piece, a battery shell and a diaphragm of the battery are disassembled and separated by a physical method, wherein the positive pole piece is reserved.
Example 1
The steps of recovering the lithium iron phosphate anode material and the current collector are shown in the flow chart of the method in figure 1, and the method comprises the following steps:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace, pretreating for 1.5h at 180 ℃ to carbonize and gasify the adhesive and the conductive agent in the positive electrode material, oxidize the current collector, and then washing to remove residual carbon in the mixed material to obtain a pretreated mixed material;
(c) And (c) placing the pretreated mixed material obtained in the step (b) into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreated material into a sodium hydroxide solution to obtain a strong alkali mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 1.2mol/L, the mass ratio of the mixed material to the sodium hydroxide solution is 8.
After the current collector is stripped, the recycled lithium iron phosphate material is respectively subjected to XRD characterization, the spectrogram is shown in figure 2, and spectrogram data shows that the adhesive is removed through the treatment, so that the positive active material lithium iron phosphate is obtained.
After the lithium iron phosphate positive plate is recycled by using the method, the aluminum content of the black powder is less than 1 percent, and the black powder content in the aluminum powder is less than 10 percent; after the lithium iron phosphate non-injected liquid waste laminated pole core (the water content is less than 0.1 percent and no aluminum shell is contained) is recycled, the aluminum content of the black powder is less than 1 percent, and the black powder content of the aluminum compound is less than 10 percent.
Example 2
And (3) recovering the lithium iron phosphate anode material and the current collector, wherein the steps are similar to those of the embodiment 1, and the method comprises the following steps:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace, pretreating for 1.5h at 220 ℃ to carbonize and gasify the adhesive and the conductive agent in the positive electrode material, oxidizing a current collector, and then washing to remove residual carbon in the material;
(c) And (2) putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment material into the mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 1.2mol/L, and filtering to respectively obtain the anode material and the current collector-containing material. The mass ratio of the mixed material to the sodium hydroxide solution is 10.
After the current collector was peeled off, the XRD characterization results of the recovered lithium iron phosphate materials were the same as those in example 1, respectively, to obtain a positive active material, lithium iron phosphate.
Example 3
And (3) recovering the lithium iron phosphate anode material and the current collector, wherein the steps are similar to those of the embodiment 1, and the method comprises the following steps:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace, pretreating for 1.5h at 260 ℃ to carbonize and gasify the adhesive and the conductive agent in the positive electrode material, oxidizing a current collector, and then washing to remove residual carbon in the material;
(c) And (2) putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment material into the mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 1.2mol/L, and filtering to respectively obtain the anode material and the current collector-containing material. The mass ratio of the mixed material to the sodium hydroxide solution is 12.
After the current collector is stripped, XRD characterization results of the recovered lithium iron phosphate material are the same as those in example 1, respectively, to obtain a positive active material, lithium iron phosphate.

Claims (9)

1. A method for recovering a lithium iron phosphate positive electrode material and a current collector is characterized by comprising the following steps:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace for pretreatment, carbonizing and gasifying the adhesive and the conductive agent in the positive electrode material, oxidizing a current collector, and then washing to remove residual carbon in the material;
(c) Putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment materials into the strong alkali solution to obtain a strong alkali mixed solution, wherein the mass ratio of the mixed positive electrode material to the strong alkali is (0.5-15): 1.15, the concentration of strong base in the strong base mixed solution is 0.3-2.5mol/L, and the positive electrode material and the current collector containing material are obtained by filtering respectively.
2. The method for recycling the lithium iron phosphate positive electrode material and the current collector in the step (a) as claimed in claim 1, wherein the power of the powerful pulverizer in the step (a) is 350-1100W.
3. The method for recycling the lithium iron phosphate positive electrode material and the current collector as claimed in claim 1, wherein the oxidation temperature in the step (b) is 150-400 ℃, the temperature rise rate is 3-8 ℃/min, and the holding time is 2-5h.
4. The method for recycling the lithium iron phosphate positive electrode material and the current collector as claimed in claim 1, wherein the strong base in the step (c) is sodium hydroxide, potassium hydroxide or lithium hydroxide.
5. The method for recovering the lithium iron phosphate cathode material and the current collector as claimed in claim 1, wherein in the step (c), the cathode material film is placed in a strong alkali mixed solution, and when freezing/pyrolysis is repeatedly performed, the mixed solution is stirred and heated to 40-80 ℃, and then cooled to a temperature below the freezing point for freezing; and then heating to raise the temperature for continuous reaction, cooling to below the freezing point after stirring, freezing, and repeatedly dissolving the current collector in the positive electrode material.
6. The method for recovering the lithium iron phosphate positive electrode material and the current collector as claimed in claim 5, wherein the temperature range for cooling to below the freezing point for freezing is-40 to-10 ℃, and the temperature range for melting and unfreezing the solution heated to above the freezing point is 5 to 20 ℃.
7. The method for recovering the lithium iron phosphate positive electrode material and the current collector as recited in any one of claims 1 to 6, comprising the steps of:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace, pretreating for 1.5h at 180 ℃ to carbonize and gasify the adhesive and the conductive agent in the positive electrode material, oxidize the current collector, and then washing to remove residual carbon in the mixed material to obtain a pretreated mixed material;
(c) Putting the pretreated mixed material obtained in the step (b) into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreated material into a sodium hydroxide solution to obtain a strong alkali mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 1.2mol/L, the mass ratio of the mixed material to the sodium hydroxide solution is 8.15, and filtering to respectively obtain a positive electrode material lithium iron phosphate and a current collector-containing material.
8. The method for recovering the lithium iron phosphate positive electrode material and the current collector as recited in any one of claims 1 to 6, comprising the steps of:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace, pretreating for 1.5 hours at 220 ℃ to carbonize and gasify the adhesive and the conductive agent in the anode material, oxidizing a current collector, and then washing to remove residual carbon in the material;
(c) And (2) putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment material into the mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 1.2mol/L, and filtering to respectively obtain the anode material and the current collector-containing material. The mass ratio of the mixed material to the sodium hydroxide solution is 10.
9. The method for recycling the lithium iron phosphate positive electrode material and the current collector as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
(a) Crushing the positive pole piece containing the lithium iron phosphate in a powerful crusher to obtain a mixed material;
(b) Placing the mixed material in a muffle furnace, pretreating for 1.5h at 260 ℃ to carbonize and gasify the adhesive and the conductive agent in the positive electrode material, oxidizing a current collector, and then washing to remove residual carbon in the material;
(c) And (2) putting the materials into a strong alkali solution, repeatedly freezing/dissolving to dissolve the metal oxide in the pretreatment material into the mixed solution, wherein the concentration of strong alkali in the strong alkali mixed solution is 1.2mol/L, and filtering to respectively obtain the anode material and the current collector containing material. The mass ratio of the mixed material to the sodium hydroxide solution is 12.
CN202211101225.7A 2022-09-09 2022-09-09 Method for recovering lithium iron phosphate positive electrode material and separating current collector Pending CN115377544A (en)

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Application Number Priority Date Filing Date Title
CN202211101225.7A CN115377544A (en) 2022-09-09 2022-09-09 Method for recovering lithium iron phosphate positive electrode material and separating current collector

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