CN112310502A - Method for recycling and reusing anode material of waste lithium manganate lithium ion battery - Google Patents
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Abstract
The invention discloses a method for recycling and reusing a waste lithium manganate lithium ion battery anode material. The method can recover LiMn from the waste lithium ion battery2O4Anode scrap and production of Li1+xMnyFe1‑yPO4the/C next-generation lithium ion battery anode material has the advantages of greenness, high efficiency, short flow and low cost.
Description
Technical Field
The invention relates to a lithium ion battery technology, in particular to a method for recycling and reusing a waste lithium manganate lithium ion battery anode material.
Background
Lithium ion batteries are widely used in electronic devices such as portable electronic devices, pure electric vehicles, and hybrid electric vehicles due to their advantages of high energy density, long cycle life, and no memory effect, but the amount of waste batteries increases with the mass production and wide use of lithium ion batteries. If the waste batteries are not reasonably treated in time, a large amount of environmental pollution and resource waste can be caused. Therefore, it is very important to effectively and reasonably recycle the waste lithium ion battery from both the environmental viewpoint and the economic benefit.
Among the various types of lithium ion batteries, lithium manganate (LiMn)2O4) The batteries have larger market share due to the low cost, and are accompanied with the generation of a large amount of waste lithium manganate batteries, wherein the waste lithium manganate batteries contain a large amount of non-renewable lithium elements and manganese elements. Therefore, the recycling of the oxide cathode material is of great significance for solving the environmental problem generated by the waste lithium ion battery and relieving the shortage of non-renewable lithium and transition metal resources.
LiMn2O4The cathode material has poor cycle stability due to the Zingiber effect, and high energy density and excellent cycle stability are the key points of the next generation of lithium ion batteries, such as phosphate material, due to highly stable PO4 3-The tetrahedral framework can be used as an ideal oxide positive electrode substitute of a lithium ion battery, and has excellent cycle stability. Therefore, the waste LiMn2O4The recovery of the anode material and the preparation of the next generation of the phosphate anode material are a research direction for recovering waste lithium ion battery materials, but at present, the research is less, and the technology is not mature.
The invention with Chinese patent publication No. CN111333048A discloses a method for preparing lithium manganese iron phosphate by using waste lithium iron phosphate and lithium manganate materials, which comprises the steps of respectively carrying out acid leaching on obtained lithium manganate waste and lithium iron phosphate waste, and then preparing a lithium manganese iron phosphate anode material by using a coprecipitation method and a high-temperature solid phase method, wherein the acid in the leachate obtained by the method cannot be reused, and the next coprecipitation can be carried out only by carrying out neutralization treatment first, so that the waste of resources and inevitable secondary pollution are caused.
The existing waste lithium ion battery recovery technology still has the problems of low recovery efficiency, low utilization rate of leached acid, secondary pollution, high recovery cost and the like.
Disclosure of Invention
The invention aims to provide a method for recycling and reusing a waste lithium manganate lithium ion battery anode material aiming at the defects of the prior art. The method can recover LiMn from the waste lithium ion battery2O4Anode scrap and production of Li1+xMnyFe1-yPO4the/C next-generation lithium ion battery anode material has the advantages of greenness, high efficiency, short flow and low cost.
The technical scheme for realizing the purpose of the invention is as follows:
a method for recycling and reusing a waste lithium manganate lithium ion battery anode material comprises the following steps:
1) fully discharging the waste lithium ion battery in a 5% NaCl solution, mechanically disassembling, and mechanically separating to obtain the positive electrode LiMn2O4Waste material, determining positive electrode LiMn by ICP or AAS analysis method2O4The content of Mn and Li in the waste;
2) leaching of LiMn2O4Waste materials: LiMn obtained in the last step2O4Adding the waste into a mixed solution of 0.1-4M acid leaching agent and 0.1-8M reducing agent for leaching, and fully reacting at a solid-to-liquid ratio of 5-100g/L, a reaction temperature of 20-100 ℃, a stirring speed of 100-2000rpm and a reaction time of 5-120min to ensure that the LiMn is reacted2O4Completely leaching Mn and Li in the solution, and filtering to obtain a leaching solution;
3) adding 0.01-2M lithium salt, 0.01-2M iron salt and 0.005-0.5M phosphoric acid or phosphate into the leachate obtained in step 2) to make Li, Fe, Mn and PO4 3-The target ratio is achieved, and the solution is fully stirred to obtain a uniformly mixed solution, wherein the target ratio meets the following requirements: li: mn: fe: PO (PO)4 3-1-y:1, x is more than or equal to 0 and less than or equal to 0.3, y is more than or equal to 0 and less than 1, and the stirring time isStirring for 30-240 min at 30-80 deg.C;
4) carrying out spray drying on the solution obtained in the step 3) at the air inlet temperature of 200-;
5) calcining the precursor material in nitrogen or argon in inert atmosphere, heating from room temperature to 350-plus-450 ℃ presintering temperature at the heating rate of 1-10 ℃/min, keeping the temperature for 2-6h, continuing heating to the reaction temperature of 550-plus-750 ℃, keeping the temperature for 3-15h, and naturally cooling to obtain Li1+xMnyFe1-yPO4a/C positive electrode material;
6) with Li1+xMnyFe1-yPO4and/C is the positive electrode material to prepare the button cell and evaluate the electrochemical performance: with Li1+xMnyFe1- yPO4The method comprises the following steps of taking/C as an electrode active material, SP as a conductive agent, PVDF as a binder, pulping according to a ratio of 80:10:10, fully and uniformly stirring the slurry, coating the slurry on an aluminum foil, drying the aluminum foil for 12 hours at 80 ℃, compacting a pole piece by using a roller press, cutting the pole piece into pole pieces with the diameter of 12 mm for later use, assembling a battery in a glove box in an argon atmosphere, taking a lithium piece as a negative electrode, taking a spare pole piece as a positive electrode, and taking 1M LiPF6Assembling the electrolyte and the diaphragm of the celgard 2400 to form the 2025 button cell, standing for 12 hours, and evaluating the electrochemistry of the 2025 button cell in a blue battery test system.
The acid leaching agent in the step 2 is phosphoric acid, pyrophosphoric acid containing or PO generated by reaction4 3-The inorganic acid of (1).
The reducing agent in the step 2 is a green organic compound with reducibility of citric acid and glucose.
The lithium salt in the step 3) is one or more of lithium citrate, lithium acetate, lithium nitrate, lithium carbonate, lithium sulfate and lithium dihydrogen phosphate.
The ferric salt in the step 3) is one or more of ferrous chloride, ferric nitrate, ferrous oxalate, ferric sulfate and ferric citrate.
The phosphate in the step 3) is one or more of diammonium hydrogen phosphate, ammonium dihydrogen phosphate and lithium dihydrogen phosphate.
The technical scheme can effectively recover the lithium manganate anode waste material, avoids the problems of resource waste and environmental pollution, and has the advantages of short flow, environmental protection and high efficiency, the acid leaching agent and the reducing agent added in the acid leaching process provide phosphate radicals and carbon sources for the regeneration of the material in the next step, the acid leaching agent and the reducing agent in the acid leaching process are effectively utilized, acid leaching waste liquid is not formed, the process not only effectively recovers valuable metals of the anode material of the waste lithium manganate lithium ion battery, but also regenerates the anode material Li of the next generation lithium ion battery1+xMnyFe1-yPO4And exhibits good electrochemical performance.
The method can recover LiMn from the waste lithium ion battery2O4Anode scrap and production of Li1+xMnyFe1- yPO4the/C next-generation lithium ion battery anode material has the advantages of greenness, high efficiency, short flow and low cost.
Drawings
FIG. 1 shows LiMn in example0.8Fe0.2PO4An XRD pattern of the anode material;
FIG. 2 shows LiMn in example0.8Fe0.2PO4SEM picture;
FIG. 3 shows LiMn in example0.8Fe0.2PO4A schematic diagram of a charge-discharge curve at a current density of 0.1C;
FIG. 4 shows LiMn in example0.75Fe0.25PO4SEM image.
Detailed Description
The invention will be further elucidated with reference to the drawings and examples, without however being limited thereto.
Example 1:
1) discharging the waste lithium ion battery in a 5% NaCl solution, mechanically disassembling, and mechanically separating to obtain waste LiMn2O4Determining the contents of Mn and Li in the positive electrode material to be 49.6% and 4.7% respectively by using an ICP (inductively coupled plasma) analysis method;
2) acid leaching waste LiMn2O4Materials: LiMn obtained in the step 1)2O4Adding the waste into a mixed solution of phosphoric acid with the concentration of 0.6M and citric acid with the concentration of 0.9M, reacting for 1h under the conditions that the solid-to-liquid ratio is 40 g/L, the reaction temperature is 60 ℃ and the stirring speed is 300 rpm, ensuring that the waste and the solution fully react, and filtering to obtain a leaching solution;
3) adding 0.2M lithium acetate, 0.4M ferrous chloride and 0.01M ammonium dihydrogen phosphate into the leaching solution obtained in the step 2) to ensure that Li, Mn, Fe and PO4 3-The ratio of (1: 0.8:0.2: 1);
4) carrying out spray drying on the solution obtained in the step 3), wherein the air inlet temperature is 250 ℃, the air outlet temperature is 150 ℃, and the feeding speed is 5ml/min, so as to obtain a precursor material;
5) calcining the precursor material in a nitrogen atmosphere, heating from room temperature to 450 ℃ at the heating rate of 5 ℃/min, preserving heat for 5h, continuously heating to 700 ℃ at the heating rate of 3 ℃/min, preserving heat for 10h, and naturally cooling to obtain the anode material LiMn0.8Fe0.2PO4/C,LiMn0.8Fe0.2PO4The SEM and XRD patterns of/C are shown in FIGS. 1 and 2, respectively, from which LiMn can be seen0.8Fe0.2PO4the/C is secondary spherical particles consisting of nanoscale primary particles, and the button cell prepared from the secondary spherical particles has excellent electrochemical performance, as shown in figure 3, the discharge specific capacity reaches 150 mAh g at 0.1C-1。
Example 2:
1) discharging the waste lithium ion battery in a 5% NaCl solution, mechanically disassembling, and mechanically separating to obtain waste LiMn2O4Determining the contents of Mn and Li in the positive electrode material to be 45.3% and 5.1% respectively by using an ICP (inductively coupled plasma) analysis method;
2) acid leaching of spent LiMn2O4 material: LiMn obtained in the step 1)2O4Adding the waste material into a mixed solution of phosphoric acid with the concentration of 1M and citric acid with the concentration of 1.5M, reacting for 30min under the conditions that the solid-to-liquid ratio is 100g/L, the reaction temperature is 70 ℃ and the stirring speed is 350rpm, ensuring that the waste material and the solution react fully, and filtering to obtain a leaching solution;
3) adding 0.3M lithium sulfate and 0.5M ferrous oxalate into the leaching solution obtained in the step 2) to ensure that Li, Mn, Fe and PO4 3-The ratio of (A) to (B) is 1:0.75:0.25: 1;
4) spray drying the solution obtained in the step 3), wherein the air inlet temperature is 220 ℃, the air outlet temperature is 150 ℃, and the feeding speed is 10ml/min, so as to obtain a precursor material;
5) calcining the precursor material in a nitrogen atmosphere, heating from room temperature to 400 ℃ at the heating rate of 3 ℃/min, preserving heat for 3h, continuing heating to 680 ℃ at the heating rate of 3 ℃/min, preserving heat for 10h, and naturally cooling to obtain the expected anode material LiMn0.75Fe0.25PO4,LiMn0.75Fe0.25PO4The SEM image is shown in figure 4, the lithium ion battery shows excellent electrochemical performance when applied to lithium ions, and the discharge specific capacity reaches 155 mAh g at 0.1C-1。
Example 3:
1) discharging the waste lithium ion battery in a 5% NaCl solution, mechanically disassembling, and mechanically separating to obtain waste LiMn2O4Determining the contents of Mn and Li in the positive electrode material to be 56.6% and 3.9% respectively by using an ICP (inductively coupled plasma) analysis method;
2) acid leaching waste LiMn2O4Materials: LiMn obtained in the step 1)2O4Adding the waste material into a mixed solution of phosphoric acid with the concentration of 0.2M and citric acid with the concentration of 0.4M, wherein the solid-to-liquid ratio is 20 g/L, the reaction temperature is 70 ℃, the stirring speed is 350rpm, the full reaction with the solution is ensured, and the leachate can be obtained by filtering;
3) adding 0.1M lithium nitrate and 0.2M ferric nitrate to the leaching solution obtained in the step 2) to ensure that Li, Mn, Fe and PO4 3-The ratio of (1.02: 0.5: 0.5): 1;
4) carrying out spray drying on the solution obtained in the step 3), wherein the air inlet temperature is 280 ℃, the air outlet temperature is 160 ℃, and the feeding speed is 8ml/min, so as to obtain a precursor material;
5) calcining the precursor material in a nitrogen atmosphere, heating from room temperature to 430 ℃ at the heating rate of 4 ℃/min, preserving heat for 4h, and continuing to performHeating to 720 ℃ at the speed of 3 ℃/min, preserving heat for 8h, and naturally cooling to obtain the expected anode material Li1.02Mn0.5Fe0.5PO4the/C shows excellent electrochemical performance when applied to lithium ions, and the specific discharge capacity can reach 123 mAh g under the current density of 10C-1The capacity retention rate is 90% after the 1C current density is circulated for 500 circles;
example 4:
1) discharging the waste lithium ion battery in a 5% NaCl solution, mechanically disassembling, and mechanically separating to obtain waste LiMn2O4Determining the contents of Mn and Li in the positive electrode material to be 45.8% and 4.9% respectively by using an ICP (inductively coupled plasma) analysis method;
2) acid leaching of spent LiMn2O4 material: LiMn obtained in the step 1)2O4Adding the waste material into a mixed solution of phosphoric acid with the concentration of 0.5M and citric acid with the concentration of 1.2M, wherein the solid-to-liquid ratio is 17 g/L, the reaction temperature is 50 ℃, the stirring speed is 250rpm, the full reaction with the solution is ensured, and the leachate can be obtained by filtering;
3) adding 0.1M lithium dihydrogen phosphate and 0.2M ferric sulfate into the leaching solution obtained in the step 2) to ensure that Li, Mn, Fe and PO4 3-The ratio of (1.02: 0.6: 0.4): 1;
4) carrying out spray drying on the solution obtained in the step 3), wherein the air inlet temperature is 220 ℃, the air outlet temperature is 160 ℃, and the feeding speed is 12ml/min, so as to obtain a precursor material;
5) calcining the precursor material in an argon atmosphere, heating to 380 ℃ from room temperature at the heating rate of 4 ℃/min, preserving heat for 5h, continuously heating to 750 ℃ at the heating rate of 2 ℃/min, preserving heat for 6h, and naturally cooling to obtain the expected anode material Li1.02Mn0.6Fe0.4PO4the/C shows excellent electrochemical performance when applied to lithium ions, and the discharge specific capacity reaches 161 mAh g under 0.1C-1And the specific discharge capacity under the current density of 10C can reach 115 mAh g-1。
Claims (6)
1. A method for recycling and reusing a waste lithium manganate lithium ion battery anode material is characterized by comprising the following steps:
1) fully discharging the waste lithium ion battery in a 5% NaCl solution, mechanically disassembling, and mechanically separating to obtain the positive electrode LiMn2O4Waste material, determining positive electrode LiMn by ICP or AAS analysis method2O4The content of Mn and Li in the waste;
2) leaching of LiMn2O4Waste materials: LiMn obtained in the last step2O4Adding the waste into a mixed solution of 0.1-4M acid leaching agent and 0.1-8M reducing agent for leaching, and fully reacting at a solid-to-liquid ratio of 5-100g/L, a reaction temperature of 20-100 ℃, a stirring speed of 100-2000rpm and a reaction time of 5-120min to ensure that the LiMn is reacted2O4Completely leaching Mn and Li in the solution, and filtering to obtain a leaching solution;
3) adding 0.01-2M lithium salt, 0.01-2M iron salt and 0.005-0.5M phosphoric acid or phosphate into the leachate obtained in step 2) to make Li, Fe, Mn and PO4 3-The target ratio is achieved, and the solution is fully stirred to obtain a uniformly mixed solution, wherein the target ratio meets the following requirements: li: mn: fe: PO (PO)4 3-1-y:1, x is more than or equal to 0 and less than or equal to 0.3, y is more than or equal to 0 and less than 1, the stirring time is 30-240 min, and the stirring temperature is 30-80 ℃;
4) carrying out spray drying on the solution obtained in the step 3) at the air inlet temperature of 200-;
5) calcining the precursor material in nitrogen or argon in inert atmosphere, heating from room temperature to 350-plus-450 ℃ presintering temperature at the heating rate of 1-10 ℃/min, keeping the temperature for 2-6h, continuing heating to the reaction temperature of 550-plus-750 ℃, keeping the temperature for 3-15h, and naturally cooling to obtain Li1+xMnyFe1-yPO4a/C positive electrode material;
6) with Li1+xMnyFe1-yPO4and/C is the positive electrode material to prepare the button cell and evaluate the electrochemical performance: with Li1+xMnyFe1- yPO4Performing pulping by using SP as conductive agent and PVDF as binder at a ratio of 80:10:10, and filling the pulp withUniformly stirring, coating on aluminum foil, drying at 80 ℃ for 12h, compacting a pole piece by using a roller press, cutting into pole pieces with the diameter of 12 mm for later use, assembling a battery in a glove box in argon atmosphere, taking a lithium piece as a negative electrode, taking a spare pole piece as a positive electrode, and taking 1M LiPF6Assembling the electrolyte and the diaphragm of the celgard 2400 to form the 2025 button cell, standing for 12 hours, and evaluating the electrochemistry of the 2025 button cell in a blue battery test system.
2. The method for recycling and reusing the anode material of the lithium ion battery containing waste lithium manganate as claimed in claim 1, wherein the acid leaching agent in step 2 is phosphoric acid, pyrophosphoric acid containing or PO generated by reaction4 3-The inorganic acid of (1).
3. The method for recycling and reusing the anode material of the waste lithium manganate lithium ion battery as claimed in claim 1, wherein the reducing agent in step 2 is a green organic compound with reducibility of citric acid and glucose.
4. The method for recycling and reusing the positive electrode material of the waste lithium manganate lithium ion battery as claimed in claim 1, wherein the lithium salt in step 3) is one or more of lithium citrate, lithium acetate, lithium nitrate, lithium carbonate, lithium sulfate and lithium dihydrogen phosphate.
5. The method for recycling and reusing the anode material of the waste lithium manganate lithium ion battery as claimed in claim 1, wherein the ferric salt in step 3) is one or more of ferrous chloride, ferric nitrate, ferrous oxalate, ferric sulfate and ferric citrate.
6. The method for recycling and reusing the anode material of the waste lithium manganate lithium ion battery as claimed in claim 1, wherein the phosphate in step 3) is one or more of diammonium hydrogen phosphate, ammonium dihydrogen phosphate and lithium dihydrogen phosphate.
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