CN115784192B - Method for recycling positive electrode powder of lithium iron phosphate battery - Google Patents
Method for recycling positive electrode powder of lithium iron phosphate battery Download PDFInfo
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Abstract
The invention relates to a method for recycling lithium iron phosphate battery positive electrode powder, and belongs to the field of waste battery treatment and resource utilization. The recovery method of the lithium iron phosphate battery anode powder comprises the following steps: 1) Discharging and disassembling the lithium iron phosphate battery, and collecting the positive plate and the diaphragm; 2) After stacking the positive plate and the diaphragm, performing oxygen consumption heat treatment in an air atmosphere; the treatment temperature of the oxygen consumption heat treatment is 350-550 ℃; 3) And carrying out mechanical separation treatment on the positive plate subjected to oxygen consumption heat treatment to obtain lithium iron phosphate positive powder. According to the invention, the positive plate and the diaphragm are stacked and then subjected to oxygen consumption heat treatment at 350-550 ℃, oxygen in the heat treatment equipment for consuming the diaphragm is carbonized, and the positive powder in the positive plate is effectively, quickly and completely separated from the aluminum foil material, so that the method has the advantages of low cost, greenness and high efficiency.
Description
Technical Field
The invention relates to a method for recycling lithium iron phosphate battery positive electrode powder, and belongs to the field of waste battery treatment and resource utilization.
Background
The high current installed rates of lithium iron phosphate batteries also mean that greater decommissioning and scrap volumes will be encountered in the future. Along with the gradual increase of the scrapped amount of the lithium iron phosphate battery and the gradual consumption of lithium resources in the global scope, the waste lithium iron phosphate battery is necessary to be subjected to harmless treatment and recycling. The lithium iron phosphate battery consists of a positive plate, a negative plate, a diaphragm, electrolyte, a shell and the like, wherein the positive plate contains lithium iron phosphate positive powder, aluminum foil and a binder, contains abundant metal resources such as iron, lithium, aluminum and the like, and is a main research object of a recovery technology. Because the lithium iron phosphate battery does not contain other high-value metals, the recovery value is relatively low compared with other waste lithium ion batteries, and therefore, the recovery method has higher requirements on high efficiency and low cost.
The recovery process in the prior art comprises the steps of battery pack disassembly, cell discharge and the like of the waste lithium iron phosphate battery, primarily sorting to obtain a positive plate, removing organic matters such as a binder and the like in the positive plate in a mode of organic dissolution or roasting/calcining and the like, so that positive plate powder falls off from an aluminum foil and is collected, and subsequently, carrying out wet extraction on the positive plate powder to obtain lithium, namely adding hydrogen peroxide as an auxiliary agent under a dilute sulfuric acid system, and extracting valuable metal lithium in the positive plate powder by acid leaching to prepare a lithium carbonate product. The method of organic dissolution can better realize the dissociation and falling of the positive electrode powder, but the organic solvent has higher cost and difficult recycling; in the roasting/calcining mode, the lithium iron phosphate material is easy to oxidize in air atmosphere to change the mineral phase, and the roasting/calcining mode also can cause embrittlement of aluminum foil on the pole piece, so that the aluminum content in the recovered positive electrode powder is higher, and the aluminum content can have adverse effect on subsequent wet extraction of lithium. In addition, the binder is easy to generate toxic gas during roasting/calcining, and brings potential safety hazard to the operating environment.
Disclosure of Invention
The invention aims to provide a recovery method of lithium iron phosphate battery positive electrode powder, which can realize high-efficiency and low-cost separation of the lithium iron phosphate positive electrode powder.
The invention relates to a recovery method of lithium iron phosphate battery positive electrode powder, which adopts the following scheme:
the method for recycling the positive electrode powder of the lithium iron phosphate battery comprises the following steps: 1) Discharging and disassembling the lithium iron phosphate battery, and collecting the positive plate and the diaphragm; 2) After stacking the positive plate and the diaphragm, performing oxygen consumption heat treatment in an air atmosphere; the treatment temperature of the oxygen consumption heat treatment is 350-550 ℃; 3) And carrying out mechanical separation treatment on the positive plate subjected to oxygen consumption heat treatment to obtain lithium iron phosphate positive powder. According to the invention, after the positive plate and the diaphragm are stacked, oxygen consumption heat treatment is carried out at 350-550 ℃, the treatment temperature is relatively lower than that of a common roasting/calcining process, and in the process, the diaphragm undergoes oxidation reaction in an air atmosphere, so that oxygen in the heat treatment equipment is consumed, hydrogen, carbon dioxide and micromolecular alkane gas are released, the inside of the heat treatment equipment is kept at positive pressure, and an anoxic or anaerobic condition is formed; the lithium iron phosphate material in the positive plate has stable ore phase under the oxygen consumption heat treatment condition, and is favorable for avoiding the oxidation reaction of the positive plate material to form Li which is difficult to leach 3 Fe 2 (PO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the In addition, the binder in the positive plate is under the anaerobic or anoxic conditionThermal decomposition occurs, and the generation of toxic and harmful gases is reduced; after the oxygen consumption heat treatment is finished, the carbon ash is formed by carbonizing the diaphragm to complete the treatment of solid waste, the binder is thermally decomposed, and the residual positive electrode powder in the positive electrode plate and the aluminum foil material can be completely separated in a high-efficiency and rapid manner only through a vibration, beating or grinding mechanical separation mode, and the method has the advantages of low cost, greenness and high efficiency.
Preferably, the stacking of the positive plate and the separator is performed by stacking the positive plate and the separator according to the layer ratio of the positive plate to the separator of (1-5): 1 are alternately stacked. The positive plate and the diaphragm are mixed according to the layer number ratio of the positive plate to the diaphragm of (1-5): 1 is to place 1-5 layers of positive plates alternately, and then place 1 layer of diaphragm sheet at the adjacent position of the positive plates, and adopt a mode of alternately stacking 1-5 layers of positive plates and 1 layer of diaphragm sheet, so that the oxygen consumption effect of the diaphragm sheet can be fully exerted, the condition of oxygen deficiency or no oxygen is rapidly achieved around the positive plates, and the generation of harmful gas and positive powder oxidation in the heat treatment process is avoided.
Further, the lower limit of the layer number ratio of the positive plate to the diaphragm when the positive plate and the diaphragm are stacked is selected from 1: 1. 2: 1. 3: 1. 4: 1; the upper limit of the layer number ratio of the positive plate to the diaphragm is selected from 2: 1. 3: 1. 4: 1. 5: 1; the layer number ratio of the positive plate to the diaphragm is in a range formed by selecting any proportion from a lower limit and an upper limit when the positive plate and the diaphragm are stacked.
Further, stacking the positive plate and the diaphragm, wherein the positive plate and the diaphragm are stacked according to the layer number ratio of the positive plate to the diaphragm of (2-3): 1 are alternately stacked. According to the invention, the stacking layer ratio of the positive plate to the diaphragm is controlled, so that the diaphragm can rapidly and thoroughly consume oxygen around the positive plate in the oxygen consumption heat treatment process, the positive powder is promoted to keep the mineral phase stable, and the extraction efficiency of the subsequent wet extraction process of lithium is improved.
Preferably, after the membrane is collected, the membrane is sheared along the folded position to obtain a single membrane. The diaphragm can adapt to the size of the positive plate after being sheared along the folding position, is beneficial to fully contacting with the positive plate during subsequent stacking, and therefore consumes oxygen around the positive plate during heat treatment.
Preferably, the temperature rising rate of the oxygen consumption heat treatment is 5-10 ℃/min; the treatment time of the oxygen consumption heat treatment is 10-120 min.
Further, the lower temperature limit of the oxygen-consuming heat treatment is selected from any one value of 350 ℃, 375 ℃, 400 ℃, 425 ℃, 450 ℃, 475 ℃, 500 ℃ and 525 ℃, the upper temperature limit of the oxygen-consuming heat treatment is selected from any one value of 375 ℃, 400 ℃, 425 ℃, 450 ℃, 475 ℃, 500 ℃, 525 ℃ and 550 ℃, and the temperature of the oxygen-consuming heat treatment is in a range formed by any one value of the lower limit and the upper limit.
Further, the lower limit of the treatment time of the oxygen consumption heat treatment is any one value selected from 10min, 20min, 40min, 60min, 80min and 100min, the upper limit of the treatment time of the oxygen consumption heat treatment is any one value selected from 20min, 40min, 60min, 80min, 100min and 120min, and the treatment time of the oxygen consumption heat treatment is a range formed by any one value selected from the lower limit and the upper limit.
Preferably, the treatment temperature of the oxygen-consuming heat treatment is 400-500 ℃; the treatment time of the oxygen consumption heat treatment is 60-90 min. The temperature is favorable for promoting the oxygen consumption heat treatment, so that the binder in the positive plate is better decomposed, the separation efficiency of the positive plate powder and the aluminum foil is improved, and meanwhile, compared with the higher heat treatment temperature, the temperature range has the advantages of ensuring high-efficiency treatment and saving cost.
Preferably, the separator is made of polypropylene and/or polyethylene.
Preferably, the heat treatment equipment used for the oxygen consumption heat treatment is of a fixed bed structure and is provided with a pyrolysis gas outlet. According to the invention, the diaphragm is used for oxygen consumption heat treatment, the pyrolysis gas is released while oxygen is consumed, air in the equipment is not required to be discharged before the oxygen consumption heat treatment, and the oxygen-deficient or anaerobic condition can be formed in the heat treatment equipment without protection of nitrogen or inert atmosphere in the oxygen consumption heat treatment process, so that the operation is simple and convenient, the process is simplified, and the cost is saved.
Preferably, the mechanical separation treatment is rod milling, and the time of the mechanical separation treatment is 1-30 min.
Further, the lower time limit of the mechanical separation treatment is selected from any one of 1 min, 5 min, 10min, 15 min, 20min and 25 min, the upper time limit of the mechanical separation treatment is selected from any one of 5 min, 10min, 15 min, 20min, 25 min and 30min, and the time of the mechanical separation treatment is selected from the range consisting of any one of the lower limit and the upper limit.
Preferably, the method further comprises cooling the positive electrode sheet after heat treatment before mechanical separation treatment.
Further, the cooling is natural cooling.
Preferably, in the oxygen consumption heat treatment, the membrane consumes oxygen in the air to realize carbonization; and the binder in the positive plate is thermally decomposed under the anaerobic condition.
For simplicity, only a few numerical ranges are explicitly disclosed. However, any lower limit may be combined with any upper limit to form a range not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and any upper limit may be combined with any other upper limit to form a range not explicitly recited. Furthermore, each point or individual value between the endpoints of the range is included within the range, although not explicitly recited. Thus, each point or individual value may be combined as a lower or upper limit on itself with any other point or individual value or with other lower or upper limit to form a range that is not explicitly recited.
Drawings
FIG. 1 is an XRD pattern of lithium iron phosphate positive electrode powder obtained in example 1;
FIG. 2 is an XRD pattern of the lithium iron phosphate positive electrode powder obtained in comparative example 1;
in the figure, 1-LiFePO 4 Phase, 2-Li 3 Fe 2 (PO 4 ) 3 And (3) phase (C).
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Examples
The following description of the embodiments of the present invention will be made with reference to specific examples, wherein the raw materials used in the examples are all from common commercial products and the equipment or apparatus used are all from conventional commercial sources.
Example 1
The method for recycling the positive electrode powder of the lithium iron phosphate battery comprises the following steps:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting the positive plate and the diaphragm; the diaphragm is made of polypropylene, and is sheared along the folding position to obtain a single diaphragm;
2) The positive plate and the single diaphragm are mixed according to the layer number ratio of the positive plate to the diaphragm of 2:1, alternately stacking, punching the stacked objects, hanging the stacked objects in the center of heat treatment equipment through a hook, and performing oxygen consumption heat treatment in air atmosphere: heating the heat treatment heat equipment provided with the positive plate and the diaphragm to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 60min, wherein the diaphragm consumes oxygen in the air to realize carbonization, carbon ash is formed, and the binder in the positive plate is thermally decomposed under the anaerobic condition;
3) Cooling the positive plate subjected to oxygen consumption heat treatment to room temperature, and mechanically colliding and rubbing for 10min through a rod mill to obtain lithium iron phosphate positive powder and aluminum foil, wherein the falling rate of the lithium iron phosphate positive powder is 99.9%; and adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder to leach, wherein the lithium leaching rate is 99.2%.
Example 2
The method for recycling the positive electrode powder of the lithium iron phosphate battery comprises the following steps:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting the positive plate and the diaphragm; the diaphragm is made of polypropylene, and is sheared along the folding position to obtain a single diaphragm;
2) The positive plate and the single diaphragm are mixed according to the layer number ratio of the positive plate to the diaphragm of 2:1, alternately stacking, punching the stacked objects, hanging the stacked objects in the center of heat treatment equipment through a hook, and performing oxygen consumption heat treatment in air atmosphere: heating the heat treatment heat equipment provided with the positive plate and the diaphragm to 350 ℃ at a heating rate of 5 ℃/min and preserving heat for 60min, wherein the diaphragm consumes oxygen in the air to realize carbonization, carbon ash is formed, and the binder in the positive plate is thermally decomposed under the anaerobic condition;
3) Cooling the positive plate subjected to oxygen consumption heat treatment to room temperature, and mechanically colliding and rubbing for 10min through a rod mill to obtain lithium iron phosphate positive powder and aluminum foil, wherein the falling rate of the lithium iron phosphate positive powder is 86.2%; and adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder to leach, wherein the lithium leaching rate is 87.9%.
Example 3
The method for recycling the positive electrode powder of the lithium iron phosphate battery comprises the following steps:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting the positive plate and the diaphragm; the diaphragm is made of polyethylene, and is sheared along the folding position to obtain a single diaphragm;
2) The positive plate and the single diaphragm are mixed according to the layer ratio of the positive plate to the diaphragm of 5:1, alternately stacking, punching the stacked objects, hanging the stacked objects in the center of heat treatment equipment through a hook, and performing oxygen consumption heat treatment in air atmosphere: heating the heat treatment heat equipment provided with the positive plate and the diaphragm to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 60min, wherein the diaphragm consumes oxygen in the air to realize carbonization, carbon ash is formed, and the binder in the positive plate is thermally decomposed under the anaerobic condition;
3) Cooling the positive plate subjected to oxygen consumption heat treatment to room temperature, and mechanically colliding and rubbing for 10min through a rod mill to obtain lithium iron phosphate positive powder and aluminum foil, wherein the falling rate of the lithium iron phosphate positive powder is 99.0%; and adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder to leach, wherein the lithium leaching rate is 93.5%.
Comparative example 1
The recovery method of the positive electrode powder of the lithium iron phosphate battery of this comparative example differs from that of example 1 only in that:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting a positive plate;
2) After punching the positive plate, hanging the positive plate at the center of a heat treatment device through a hook, and carrying out heat treatment in an air atmosphere: heating the heat treatment hot standby provided with the positive plate and the diaphragm to 450 ℃ at a heating rate of 5 ℃/min and preserving heat for 60min, wherein the binder in the positive plate is thermally decomposed;
3) Cooling the heat-treated positive plate to room temperature, and mechanically colliding and rubbing for 10min through a rod mill to obtain lithium iron phosphate positive powder and aluminum foil, wherein the falling rate of the lithium iron phosphate positive powder is 98.3%; and adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder to leach, wherein the lithium leaching rate is 68.5%.
Experimental example
XRD tests were performed on the lithium iron phosphate positive electrode powders obtained in example 1 and comparative example 1, and XRD patterns of both are shown in fig. 1 and fig. 2, respectively. As can be seen from fig. 1 to 2, the recovery method of comparative example 1 generates Li by partially changing the ore phase of the positive electrode powder of the lithium iron phosphate battery after heat treatment 3 Fe 2 (PO 4 ) 3 The ore phase is unfavorable for the subsequent wet leaching extraction of lithium element; in the recovery method of the embodiment 1, in the oxygen consumption heat treatment process, the positive electrode powder ore phase of the lithium iron phosphate battery is stable, so that the selective and efficient extraction of the subsequent lithium is facilitated.
The heat treatment parameters and positive electrode powder recovery data of examples 1 to 3 and comparative example 1 are shown in table 1 below:
table 1 heat treatment parameters and positive electrode powder recovery data of examples 1 to 3 and comparative example 1
As can be seen from Table 1, the recovery method of the positive electrode powder of the lithium iron phosphate battery of examples 1 to 3 is easy to separate from the aluminum foil after oxygen-consuming heat treatment, the positive electrode powder falling rate is high and reaches 86.2 to 99.9%, wherein the positive electrode powder falling rates of examples 1 and 3 with the heat treatment temperature above 450 ℃ reach 99.0 to 99.9%, and excellent separation effect is shown; meanwhile, the positive electrode powder in the embodiment 1-3 keeps stable mineral phase after heat treatment, has extremely high lithium leaching rate, and reaches 87.9-99.2%; compared with comparative example 1, the example 1 adopting the same heat treatment parameters shows that the invention is beneficial to separating the positive electrode powder from the aluminum foil and stabilizing the ore phase of the positive electrode powder by heat treatment after stacking the positive electrode plate and the diaphragm, the falling rate of the positive electrode powder is improved by 1.6%, the lithium leaching rate is improved by 30.7%, and the recovery efficiency of the positive electrode powder of the lithium iron phosphate battery is greatly improved.
The applicant states that the detailed method of the present invention is illustrated by the above examples, but the present invention is not limited to the detailed method described above, i.e. it does not mean that the present invention must be practiced in dependence upon the detailed method described above. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (9)
1. The method for recycling the positive electrode powder of the lithium iron phosphate battery is characterized by comprising the following steps of:
1) Discharging and disassembling the lithium iron phosphate battery, and collecting the positive plate and the diaphragm;
2) After stacking the positive plate and the diaphragm, performing oxygen consumption heat treatment in an air atmosphere; the treatment temperature of the oxygen consumption heat treatment is 350-550 ℃; after the oxygen consumption heat treatment is finished, carbonizing the diaphragm to form carbon ash, and thermally decomposing the binder;
3) And carrying out mechanical separation treatment on the positive plate subjected to oxygen consumption heat treatment to obtain lithium iron phosphate positive powder.
2. The method for recycling positive electrode powder of lithium iron phosphate battery according to claim 1, wherein the stacking of the positive electrode plate and the separator is performed by the steps of: 1 are alternately stacked.
3. The method for recycling lithium iron phosphate battery positive electrode powder according to claim 2, wherein the stacking of the positive electrode plate and the separator is performed by the steps of (2-3) according to the layer ratio of the positive electrode plate to the separator: 1 are alternately stacked.
4. The method for recycling the lithium iron phosphate battery positive electrode powder according to claim 1, wherein the temperature rising rate of the oxygen consumption heat treatment is 5-10 ℃/min; the treatment time of the oxygen consumption heat treatment is 10-120 min.
5. The method for recycling lithium iron phosphate battery positive electrode powder according to claim 4, wherein the treatment temperature of the oxygen consumption heat treatment is 400-500 ℃; the treatment time of the oxygen consumption heat treatment is 60-90 min.
6. The method for recycling lithium iron phosphate battery positive electrode powder according to claim 1, wherein the separator is made of polypropylene and/or polyethylene.
7. The method for recycling lithium iron phosphate battery positive electrode powder according to claim 1, wherein the mechanical separation treatment is rod milling, and the mechanical separation treatment time is 1-30 min.
8. The method for recycling lithium iron phosphate battery positive electrode powder according to claim 1, wherein the method further comprises cooling the positive electrode sheet after the heat treatment and before the mechanical separation treatment.
9. The method for recycling lithium iron phosphate battery positive electrode powder according to claim 1, wherein in the oxygen consumption heat treatment, the diaphragm consumes oxygen in the air to realize carbonization; and the binder in the positive plate is thermally decomposed under the anaerobic condition.
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| CN101383441B (en) * | 2007-09-06 | 2011-10-26 | 深圳市比克电池有限公司 | Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell |
| CN109904546A (en) * | 2017-12-08 | 2019-06-18 | 北京有色金属研究总院 | The technique of aluminium foil and positive electrode is recycled from applying waste lithium ionic power battery |
| CN111934042B (en) * | 2020-08-03 | 2023-01-31 | 新乡市力科循环技术有限公司 | Physical recycling method for retired power battery |
| CN113083848A (en) * | 2021-03-10 | 2021-07-09 | 深圳清研装备科技有限公司 | Sorting and recycling method for positive and negative electrode materials of waste lithium iron phosphate batteries |
| CN114335781A (en) * | 2021-12-27 | 2022-04-12 | 上海电力大学 | Method for extracting precious metal from waste lithium battery |
| CN114752769B (en) * | 2022-04-08 | 2023-09-22 | 中国矿业大学 | Method for recycling valuable metals of waste lithium battery materials assisted by diaphragm pyrolysis |
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