CN115784192A - Method for recovering lithium iron phosphate battery positive electrode powder - Google Patents
Method for recovering lithium iron phosphate battery positive electrode powder Download PDFInfo
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- CN115784192A CN115784192A CN202310051199.XA CN202310051199A CN115784192A CN 115784192 A CN115784192 A CN 115784192A CN 202310051199 A CN202310051199 A CN 202310051199A CN 115784192 A CN115784192 A CN 115784192A
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- 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 relates to a method for recovering anode powder of a lithium iron phosphate battery, belonging to the field of waste battery treatment and resource utilization. The method for recovering the lithium iron phosphate battery positive electrode powder comprises the following steps: 1) Discharging and disassembling the lithium iron phosphate battery, and collecting a positive plate and a diaphragm; 2) Stacking the positive plate and the diaphragm, and then carrying out oxygen-consuming heat treatment in an air atmosphere; the treatment temperature of the oxygen-consuming heat treatment is 350-550 ℃; 3) And mechanically separating the positive plate subjected to the oxygen-consuming heat treatment to obtain the lithium iron phosphate positive powder. According to the invention, the anode plate and the diaphragm are stacked and then subjected to oxygen-consuming heat treatment at 350-550 ℃, the diaphragm consumes oxygen in heat treatment equipment to realize carbonization, and the anode powder and an aluminum foil material in the anode plate are completely separated efficiently, quickly and effectively, so that the method has the advantages of low cost, greenness and high efficiency.
Description
Technical Field
The invention relates to a method for recovering anode powder of a lithium iron phosphate battery, belonging to the field of waste battery treatment and resource utilization.
Background
The high installation probability of lithium iron phosphate batteries also means that the lithium iron phosphate batteries face a large amount of retirement and scrap in the future. Along with the increasing of the scrappage of the lithium iron phosphate battery and the gradual consumption of lithium resources in the global scope, the waste lithium iron phosphate battery needs to be subjected to harmless treatment and resource recycling. The lithium iron phosphate battery comprises a positive plate, a negative plate, a diaphragm, electrolyte, a shell and the like, wherein the lithium iron phosphate positive plate comprises lithium iron phosphate positive powder, aluminum foil and a binder, contains abundant iron, lithium, aluminum and other metal resources, and is a main research object of a recovery technology. Because the lithium iron phosphate battery does not contain other high-value metals, and the recovery value is relatively lower compared with other waste lithium ion batteries, the method has higher requirements on high efficiency and low cost of the recovery method.
The recovery process in the prior art comprises the steps of carrying out procedures such as battery pack disassembly and battery cell discharge on waste lithium iron phosphate batteries, carrying out preliminary separation to obtain a positive plate, removing organic matters such as a binder in the plate in organic dissolution or roasting/calcining and the like, so that positive powder falls off and is collected from an aluminum foil, and subsequently carrying out wet extraction on the positive powder, namely adding hydrogen peroxide as an auxiliary agent in a dilute sulfuric acid system, and extracting valuable metal lithium in the positive powder by acid leaching to prepare a lithium carbonate product. The organic dissolving mode can better realize the dissociation and the shedding of the anode powder, but the organic solvent has higher cost and is difficult to recycle; in the roasting/calcining mode, the ferric lithium phosphate material is easy to oxidize in the air atmosphere to change the mineral phase, and the roasting/calcining mode can also cause embrittlement of aluminum foil on the pole piece, so that the recovered positive pole powder has high aluminum content, which can generate adverse effects on the subsequent wet extraction of lithium. In addition, the binder is easy to generate toxic gas during roasting/calcining, and brings potential safety hazards to the operating environment.
Disclosure of Invention
The invention aims to provide a method for recovering 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 method for recovering anode powder of a lithium iron phosphate battery, which adopts the following scheme:
a method for recovering lithium iron phosphate battery positive electrode powder comprises the following steps: 1) Discharging and disassembling the lithium iron phosphate battery, and collecting a positive plate and a diaphragm; 2) Stacking the positive plate and the diaphragm, and then carrying out oxygen-consuming heat treatment in an air atmosphere; the treatment temperature of the oxygen-consuming heat treatment is 350-550 ℃; 3) And mechanically separating the positive plate subjected to the oxygen-consuming heat treatment to obtain the lithium iron phosphate positive powder. The positive plate and the diaphragm are stacked and then subjected to oxygen-consuming heat treatment at 350-550 ℃, the treatment temperature is relatively lower than that of a common roasting/calcining process, and the diaphragm is subjected to oxidation reaction in the air atmosphere in the process, so that oxygen in heat treatment equipment is consumed, hydrogen, carbon dioxide and micromolecular alkane gas are released, the interior of the heat treatment equipment is kept at positive pressure, and an oxygen-poor or oxygen-free condition is formed; the lithium iron phosphate material in the positive plate has stable mineral phase under the condition of the oxygen-consuming heat treatment of the invention, which is beneficial to avoiding the formation of difficult-to-leach Li caused by the oxidation reaction of the positive material 3 Fe 2 (PO 4 ) 3 (ii) a In addition, the binder in the positive plate is thermally decomposed under the condition of oxygen deficiency or no oxygen, so that the generation of toxic and harmful gases is reduced; after the oxygen-consuming heat treatment is finished, the diaphragm is carbonized to form carbon dust to finish the treatment of solid waste, the binder realizes thermal decomposition, and the residual anode powder in the anode plate and the aluminum foil material can be efficiently, quickly and completely separated only by a mechanical separation mode of vibration, beating or grinding, and the method has the advantages of low cost, greenness and high efficiency.
Preferably, the stacking of the positive electrode sheet and the separator is performed by stacking the positive electrode sheet and the separator according to the layer number ratio of the positive electrode sheet to the separator of (1~5): 1 are alternately stacked. The invention makes the anode plate and the diaphragm have the layer number ratio of (1~5): the alternating stacking of 1 means that after 1~5 layers of positive plates are placed, 1 layer of diaphragm plates are placed at the adjacent positions of the positive plates, and the 1~5 layers of positive plates and 1 layer of diaphragms are stacked alternately, so that the oxygen consumption function of the diaphragm plates can be fully exerted, the periphery of the positive plates can quickly reach the anoxic or anoxic condition, 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; when the positive plate and the diaphragm are stacked, 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; when the positive plate and the diaphragm are stacked, the layer number ratio of the positive plate to the diaphragm is in a range formed by any one of the lower limit and the upper limit.
Further, the stacking of the positive electrode plate and the diaphragm is carried out by stacking the positive electrode plate and the diaphragm according to the layer number ratio of the positive electrode plate to the diaphragm of (2~3): 1 are alternately stacked. According to the invention, by controlling the stacking layer ratio of the positive plate and the diaphragm, the diaphragm is favorable for rapidly and thoroughly consuming oxygen around the positive plate in the oxygen-consuming heat treatment process, so that the positive powder is promoted to keep the mineral phase stable, and the extraction efficiency of the subsequent lithium wet extraction process is improved.
Preferably, after the membrane is collected, the membrane is cut along the folded position to provide a single piece of membrane. The diaphragm can be adapted to the size of the positive plate after being cut along the folding position, and is beneficial to fully contacting the positive plate when being stacked subsequently, so that oxygen around the positive plate is consumed in the heat treatment process.
Preferably, the heating rate of the oxygen-consuming heat treatment is 5 to 10 ℃/min; the treatment time of the oxygen-consuming heat treatment is 10 to 120min.
Further, the lower temperature limit of the oxygen-consuming heat treatment is selected from any 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 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 value of the lower limit and the upper limit.
Further, the lower limit of the treatment time of the oxygen-consuming heat treatment is selected from any one of 10min, 20min, 40min, 60min, 80min and 100min, the upper limit of the treatment time of the oxygen-consuming heat treatment is selected from any one of 20min, 40min, 60min, 80min, 100min and 120min, and the treatment time of the oxygen-consuming heat treatment is a range formed by any one of the lower limit and the upper limit.
Preferably, the treatment temperature of the oxygen-consuming heat treatment is 400 to 500 ℃; the treatment time of the oxygen-consuming heat treatment is 60 to 90min. The temperature is favorable for promoting the oxygen consumption heat treatment, the binder in the positive plate is better decomposed, the separation efficiency of the positive powder and the aluminum foil is improved, and compared with the higher heat treatment temperature, the temperature range has the advantage of saving the cost while ensuring the high-efficiency treatment.
Preferably, the material of the diaphragm is polypropylene and/or polyethylene.
Preferably, the heat treatment equipment for oxygen-consuming heat treatment is in a fixed bed structure and is provided with a pyrolysis gas outlet. The invention carries out oxygen-consuming heat treatment through the diaphragm, releases pyrolysis gas while consuming oxygen, does not need to exhaust air in equipment before the oxygen-consuming heat treatment, can enable the interior of the heat treatment equipment to form an anoxic or anaerobic condition without nitrogen or inert atmosphere protection in the oxygen-consuming heat treatment process, has simple and convenient operation, is beneficial to simplifying the process and saving the cost.
Preferably, the mechanical separation treatment is a rod mill, and the time of the mechanical separation treatment is 1 to 30min.
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 treatment is selected from a range consisting of any one of the lower limit and the upper limit.
Preferably, the method further comprises cooling the positive electrode plate after the heat treatment and before the mechanical separation treatment.
Further, the cooling is natural cooling.
Preferably, in the oxygen consumption heat treatment, the membrane consumes oxygen in air to realize carbonization; the binder in the positive plate is thermally decomposed under an anaerobic condition.
For the sake of brevity, only a few numerical ranges are explicitly disclosed. However, any lower limit may be combined with any upper limit to form ranges not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and similarly any upper limit may be combined with any other upper limit to form a range not explicitly recited. Also, although not explicitly recited, each point or individual value between endpoints of a range is encompassed within the range. Thus, each point or individual value can form a range not explicitly recited as its own lower or upper limit in combination with any other point or individual value or in combination with other lower or upper limits.
Drawings
Fig. 1 is an XRD spectrum of the lithium iron phosphate positive electrode powder obtained in example 1;
fig. 2 is an XRD spectrum 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 (4) phase.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Examples
The technical scheme of the invention is explained by combining specific examples, raw materials used in the following examples are all from common commercial products, and devices or equipment used are all purchased from conventional commercial sales channels.
Example 1
The method for recovering the positive electrode powder of the lithium iron phosphate battery comprises the following steps of:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting a positive plate and a diaphragm; the diaphragm is made of polypropylene, and is cut along the folding position to obtain a single diaphragm;
2) And (2) arranging a positive plate and a single diaphragm according to the layer number ratio of the positive plate to the diaphragm of 2:1 alternately stacking, punching the stacked substance, suspending the punched stacked substance in the center of heat treatment equipment through a hook, and carrying out oxygen-consuming heat treatment in air atmosphere: heating the heat treatment heat backup device provided with the positive plate and the diaphragm to 450 ℃ at the heating rate of 5 ℃/min and preserving heat for 60min, wherein the diaphragm consumes oxygen in air to realize carbonization to form carbon dust, and the binder in the positive plate realizes thermal decomposition under the anaerobic condition;
3) Cooling the anode plate subjected to oxygen consumption heat treatment to room temperature, and mechanically colliding and rubbing the anode plate for 10min by using a rod mill to obtain lithium iron phosphate anode powder and aluminum foil, wherein the falling rate of the lithium iron phosphate anode powder is 99.9%; adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder for leaching, wherein the leaching rate of lithium is 99.2%.
Example 2
The method for recovering the positive electrode powder of the lithium iron phosphate battery comprises the following steps of:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting a positive plate and a diaphragm; the diaphragm is made of polypropylene, and is cut along the folding position to obtain a single diaphragm;
2) And (3) enabling the positive plate and the single diaphragm to be in a layer number ratio of 2:1, alternately stacking, punching the stacked substance, suspending the punched substance in the center of a heat treatment device through a hook, and carrying out oxygen-consuming heat treatment in an air atmosphere: heating the heat treatment heat backup device provided with the positive plate and the diaphragm to 350 ℃ at the heating rate of 5 ℃/min, preserving heat for 60min, enabling the diaphragm to consume oxygen in the air to realize carbonization to form carbon dust, and enabling a binder in the positive plate to realize thermal decomposition under the anaerobic condition;
3) Cooling the anode plate subjected to the oxygen-consuming heat treatment to room temperature, and mechanically colliding and rubbing the anode plate for 10min by using a rod mill to obtain lithium iron phosphate anode powder and aluminum foil, wherein the falling rate of the lithium iron phosphate anode powder is 86.2%; adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder for leaching, wherein the leaching rate of lithium is 87.9%.
Example 3
The method for recovering the positive electrode powder of the lithium iron phosphate battery comprises the following steps of:
1) Discharging and disassembling the waste lithium iron phosphate battery, and collecting a positive plate and a diaphragm; the diaphragm is made of polyethylene, and is cut along the folding position to obtain a single diaphragm;
2) And (3) arranging a positive plate and a single diaphragm according to the layer number ratio of the positive plate to the diaphragm of 5:1, alternately stacking, punching the stacked substance, suspending the punched substance in the center of a heat treatment device through a hook, and carrying out oxygen-consuming heat treatment in an air atmosphere: heating the heat treatment heat preparation with the positive plate and the diaphragm plate to 450 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 60min, wherein the diaphragm consumes oxygen in the air to realize carbonization to form carbon dust, and the binder in the positive plate realizes thermal decomposition under the anaerobic condition;
3) Cooling the anode plate subjected to oxygen consumption heat treatment to room temperature, and mechanically colliding and rubbing the anode plate for 10min by using a rod mill to obtain lithium iron phosphate anode powder and aluminum foil, wherein the falling rate of the lithium iron phosphate anode powder is 99.0%; adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder for leaching, wherein the leaching rate of lithium is 93.5%.
Comparative example 1
The method for recovering the positive electrode powder of the lithium iron phosphate battery of the comparative example is different from the method 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, suspending the positive plate in the center of heat treatment equipment through a hook, and carrying out heat treatment in air atmosphere: heating the heat treatment heat equipment provided with the positive plate and the diaphragm to 450 ℃ at the heating rate of 5 ℃/min and preserving heat for 60min, so that 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 by using a rod mill to obtain lithium iron phosphate positive powder and an aluminum foil, wherein the falling rate of the lithium iron phosphate positive powder is 98.3%; adding sulfuric acid and an auxiliary agent into the obtained lithium iron phosphate anode powder for leaching, wherein the leaching rate of lithium is 68.5%.
Examples of the experiments
XRD tests were performed on the lithium iron phosphate positive electrode powders obtained in example 1 and comparative example 1, and XRD patterns of the two positive electrode powders are shown in fig. 1 and fig. 2, respectively. From 1~2, it can be seen that the recovery method of comparative example 1 partially changed the mineral phase of the lithium iron phosphate battery positive electrode powder after heat treatment to produce Li 3 Fe 2 (PO 4 ) 3 Mineral phase not beneficial to subsequent wet leaching extraction of lithium elementTaking; in the recovery method of the embodiment 1, the iron phosphate lithium battery anode powder is stable in mineral phase in the oxygen-consuming heat treatment process, and selective and efficient extraction of subsequent lithium is facilitated.
The heat treatment parameters and the positive electrode powder recovery data for example 1~3 and comparative example 1 are shown in table 1 below:
TABLE 1 Heat treatment parameters and cathode powder recovery data for example 1~3 and comparative example 1
As can be seen from table 1, the method for recovering the positive electrode powder of the lithium iron phosphate battery in example 1~3 is easy to separate from the aluminum foil after the oxygen-consuming heat treatment, the dropping rate of the positive electrode powder is high and reaches 86.2 to 99.9%, wherein the dropping rates of the positive electrode powder of example 1 and example 3 with the heat treatment temperature of 450 ℃ or higher reach 99.0 to 99.9%, and the method shows excellent separation effect; meanwhile, the mineral phase of the positive electrode powder of the embodiment 1~3 is kept stable after heat treatment, and the lithium leaching rate is extremely high and reaches 87.9 to 99.2 percent; compared with the comparative example 1, the embodiment 1 adopting the same heat treatment parameters has the advantages that the positive plate and the diaphragm are stacked and then subjected to heat treatment, so that the separation of the positive powder and the aluminum foil is facilitated, the mineral phase of the positive powder is stable, the falling rate of the positive powder is improved by 1.6%, the lithium leaching rate is improved by 30.7%, and the recovery efficiency of the positive powder of the lithium iron phosphate battery is greatly improved.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (9)
1. The method for recovering 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 a positive plate and a diaphragm;
2) Stacking the positive plate and the diaphragm, and then carrying out oxygen-consuming heat treatment in an air atmosphere; the processing temperature of the oxygen-consuming heat treatment is 350 to 550 ℃;
3) And mechanically separating the positive plate subjected to the oxygen-consuming heat treatment to obtain the lithium iron phosphate positive powder.
2. The method for recovering the positive electrode powder of the lithium iron phosphate battery as claimed in claim 1, wherein the stacking of the positive electrode sheet and the separator is performed such that the positive electrode sheet and the separator are stacked according to a layer number ratio of the positive electrode sheet to the separator of (1~5): 1 are alternately stacked.
3. The method for recovering the positive electrode powder of the lithium iron phosphate battery as claimed in claim 2, wherein the stacking of the positive electrode sheet and the separator is performed such that the positive electrode sheet and the separator are stacked according to a layer number ratio of the positive electrode sheet to the separator of (2~3): 1 are alternately stacked.
4. The method for recovering the positive powder of the lithium iron phosphate battery as claimed in claim 1, wherein the temperature rise rate of the oxygen-consuming heat treatment is 5 to 10 ℃/min; the treatment time of the oxygen-consuming heat treatment is 10 to 120min.
5. The method for recovering the lithium iron phosphate battery positive electrode powder as claimed in claim 4, wherein the treatment temperature of the oxygen-consuming heat treatment is 400 to 500 ℃; the treatment time of the oxygen-consuming heat treatment is 60 to 90min.
6. The method for recovering the positive electrode powder of the lithium iron phosphate battery as claimed in claim 1, wherein the separator is made of polypropylene and/or polyethylene.
7. The method for recovering the positive electrode powder of the lithium iron phosphate battery as claimed in claim 1, wherein the mechanical separation treatment is a bar mill, and the time of the mechanical separation treatment is 1 to 30min.
8. The method for recovering positive electrode powder for lithium iron phosphate batteries according to claim 1, further comprising cooling the heat-treated positive electrode sheet after the heat treatment and before the mechanical separation treatment.
9. The method for recovering the positive powder of the lithium iron phosphate battery as claimed in claim 1, wherein in the oxygen-consuming heat treatment, the diaphragm consumes oxygen in air to realize carbonization; the binder in the positive plate is thermally decomposed under an anaerobic condition.
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| 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 |
| CN114752769A (en) * | 2022-04-08 | 2022-07-15 | 中国矿业大学 | Method for recovering valuable metals of waste lithium battery materials by aid of pyrolysis of diaphragms |
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Patent Citations (6)
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| CN101383441A (en) * | 2007-09-06 | 2009-03-11 | 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 |
| CN111934042A (en) * | 2020-08-03 | 2020-11-13 | 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 |
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