CN115806292A - Impurity removal method for waste graphite cathode - Google Patents
Impurity removal method for waste graphite cathode Download PDFInfo
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- CN115806292A CN115806292A CN202211508541.6A CN202211508541A CN115806292A CN 115806292 A CN115806292 A CN 115806292A CN 202211508541 A CN202211508541 A CN 202211508541A CN 115806292 A CN115806292 A CN 115806292A
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Abstract
The invention relates to a method for removing impurities from a waste graphite cathode, which comprises the steps of calcining waste graphite residues at a high temperature to oxidize metal simple substances in the graphite residues; acid leaching the graphite residue after high-temperature calcination in a hydrothermal reaction mode; cooling and crystallizing the reaction liquid; filtering the metal salt crystal in the reaction liquid to obtain graphite reaction liquid; filtering and washing the graphite reaction solution to obtain a graphite filter cake; and drying the graphite filter cake to obtain the graphite with low metal impurity content. The beneficial effects are that: through high-temperature calcination, metal simple substances in the graphite slag are oxidized to be reacted with acid subsequently, the calcined graphite slag is subjected to acid leaching in a hydrothermal reaction mode, the reaction activity of metal oxidation and acid is increased, the contact probability of an acid solution and metal oxide particles in the graphite slag is increased, more metal ions enter a solution in the form of metal ions and reach a saturated state, and then the metal ions are crystallized and separated out at a low temperature, so that the probability that the metal ions are adsorbed or wrapped between graphite layers in the solution is greatly reduced, and the metal content of the graphite slag is effectively reduced.
Description
Technical Field
The invention relates to the field of graphite cathode recovery, in particular to a waste graphite cathode impurity removal method.
Background
The lithium battery has the advantages of high energy density, large capacity, good cycle performance and the like, and is widely applied to the field of electric automobiles. Under the background of the vigorous development of new energy automobiles in China, the loading capacity and the retirement capacity of lithium batteries of lithium ion power battery automobiles are greatly increased in recent years, waste lithium batteries contain various metal elements such as Li, ni, co, mn and the like, metal resources are in short supply in China, and the utilization rate of the resources can be improved and the cost can be reduced by recycling the metal in the waste lithium batteries.
The lithium ion battery pack is complex, the electrode materials are various, and the complete recovery of the waste lithium ion battery comprises the following two steps: physical and chemical methods. The waste lithium ion battery still has residual energy, the waste lithium ion battery needs to be discharged before being physically crushed, and then the methods of disassembly, crushing, screening, chemical washing, heat treatment and the like are carried out, so that metal elements in the waste lithium ion battery are recycled, a large amount of residual waste graphite negative electrodes are not valued by people for a long time, and the graphite slag contains more metal ion impurities, so that the recycling difficulty is high. The waste graphite cathode is difficult to recycle due to the action of inorganic acid and hydrogen peroxide, the graphite is of a layered two-dimensional structure, and the waste graphite cathode is frequently separated and embedded from electrolyte and lithium ions to destroy the surface structure of the graphite, so that the specific surface area of the graphite is increased, and the graphite is easier to adsorb metal ions and coat metal oxides or metal salts.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for removing impurities from a waste graphite cathode so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a method for removing impurities from a waste graphite cathode comprises the following steps:
s100, calcining the waste graphite residues at high temperature to oxidize metal simple substances in the graphite residues;
s200, acid leaching the graphite residue after high-temperature calcination in a hydrothermal reaction mode;
s300, cooling and crystallizing the reaction liquid;
s400, filtering metal salt crystals in the reaction liquid to obtain graphite reaction liquid;
s500, filtering and washing the graphite reaction liquid to obtain a graphite filter cake;
s600, drying the graphite filter cake to obtain graphite with low metal impurity content.
On the basis of the technical scheme, the invention can be improved as follows.
Further, the waste graphite negative electrode slag is: the graphite powder separated by a physical method, the graphite of the cathode of the battery which is not made, the graphite of the cathode of the battery which is not circulated, the graphite slag after the metal element is recovered from the ternary black powder mixed with the graphite, the graphite slag after the metal element is recovered from the lithium iron phosphate and graphite mixed black powder, and the graphite slag after the metal element is recovered from the ternary black powder mixed with the lithium iron phosphate are mixed.
Further, the total amount of metal impurities in the waste graphite residues is 10-30%.
Further, the high-temperature calcination temperature is 400-500 ℃, the heating rate is 10-20 ℃/min, and the calcination time is 1-2 h.
Further, the ratio of the graphite residue to the acid solution in the acid leaching is 1:2 to 1:5.
Further, the acid adopted in the acid leaching is one or more mixed acid of sulfuric acid, hydrochloric acid, nitric acid, citric acid and malic acid, and the concentration of the acid solution is 20-30%.
Further, S200 specifically is: adding the graphite residue after high-temperature calcination into an acid solution, transferring the graphite residue into a pot of a hydrothermal reaction kettle, sealing the pot, and then placing the pot in an environment of 100-160 ℃.
Further, the hydrothermal reaction kettle is transferred into an oven, and the temperature of the oven is 100-160 ℃.
Further, the temperature of cooling crystallization is 5-10 ℃, and the time is 2-4 h.
Further, the cooling crystallization was carried out in an explosion-proof refrigerator.
In S400, the metal salt crystals in the reaction solution are filtered by using a screen with a mesh size of 100-1000 meshes.
Further, in S500, sand core filtration is adopted for filtration, and ionized water is adopted for washing the pH value of the graphite filter cake obtained by filtration to 6-7.
Further, the drying temperature is 100-110 ℃, and the drying time is 8-12 h.
The invention has the beneficial effects that:
1) The method has the advantages that metal elements in the waste graphite slag are removed through high-temperature calcination and hydrothermal reaction, compared with acid washing under common conditions, the reaction temperature can be higher, the reaction pressure can be controlled, and the contact probability of acid liquor and metal oxides or simple substances in graphite is increased under the conditions of higher temperature and high pressure, so that the reaction efficiency is greatly increased, and the acid washing efficiency is increased;
2) Compared with the method that deionized water is directly adopted to wash the pickle liquor, especially in waste graphite slag with high metal impurity content and complex metal impurities, excessive metal ions are prevented from being adsorbed on the surface or between layers of graphite and are not beneficial to washing of the deionized water, and low-temperature cooling crystallization is adopted, so that the method is beneficial to forming metal salt after acid leaching to form large crystallized particles and is convenient to filter; the content of metal ions in the filtered solution is greatly reduced, the washing times of deionized water and the water consumption are reduced, and the impurity content in graphite is low, so that a crystallized product is formed, and a raw material can be synthesized by preparing a positive electrode material;
3) The metal content of the graphite residue is reduced to below 4.9 percent.
Drawings
FIG. 1 is a flow chart of the impurity removal method for the waste graphite cathode.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing the graphite slag obtained after recovering the metal elements from the ternary and graphite mixed black powder into a corundum crucible, placing the corundum crucible into a tubular furnace, heating to 450 ℃ at the heating rate of 15 ℃/min, preserving heat for 1h, and calcining the metal simple substance in the graphite slag at high temperature so as to facilitate subsequent reaction with acid;
weighing 30g of the calcined graphite slag, placing the weighed graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 24.3g of concentrated sulfuric acid and 65.7g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a hydrothermal reaction kettle, placing the reaction kettle into an oven with the temperature of 100 ℃ for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, setting the temperature at 5 ℃ and setting the time at 2h, so as to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 300-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma) to obtain the total content of metal ions of 4.5%.
Example 2
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing the graphite slag obtained after recovering the metal elements from the ternary and lithium iron phosphate mixed black powder into a corundum crucible, placing the corundum crucible into a tubular furnace, heating to 500 ℃ at a heating rate of 15 ℃/min, preserving the temperature for 1h, and calcining the metal simple substance in the graphite slag at a high temperature so as to facilitate subsequent reaction with acid;
weighing 40g of the calcined graphite slag, placing the calcined graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 32.4g of concentrated sulfuric acid and 87.6g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a reaction kettle, placing the reaction kettle into an oven with the temperature of 120 ℃ for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, and setting the temperature at 5 ℃ and the time at 2h to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 200-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma) to obtain the total content of metal ions of 4.0%.
Example 3
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing the graphite slag obtained after recovering metal elements from the ternary and graphite mixed black powder into a corundum crucible, placing the corundum crucible into a tubular furnace, heating to 400 ℃ at the heating rate of 12 ℃/min, preserving heat for 1h, and calcining and oxidizing metal simple substances in the graphite slag at high temperature so as to facilitate subsequent reaction with acid;
weighing 30g of the calcined graphite slag, placing the weighed graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 24.3g of concentrated sulfuric acid and 65.7g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a reaction kettle, placing the reaction kettle into an oven at the temperature of 130 ℃ for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, setting the temperature at 10 ℃ and setting the time for 2 hours, so as to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 300-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma) to obtain the total content of metal ions of 4.9%.
Example 4
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing graphite slag obtained after recovering metal elements from mixed black powder of lithium iron phosphate and graphite in a corundum crucible, placing the corundum crucible in a tubular furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, preserving heat for 1h, and oxidizing metal simple substances in the graphite slag through high-temperature calcination so as to facilitate subsequent reaction with acid;
weighing 40g of the calcined graphite slag, placing the calcined graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 32.4g of concentrated sulfuric acid and 87.6g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a reaction kettle, placing the reaction kettle into an oven at the temperature of 150 ℃ for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, and setting the temperature at 5 ℃ and the time at 2h to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 200-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma) to obtain the total content of metal ions of 4.9%.
Example 5
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing the graphite slag obtained after recovering the metal elements from the ternary and graphite mixed black powder in a corundum crucible, placing the corundum crucible in a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 1h, and calcining the metal simple substance in the graphite slag at high temperature so as to facilitate the subsequent reaction with acid;
weighing 40g of the calcined graphite slag, placing the calcined graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 32.4g of concentrated sulfuric acid and 87.6g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a reaction kettle, placing the reaction kettle into a 160 ℃ oven for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, setting the temperature at 8 ℃ and setting the time for 2 hours, so as to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 200-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma) to obtain the total content of metal ions of 3.5%.
Example 6
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing the graphite slag obtained after recovering the metal elements from the ternary and graphite mixed black powder into a corundum crucible, placing the corundum crucible into a tubular furnace, heating to 500 ℃ at a heating rate of 15 ℃/min, preserving heat for 1h, and calcining the metal simple substance in the graphite slag at a high temperature so as to facilitate subsequent reaction with acid;
weighing 40g of the calcined graphite slag, placing the calcined graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 32.4g of concentrated sulfuric acid and 87.6g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a reaction kettle, then placing the reaction kettle into an oven with the temperature of 120 ℃ for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, setting the temperature at 5 ℃ and setting the time at 2h, so as to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 200-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma) to obtain the total content of metal ions of 4.0%.
Example 7
As shown in fig. 1, a method for removing impurities from a waste graphite negative electrode comprises the following steps:
placing graphite powder separated by a physical method into a corundum crucible, placing the corundum crucible into a tubular furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 1h, and calcining a metal simple substance in the graphite oxide slag at high temperature so as to facilitate subsequent reaction with acid;
weighing 40g of the calcined graphite slag, placing the calcined graphite slag into a 500ml polytetrafluoroethylene lining tank, then weighing 32.4g of concentrated sulfuric acid and 87.6g of deionized water respectively, slowly adding the concentrated sulfuric acid into the deionized water to prepare dilute sulfuric acid with the concentration of 27%, pouring the dilute sulfuric acid into the lining tank filled with the graphite slag, screwing a steel cover of a reaction kettle, placing the reaction kettle into an oven at the temperature of 150 ℃ for 8 hours, taking out the reaction kettle from the oven, placing the reaction kettle into cold water, and cooling the temperature of the reaction kettle to room temperature;
pouring the reaction liquid into a beaker, placing the beaker on the upper layer of an explosion-proof refrigerator, setting the temperature at 8 ℃ and setting the time for 2 hours, so as to generate metal salt crystals in the reaction liquid;
taking out the metal salt crystal formed in the reaction solution by filtering with a 200-mesh nylon screen;
filtering the graphite reaction solution obtained by filtering by adopting a sand core, and washing with water until the pH value is 7 to obtain a graphite filter cake;
and (3) putting the graphite filter cake into a 100 ℃ oven for drying for 12h, and detecting by ICP (inductively coupled plasma), wherein the total content of metal ions is 2.5%.
In addition, the calcined graphite residue is subjected to acid leaching in a hydrothermal reaction mode, so that the activity of metal oxidation and acid reaction and the contact probability of an acid solution and metal oxide particles in the graphite residue are increased, more metal ions enter the solution in the form of metal ions and reach a saturated state, and then the metal ions are crystallized and separated out in a low-temperature state, so that the probability of the metal ions absorbing or wrapping graphite layers in the solution is greatly reduced, and the metal content of the graphite residue is effectively reduced.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for removing impurities from a waste graphite cathode is characterized by comprising the following steps:
s100, calcining the waste graphite residues at high temperature to oxidize metal simple substances in the graphite residues;
s200, acid leaching the graphite residue after high-temperature calcination in a hydrothermal reaction mode;
s300, cooling and crystallizing the reaction liquid;
s400, filtering metal salt crystals in the reaction liquid to obtain graphite reaction liquid;
s500, filtering and washing the graphite reaction liquid to obtain a graphite filter cake;
s600, drying the graphite filter cake to obtain graphite with low metal impurity content.
2. The impurity removing method for the waste graphite negative electrode according to claim 1, characterized by comprising the following steps: the waste graphite negative electrode slag comprises the following components: the graphite powder separated by a physical method, the graphite of the cathode of the battery which is not made, the graphite of the cathode of the battery which is not circulated, the graphite slag after the metal element is recovered from the ternary black powder mixed with the graphite, the graphite slag after the metal element is recovered from the lithium iron phosphate and graphite mixed black powder, and the graphite slag after the metal element is recovered from the ternary black powder mixed with the lithium iron phosphate are mixed.
3. The impurity removing method for the waste graphite negative electrode according to claim 1 or 2, characterized by comprising the following steps: the total amount of metal impurities in the waste graphite residues is 10-30%.
4. The impurity removing method for the waste graphite negative electrode as claimed in claim 1, 2 or 3, wherein the impurity removing method comprises the following steps: the high-temperature calcination temperature is 400-500 ℃, the heating rate is 10-20 ℃/min, and the calcination time is 1-2 h.
5. The impurity removing method for the waste graphite negative electrode according to claim 1, characterized by comprising the following steps: the ratio of the graphite residue to the acid solution in the acid leaching is 1:2-1:5.
6. The impurity removing method for the waste graphite negative electrode as claimed in claim 1, which is characterized in that: the acid adopted by the acid leaching is one or more mixed acid of sulfuric acid, hydrochloric acid, nitric acid, citric acid and malic acid, and the concentration of the acid solution is 20-30%.
7. The impurity removing method for the waste graphite negative electrode according to claim 1, characterized by comprising the following steps: the S200 specifically comprises the following steps: adding the graphite residue after high-temperature calcination into an acid solution, transferring the graphite residue into a pot of a hydrothermal reaction kettle, sealing the pot, and then placing the pot in an environment of 100-160 ℃.
8. The impurity removing method for the waste graphite negative electrode according to claim 1, characterized by comprising the following steps: the temperature of the cooling crystallization is 5-10 ℃, and the time is 2-4 h.
9. The impurity removing method for the waste graphite negative electrode according to claim 1, characterized by comprising the following steps: in the step S400, the metal salt crystals in the reaction solution are filtered by a screen with the mesh number of 100-1000 meshes.
10. The impurity removing method for the waste graphite negative electrode as claimed in claim 1, which is characterized in that: the drying temperature is 100-110 ℃, and the drying time is 8-12 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116404293A (en) * | 2023-06-08 | 2023-07-07 | 山东产研绿洲环境产业技术研究院有限公司 | Waste lithium battery graphite negative electrode recycling method based on oil sludge microwave pyrolysis cladding |
| CN116639685A (en) * | 2023-06-19 | 2023-08-25 | 深圳光风新能源科技创新中心有限公司 | Recycling method of waste lithium-carbide graphite cathode |
-
2022
- 2022-11-28 CN CN202211508541.6A patent/CN115806292A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116404293A (en) * | 2023-06-08 | 2023-07-07 | 山东产研绿洲环境产业技术研究院有限公司 | Waste lithium battery graphite negative electrode recycling method based on oil sludge microwave pyrolysis cladding |
| CN116404293B (en) * | 2023-06-08 | 2023-08-29 | 山东产研绿洲环境产业技术研究院有限公司 | Waste lithium battery graphite negative electrode recycling method based on oil sludge microwave pyrolysis cladding |
| CN116639685A (en) * | 2023-06-19 | 2023-08-25 | 深圳光风新能源科技创新中心有限公司 | Recycling method of waste lithium-carbide graphite cathode |
| CN116639685B (en) * | 2023-06-19 | 2023-12-22 | 深圳光风新能源科技创新中心有限公司 | Recycling method of waste lithium-carbide graphite cathode |
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