CN112938949A - Method for preparing graphene by using waste negative electrode graphite of lithium battery and graphene - Google Patents
Method for preparing graphene by using waste negative electrode graphite of lithium battery and graphene Download PDFInfo
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Abstract
The invention belongs to the technical field of recycling waste lithium battery materials, and discloses a method for preparing graphene by using waste negative graphite of a lithium battery and the graphene, wherein the method comprises the following steps: (1) clamping graphite powder recovered from waste batteries in a conductive net, and connecting to an anode of a direct-current power supply; (2) heating the electrolyte in the electrolytic bath to be molten, preserving heat, immersing the anode and the cathode of the direct current power supply into the electrolyte, standing, and turning on the direct current power supply for electrolysis to obtain electrolytic graphite; (3) and taking out the electrolytic graphite, washing, ultrasonically dispersing, centrifuging and drying to obtain the graphene. According to the invention, the waste cathode graphite powder is clamped in the conductive wire mesh in a limited mode, and the cathode graphite can be fixed by the mode, so that the step of preparing the waste cathode graphite powder into a graphite block and then carrying out subsequent electrolysis is omitted, and the process is simplified.
Description
Technical Field
The invention belongs to the technical field of recycling waste lithium battery materials, and particularly relates to a method for preparing graphene by using waste negative graphite of a lithium battery and the graphene.
Background
Lithium ion batteries have been on the market for nearly 30 years, and develop from portable electronic equipment to power devices, and products of the lithium ion batteries affect aspects of production and life of people. While lithium ion batteries are rapidly developing, the problem of battery decommissioning is paid much attention to by battery and equipment manufacturers. Because the value of the lithium ion battery cathode material is low, the recycling and reusing aspects of the lithium ion battery cathode material are not focused. Therefore, the waste negative electrode graphite is added with high value, and the key for realizing the win-win purpose of resource regeneration and economic benefit is realized. Graphene, as a novel nanocarbon material, has a great market application value due to its excellent characteristics such as light, electricity, and heat. But the cost and the quality of the product become key factors for limiting the further development of the product. Therefore, from waste negative electrode graphite to graphene, the problems of waste negative electrode recycling and graphene low-cost preparation can be solved simultaneously. For the related technology, a method for recycling waste lithium ion battery cathode materials is disclosed. The method comprises the step of immersing a graphite material of a negative electrode of a waste lithium ion battery in a solution containing a certain concentration of H+The aqueous solution of (A) is washed by shaking up and down or by refluxing and circulating. And (3) expanding graphite interlayers while recovering lithium resources, and preparing the graphene material by using a liquid-phase mechanical stripping method. The method can simultaneously recover the graphite cathode and the lithium source, but has the disadvantages of complex process, long time consumption and low rate of return. The related technology also discloses a method for recycling and regenerating graphene from the waste lithium ion battery. The method comprises the steps of pre-charging or pre-discharging the waste lithium ion battery, and coating the cathode and the anodeSeparating from the current collector and the outer package to obtain a cathode and anode blending material; after crushing and grading, the intercalated fossil toner is used as a raw material, and graphene is prepared by adopting an oxidation-reduction method or an ultrasonic stripping method. According to the method, the graphene is prepared by stripping by using a redox method, the raw materials required to be input and the equipment cost are high, and the intrinsic structure of the graphite is seriously damaged in the redox process.
Therefore, it is urgently needed to develop a method for preparing graphene by combining the existing disassembly process of the waste lithium ion battery and developing according to the characteristics of the recycled waste negative graphite.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the method for preparing the graphene by using the waste negative graphite of the lithium battery and the graphene realize the conversion of the waste negative graphite from waste materials to black gold in the lithium battery, the recovery rate of the waste negative graphite of the lithium battery is more than 80%, and the conversion rate of the waste negative graphite to the graphene is more than 99%.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing graphene by using waste negative electrode graphite of a lithium battery comprises the following steps:
(1) clamping graphite powder recovered from waste batteries in a conductive wire mesh, and connecting an anode of a direct-current power supply;
(2) heating the electrolyte in the electrolytic bath to be molten, preserving heat, immersing the anode and the cathode of the direct current power supply into the electrolyte, standing, and turning on the direct current power supply for electrolysis to obtain electrolytic graphite;
(3) taking out the electrolytic graphite, washing, ultrasonically dispersing, centrifuging and drying to obtain the graphene; in the step (2), the electrolyte is sulfuric acid type ammonium salt.
Preferably, the step (3) further comprises the step of simultaneously re-clamping the electrolytic slag obtained by centrifugal classification in the conductive wire mesh, and carrying out electrolysis again, wherein the conductive wire mesh can be reused in the circulation process.
After the negative electrode graphite in the lithium ion battery is subjected to endless cyclic charge and discharge, the graphite interlayer spacing is gradually enlarged, and the intercalation compound is favorably fed into the graphite interlayer. In addition, metal impurities (aluminum, copper and the like) and metal compounds (nickel, cobalt, manganese and the like) remained in the cathode graphite in the disassembly process can improve the conductivity of the waste cathode graphite. According to the characteristics of the waste negative electrode graphite, the method for preparing the graphene through the limited-area molten salt electrolysis is developed, after electrolysis, metal impurities in the waste negative electrode graphite are enriched at the cathode, and the graphene subjected to anode electrolysis is purified.
Preferably, in step (1), the conductive wire mesh is one of a molybdenum wire mesh, a titanium wire mesh, an alloy wire mesh or a polypyrrole wire mesh.
More preferably, the mesh number of the conductive wire mesh is equal to that of the graphite powder.
Preferably, in step (2), the cathode is an inert electrode, and the material of the inert electrode is one of platinum, gold, titanium alloy or tungsten.
Preferably, in the step (2), the sulfuric acid type ammonium salt is at least one of ammonium sulfate, ammonium bisulfate and ammonium sulfite.
The anions in the electrolyte move to the anode to release electrons, and oxidation occurs, and the process is the key of intercalation stripping of the anode graphite. The reason for using ammonium sulfate salts is that such electrolytes can ionize sulfate ions. SO (SO)4 2-Has a size (0.46nm) similar to the graphite interlayer spacing (0.335nm), and at the melting temperature, Van der Waals force between graphite layers is weakened, interlayer spacing is enlarged, and SO4 2-More easily inserted into graphite layers than other anions, and SO4 2-Decomposing escaped SO2The gas plays an important role in graphite expansion and exfoliation.
Preferably, in the step (2), the heating to melting temperature is 100-500 ℃, and the holding time is 5-120 min.
Preferably, in the step (2), the standing time is 20-40 min.
Preferably, in the step (2), during the electrolysis, the current is 1-150A, and the voltage is 1-300V; the electrolysis time is 5-120 min.
Preferably, in the step (3), the washing is performed by using deionized water until the pH is neutral.
Preferably, in the step (3), the power of the ultrasonic dispersion is 600-1200W, and the time of the ultrasonic dispersion is 20-40 min.
Preferably, in step (3), the rotation speed of the centrifugation is 1800 and 2500rmp, and the time of the centrifugation is 1-5 min.
The graphene is prepared by the method, and the specific surface area of the graphene is 200-600m2·g-1The number of the layers is 3-10.
The principle of the invention is as follows:
the invention takes waste graphite as an anode, so an anodic oxidation stripping method is adopted, and the basic principle is as follows: external voltage is applied to drive anions in the electrolyte to be effectively embedded into the graphite anode layer to form a Graphite Intercalation Compound (GIC), and the expansion force of gas generated by oxidation or reduction reaction of the GIC preferentially opens the grain boundary, edge and other defect positions with weak van der Waals force among the graphite layers, so that the microstructure of the graphite layers expands in a large proportion and effectively peels off, and finally, the preparation of graphene is realized. Most of the recovered negative graphite is powder, no conductive bridge exists among particles, graphite is needed to be used as a conductor in the electrolysis process and is similar to a conductive rod/block, the most simple method is to fix the negative graphite powder by using a conductive wire mesh, and the conductive wire mesh and the graphite form a conductive path in the electrolysis process to form a complete anode. Since the material of the conductive mesh is related to the activity of the metal, the active metal serving as the conductive mesh will be ionized into the electrolyte and cannot fix the graphite, and therefore, the anode is required to be an inert metal which is difficult to ionize and has conductivity for the selection of the anode electrode material.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the waste cathode graphite powder is clamped in the conductive wire mesh in a limited mode, and the cathode graphite can be fixed by the mode, so that the step of preparing the waste cathode graphite powder into a graphite block and then carrying out subsequent electrolysis is omitted, and the process is simplified.
2. Hair brushThe molten salt is used as electrolyte to continuously electrolyze the waste cathode graphite, and the metal impurities in the waste cathode graphite are beneficial to improving the conductivity of the waste cathode graphite. The graphite interlayer spacing is enlarged at the melting temperature, so that anions can enter the graphite interlayer spacing to perform intercalation and stripping on graphite in the electrolysis process, the recovery rate of the waste lithium ion battery negative electrode graphite is more than 80%, and the conversion rate from the waste negative electrode graphite to graphene is more than 99%. The specific surface area of the obtained graphene is 200-600m2·g-1The number of the layers is 3-10.
3. The negative electrode graphite in the waste lithium ion battery material is subjected to high-value-assigned recycling, so that the pollution problem of electronic waste can be solved, the waste negative electrode graphite can be extracted to serve as a raw material to prepare graphene, and the resource utilization of the waste lithium ion battery negative electrode material is realized.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a process flow diagram of example 1 of the present invention;
fig. 2 is a structural view of an apparatus for molten salt electrolysis of waste negative electrode graphite according to embodiment 1 of the present invention.
In fig. 2: 1 is a cathode, 2 is an electrolytic bath, 3 is a molten electrolyte, 4 is waste cathode graphite powder, 5 is a conductive wire mesh, and 6 is a direct current power supply.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
The method for preparing graphene by using waste negative graphite of a lithium battery comprises the following steps:
(1) 5g of waste lithium ion is takenThe graphite of the negative electrode of the pool is filtered by a 400-mesh screen, and the graphite powder or block on the screen is clamped in a 400-mesh screen with the area of 20cm2In a double-layer stainless steel conductive wire mesh (brand: 316L), and the area of the anode is 20cm2The pot piece is used as a cathode;
(2) turning on a heater, setting the temperature at 150 deg.C, heating ammonium bisulfate in the electrolytic bath to melt, maintaining constant temperature, soaking the prepared cathode and anode in molten electrolyte after ammonium bisulfate is completely melted, standing for 0.5 hr to completely infiltrate graphite powder with the electrolyte, connecting the cathode and anode with DC power supply, and controlling the current density at 3 A.dm-2After continuous electrolysis for 2h, turning off the power supply to obtain electrolytic graphite, wherein the electrolysis device is shown as a figure II;
(3) taking out the electrolytic graphite, washing the electrolytic graphite with water to make the pH value of the product neutral to obtain a suspension, carrying out 1000W ultrasonic treatment for 30min, centrifuging for 2min at 2000rmp, extracting the upper layer liquid to obtain a graphene dispersion liquid, and freeze-drying for 24h to obtain graphene, (after carrying out vacuum drying on the lower layer at 80 ℃ for 3h, returning to the first step to be used as an electrolytic raw material for continuous electrolysis).
The graphene of the present example has a specific surface area of 420m measured by physical adsorption2·g-1The number of the layers is 5-8, the recovery rate of the waste lithium ion battery cathode graphite is 80% (the recovery rate refers to the extraction rate from the cathode to the cathode graphite in the battery), and the conversion rate from the waste cathode graphite to the graphene is more than 99%.
Example 2
The method for preparing graphene by using waste negative graphite of a lithium battery comprises the following steps:
(1) taking 5g of waste lithium ion battery negative electrode graphite, sieving with a 400-mesh sieve, and clamping the sieved graphite powder or block in a 400-mesh sieve with an area of 20cm2In a double-layer stainless steel conductive wire mesh (brand: 316L), and the area of the anode is 20cm2The pot piece is used as a cathode;
(2) turning on a heater, setting the temperature at 250 deg.C, heating ammonium sulfate in the electrolytic bath to melt, maintaining constant temperature, and melting ammonium bisulfate completely, and mixing the above prepared cathode and anodeSoaking in molten electrolyte, standing for 0.5 hr to completely soak graphite powder with the electrolyte, connecting the cathode and anode to DC power supply with current density of 3 A.dm-2After continuous electrolysis for 2h, turning off the power supply to obtain electrolytic graphite;
(3) taking out the electrolytic graphite, washing the electrolytic graphite with water to make the pH value of the product neutral to obtain a suspension, carrying out 600W ultrasonic treatment for 30min, centrifuging for 2min at 2000rmp, extracting the upper layer liquid to obtain a graphene dispersion, and carrying out freeze drying for 24h to obtain graphene (the lower layer is subjected to vacuum drying at 80 ℃ for 3h, and then returning to the first step to be used as an electrolytic raw material for continuous electrolysis).
The graphene of the embodiment has a specific surface area of 350m measured by a physical adsorption method2·g-1The number of the layers is 5-10, the recovery rate of the waste lithium ion battery cathode graphite is 80%, and the conversion rate from the waste cathode graphite to graphene is more than 99%. .
Example 3
The method for preparing graphene by using waste negative graphite of a lithium battery comprises the following steps:
(1) taking 5g of waste lithium ion battery negative electrode graphite, sieving with a 500-mesh sieve, and clamping the sieved graphite powder or block in a 500-mesh sieve with an area of 20cm2In a double-layer stainless steel conductive wire mesh (brand: 316L), and the area of the anode is 20cm2The pot piece is used as a cathode;
(2) turning on a heater, setting the temperature at 150 deg.C, heating ammonium bisulfate in the electrolytic bath to melt, maintaining constant temperature, soaking the prepared cathode and anode in molten electrolyte after ammonium bisulfate is completely melted, standing for 0.5 hr to completely infiltrate graphite powder with the electrolyte, connecting the cathode and anode with DC power supply, and controlling the current density at 6 A.dm-2After continuous electrolysis for 1h, turning off the power supply to obtain electrolytic graphite;
(3) taking out the electrolytic graphite, washing the electrolytic graphite with water to make the pH value of the product neutral to obtain a suspension, carrying out 1000W ultrasonic treatment for 30min, centrifuging for 2min at 2000rmp, extracting the upper layer liquid to obtain a graphene dispersion liquid, and carrying out spray drying to obtain graphene (the lower layer is subjected to vacuum drying at 80 ℃ for 3h, and then returning to the first step to be used as an electrolytic raw material for continuous electrolysis).
The graphene of the present example has a specific surface area of 382m measured by physical adsorption2·g-1The number of the layers is 5-10, the recovery rate of the waste lithium ion battery cathode graphite is 80%, and the conversion rate from the waste cathode graphite to graphene is more than 99%.
Comparative example 1
The method for preparing graphene by using waste negative graphite of the lithium battery in the comparative example comprises the following steps:
(1) taking 5g of waste lithium ion battery negative electrode graphite, sieving with a 400-mesh sieve, and clamping the sieved graphite powder or block in a 400-mesh sieve with an area of 20cm2In a double-layer stainless steel conductive wire mesh (brand: 316L), and the area of the anode is 20cm2The pot piece is used as a cathode;
(2) turning on a heater, setting the temperature at 110 deg.C, heating ammonium bicarbonate in the electrolytic bath to melt, maintaining constant temperature, soaking the prepared cathode and anode electrodes in molten electrolyte after the ammonium bicarbonate is completely melted, standing for 0.5 hr to make graphite powder completely soaked by the electrolyte, connecting the cathode and anode into a DC power supply, and controlling the current density at 3 A.dm-2Continuously electrolyzing for 2h to obtain electrolytic graphite, and turning off a power supply;
(3) taking out the electrolytic graphite, washing the electrolytic graphite with water to make the pH value of the product neutral to obtain a suspension, carrying out 1000W ultrasonic treatment for 30min, centrifuging for 2min at 2000rmp, extracting the upper layer solution to obtain a graphene dispersion solution, and carrying out freeze drying for 24h to obtain graphene (the lower layer is subjected to vacuum drying at 80 ℃ for 3h, and then returning to the first step to be used as an electrolytic raw material for continuous electrolysis).
The graphene of the comparative example has a specific surface area of 60m measured by a physical adsorption method2·g-1And the number of layers is more than 10, the recovery rate of the waste lithium ion battery cathode graphite is 80%, and the conversion rate from the waste cathode graphite to graphene is less than 60%. Since ammonium bicarbonate has a melting point of 105 ℃ and is easily decomposed into water and carbon dioxide by heating, the effect of using ammonium bicarbonate as an electrolyte is inferior to that of ammonium bisulfate.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A method for preparing graphene by using waste negative electrode graphite of a lithium battery is characterized by comprising the following steps:
(1) clamping graphite powder recovered from waste batteries in a conductive wire mesh, and connecting an anode of a direct-current power supply;
(2) heating the electrolyte in the electrolytic bath to be molten, preserving heat, immersing the anode and the cathode of the direct current power supply into the electrolyte, standing, and turning on the direct current power supply for electrolysis to obtain electrolytic graphite;
(3) taking out the electrolytic graphite, washing, ultrasonically dispersing, centrifuging and drying to obtain the graphene; in the step (2), the electrolyte is sulfuric acid type ammonium salt.
2. The method of claim 1, wherein in step (1), the electrically conductive wire mesh is one of a molybdenum wire mesh, a titanium wire mesh, an alloy wire mesh, or a polypyrrole wire mesh.
3. The method according to claim 1, wherein in the step (2), the cathode is an inert electrode, and the material of the inert electrode is one of platinum, gold, titanium alloy or tungsten.
4. The method according to claim 1, wherein the ammonium sulfate-type salt is at least one of ammonium bisulfate, ammonium sulfate or ammonium sulfite.
5. The method according to claim 1, wherein in the step (2), the heating to the melting temperature is 100-500 ℃, and the holding time is 5-120 min.
6. The method according to claim 1, wherein in the step (2), during the electrolysis, the current is 1-150A, and the voltage is 1-300V; the electrolysis time is 5-120 min.
7. The method according to claim 1, wherein in the step (2), the standing time is 20-40 min.
8. The method as claimed in claim 1, wherein in step (3), the power of the ultrasonic dispersion is 600-1200W, and the time of the ultrasonic dispersion is 20-40 min.
9. The method as claimed in claim 1, wherein in step (3), the rotation speed of the centrifugation is 1800-2500rmp, and the time of the centrifugation is 1-10 min.
10. Graphene prepared by the method of any one of claims 1 to 9, wherein the specific surface area of the graphene is 200-600m2·g-1The number of the layers is 3-10.
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| CN113881851A (en) * | 2021-09-28 | 2022-01-04 | 华东理工大学 | Method for simultaneously recovering anode and cathode of lithium ion battery by adopting multilayer electrode structure |
| CN113881850A (en) * | 2021-09-28 | 2022-01-04 | 华东理工大学 | Method for simultaneously recovering anode and cathode of lithium ion battery |
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| CN104291327A (en) * | 2014-09-24 | 2015-01-21 | 北京化工大学常州先进材料研究院 | Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt |
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| CN102868006A (en) * | 2012-09-21 | 2013-01-09 | 华东理工大学 | Method for preparing graphene through waste lithium batteries |
| CN104291327A (en) * | 2014-09-24 | 2015-01-21 | 北京化工大学常州先进材料研究院 | Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt |
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| CN113881850A (en) * | 2021-09-28 | 2022-01-04 | 华东理工大学 | Method for simultaneously recovering anode and cathode of lithium ion battery |
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