CN111416170A - Method for recycling waste lithium ion battery negative electrode and co-producing conductive agent - Google Patents
Method for recycling waste lithium ion battery negative electrode and co-producing conductive agent Download PDFInfo
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- CN111416170A CN111416170A CN202010166439.7A CN202010166439A CN111416170A CN 111416170 A CN111416170 A CN 111416170A CN 202010166439 A CN202010166439 A CN 202010166439A CN 111416170 A CN111416170 A CN 111416170A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a conductive agent prepared from a waste lithium ion battery cathode and a preparation method thereof. The D50 particle size range of the conductive agent is 5nm-3.5um, and the specific surface area is 300-1000m2Per g, conductivity 1 × 104‑1×105S/m; the preparation method comprises the steps of removing the water-soluble organic binder in the waste negative electrode, separating the carbonaceous material in the waste negative electrode, deeply removing and modifying the impurity elements in the carbonaceous material, reducing and the like. The invention not only realizes the conversion of the carbonaceous component in the anode material of the waste lithium ion battery into the conductive agent and the conductive agent with high added value, but also has the advantages of short flow, low cost, suitability for large-scale production and the like.
Description
Technical Field
The invention belongs to the field of waste battery recovery, and particularly relates to a method for recovering a negative electrode of a waste lithium ion battery and co-producing a conductive agent.
Background
Lithium ion batteries are widely used in various electronic fields due to their excellent electrochemical properties. According to the data of the State statistical administration, the output of the lithium ion batteries in China in 2013 is about 18 hundred million, and the total production number of the lithium ion batteries in China is more than 250 hundred million by 2020. The service life of the lithium ion battery is generally 2-3 years, and the lithium ion battery is not suitable for being used continuously when the battery capacity is reduced to be below 80%. The increase of the using amount of the lithium ion battery brings a large amount of waste batteries, the lithium ion battery mainly comprises an anode, a cathode, an organic electrolyte and a diaphragm, the waste lithium ion battery contains a large amount of noble metals such as cobalt, lithium and the like, which account for at least one third of the cost of the battery, and the waste battery also contains the electrolyte which is harmful to the environment, so how to recycle the waste lithium ion battery is a hot problem in the current research. However, the recovery treatment of the waste batteries mainly focuses on the recovery of positive metal and negative copper materials, the research on the recovery treatment of negative active materials is few, and the existing negative material recovery scheme is complex, high in cost and single in recovery target, so that a high-value recovery scheme which is short in process, low in cost and capable of simultaneously recovering multiple valuable materials is found, and the method has great significance for the sustainable development of battery recovery industry and resources.
In recent years, with the increasing consumption of fossil fuels and the increasing awareness of environmental protection, chemical power sources have been widely used as alternative energy sources, especially in the field of electric vehicles. According to the forecast of the research center of automobile technology in China, the accumulated scrappage of the power battery of only hybrid power and pure electric (including plug-in type) passenger vehicles in China can reach 12-17 ten thousand tons by estimating according to 30 more than ten thousand new energy automobile sales in 2015 and about 500 ten thousand new energy automobile reserves in 2020 to reach 2020. At present, the recovery treatment of waste batteries mainly focuses on the recovery of high-value metals such as nickel, cobalt, manganese and the like in the positive electrode and the copper of the negative electrode current collector, most of carbon components in the discarded negative electrode are incinerated at high temperature, and the waste of carbon resources in the negative electrode is actually caused. Therefore, it is important to develop a technology for informing the recycling of carbonaceous components in the discarded negative electrode.
Disclosure of Invention
The invention aims to solve the problems that the existing waste negative electrode materials are mainly directly incinerated and the recovery means is lack of different technologies, and mainly aims to provide a method for co-producing a high-performance conductive agent by utilizing a scrapped lithium ion battery negative electrode, so that the high-value reuse of the waste negative electrode materials is realized, and the high-performance conductive agent is obtained by co-production.
A method for recycling a waste lithium ion battery cathode and co-producing a conductive agent comprises the following steps:
crushing the negative pole pieces of the waste lithium ion batteries, placing the crushed negative pole pieces in water, and stirring to obtain mixed slurry;
step two, placing the mixed slurry in a vibration separation sieve for treatment, wherein oversize products are residual diaphragms or residual copper sheets; filtering the slurry under the sieve to obtain a waste anode material filter cake;
thirdly, removing impurities from the filter cake obtained in the second step by using concentrated sulfuric acid to obtain purified carbon powder;
step four, carrying out surface modification treatment on the purified carbon powder to obtain modified carbon powder;
step five: and reducing the modified carbon powder to obtain the conductive agent.
The invention changes the technical prejudice that the existing cathode material is mainly treated by burning, and innovatively provides a thought for preparing a conductive agent by using the cathode material. In order to realize the brand new thought, the invention innovatively provides the method, the anode material is obtained by stirring and separating water, and the processes of impurity removal by concentrated sulfuric acid, surface modification and reduction are innovatively utilized, so that the components in the waste anode material are converted into the material required by the composite conductive agent.
Preferably, the negative electrode sheet is crushed to obtain a material with the particle size of 1-10 mm.
Preferably, in the step one, the liquid-solid ratio (m L/g) of the crushed negative pole pieces added into water is (3-5):1, the stirring speed is 1000-.
Preferably, the mesh opening of the oscillating separating screen in the second step is 240-400 meshes.
Step three, mixing concentrated sulfuric acid with the filter cake obtained in the step two according to a liquid-solid ratio (0.5-2):1, then placing the mixture in a closed furnace at the temperature of 150-; then, the treated material is rinsed by deionized water until the pH value is 6.8-7, and then the material is filtered to obtain purified carbon powder.
The fourth step comprises the following steps:
step 1, slowly adding the purified filter cake obtained in the step three into concentrated sulfuric acid according to a liquid-solid ratio (m L/g) (10-40) of 1, uniformly stirring, transferring the solution into an ice bath (0 ℃), then adding sodium nitrate with the same mass as the filter cake, stirring for 1-1.5h, adding potassium permanganate with the weight being 3-5 times that of the filter cake, and continuously stirring for 1-1.5 h;
step 2, transferring the solution into a constant temperature water bath at 35-40 ℃, adding deionized water into a sulfuric acid solution at the speed of 1-2m L/min, wherein the adding amount of the deionized water is 1 time of the amount of the sulfuric acid, and then adding H with the volume of the sulfuric acid (1/8-1/10)2O2Obtaining a suspension;
step 3, slowly pouring the suspension into a dilute hydrochloric acid solution with the concentration of 5-10 percent and the volume of 5-10 times of the suspension, standing for 1-2 hours, pouring out supernatant liquid, and then adding deionized water until the pH value of the suspension reaches 6.8-7;
and 4, placing the suspension obtained in the previous step in a freeze drying box for freeze drying to obtain the modified carbon powder.
Preferably, in step five, the modified carbon powder is added in H2And under the protection of Ar atmosphere, heating to 600-800 ℃ at the speed of 1-5 ℃/min, and carrying out reduction treatment to obtain the conductive agent.
The invention is beneficial to obtaining the conductive agent material taking the lamellar structure as the main body through the combined control of the steps and the parameters, and the co-produced material is found to have excellent conductive performance.
Preferably, the main indexes of the prepared conductive agent are ① D50 particle size range of 5nm-3.5um, ② specific surface area of 300-1000m2③ conductivity 1 × 104-1×105S/m。
Compared with the prior art, the invention has the following advantages:
(1) provides a brand-new idea of high-value recovery of waste negative electrodes, namely co-producing the waste negative electrodes to obtain the high-quality conductive agent.
(2) The conductive agent with high performance can be prepared by water treatment, concentrated sulfuric acid impurity removal, surface modification and reduction and the combination of the parameters of all the steps.
Drawings
FIG. 1 is a flow chart of an embodiment of the present invention
FIG. 2 is an SEM photograph of a conductive agent obtained in an example of the present invention
Detailed Description
The following further describes the practice of the present invention with reference to the drawings, but the present invention is not limited thereto.
See fig. 1.
The invention provides a preparation method of a conductive agent prepared from a waste lithium ion battery cathode, which comprises the following steps:
in the step, the liquid-solid ratio (m L/g) of the waste lithium ion battery negative electrode added into the water is (3-5):1, and the strong stirring refers to continuously stirring the solution at the stirring speed of 1000 plus materials and 5000rpm for 1-3h, wherein the temperature of the solution system is 60-90 ℃.
And step two, separating the carbonaceous components in the mixed slurry. The mixed slurry is placed in a vibration separation sieve for treatment, the oversize product is a residual diaphragm or a residual copper sheet in the large-size waste lithium ion battery cathode, and the filter cake obtained after the undersize slurry is filtered enters the next step. And step two, the mesh opening of the oscillating separation screen is 240-400 meshes.
And step three, deeply removing impurities, namely removing fluorine, organic matters and metal impurities in the filter cake obtained in the step two to obtain purified carbon powder. Thirdly, deeply removing impurities, namely removing fluorine, organic matters and metal impurities in the carbon components by adopting concentrated sulfuric acid, and specifically, mixing the concentrated sulfuric acid with the filter cake obtained in the second step according to a liquid-solid ratio (0.5-2):1, then placing the mixture in a closed furnace at the temperature of 150-240 ℃ for treatment for 2-4h, continuously introducing air into the furnace in the treatment process, and maintaining the positive pressure in the furnace at 0.1-0.2 Mpa; and then, rinsing the treated material by using deionized water until the pH value is 6.8-7, and filtering to obtain a purified filter cake.
Step 1, slowly adding the purified filter cake obtained in the step three into concentrated sulfuric acid according to a liquid-solid ratio (m L/g) (10-40):1, uniformly stirring, transferring the solution into an ice bath (0 ℃), adding sodium nitrate with the same mass as the filter cake, stirring for 1-1.5h, adding a filter, and filteringStirring for 1-1.5 hr with 3-5 times of potassium permanganate, transferring the solution to 35-40 deg.C constant temperature water bath, adding deionized water at 1-2m L/min to sulfuric acid solution with the amount of deionized water being 1 time of sulfuric acid, and adding hydrogen (1/8-1/10) in volume2O2Obtaining a suspension; step 3, slowly pouring the suspension into a dilute hydrochloric acid solution with the concentration of 5-10 percent and the volume of 5-10 times of the suspension, standing for 1-2 hours, pouring out supernatant liquid, and then adding deionized water until the pH value of the suspension reaches 6.8-7; and 4, placing the suspension obtained in the previous step in a freeze drying box for freeze drying to obtain the modified carbon powder.
Step five: and reducing the modified carbon powder to obtain the conductive agent prepared from the waste lithium ion battery cathode. The reduction of the modified carbon powder in the step refers to that the modified carbon powder is reduced in H2and/Ar atmosphere protection, heating at 1-5 ℃/min and 600-.
Example 1: preparation of conductive agent for high-capacity high-rate lithium ion battery by using scrapped lithium battery cathode
Step one, adding a waste graphite cathode into deionized water according to a liquid-solid ratio of 5:1, and continuously stirring for 3 hours at a stirring speed of 5000rpm, wherein the temperature of a solution system is 90 ℃, so as to obtain mixed slurry;
and step two, placing the mixed slurry obtained in the previous step into a vibration separation sieve with a 400-mesh sieve for treatment, and filtering the obtained slurry under the sieve to obtain a filter cake which is fed into the next step.
Thirdly, adding the filter cake obtained in the second step into concentrated sulfuric acid according to the liquid-solid ratio of 2:1, then placing the mixture into a closed furnace at 220 ℃ for treatment for 4 hours, continuously introducing air into the furnace in the treatment process, and maintaining the positive pressure in the furnace to be 0.15 Mpa; then, the treated material was rinsed with deionized water until the pH was 6.8-7 and filtered to obtain a purified filter cake (purified carbon powder).
Step 1, slowly adding the purified filter cake obtained in the step three into concentrated sulfuric acid according to a (m L/g) liquid-solid ratio of 40:1, uniformly stirring, transferring the solution into an ice bath (0 ℃), and then adding nitric acid with the same mass as the filter cakeSodium, stirring for 1.5H, adding potassium permanganate with the amount 5 times that of the filter cake, stirring for 1.5H, moving the solution to a constant-temperature water bath at 35 ℃, adding deionized water into a sulfuric acid solution at the speed of 1-2m L/min, wherein the addition amount of the deionized water is 1 time of that of the sulfuric acid, and then adding H with the volume of 1/8 sulfuric acid2O2Obtaining a suspension; step 3, slowly pouring the suspension into a dilute hydrochloric acid solution with the concentration of 10 percent and the volume of 10 times of the suspension, standing for 2 hours, pouring out supernatant liquor, and then adding deionized water until the pH value of the suspension reaches 6.8-7; and 4, placing the suspension obtained in the previous step in a freeze drying box for freeze drying to obtain the modified carbon powder.
Step five: and reducing the modified carbon powder to obtain the conductive agent prepared from the waste lithium ion battery cathode. The reduction of the modified carbon powder in the step refers to that the modified carbon powder is reduced in H2And heating to 600-800 ℃ at 1 ℃/min under the protection of Ar atmosphere for reduction treatment to obtain the conductive agent of the embodiment.
The SEM photograph of the conductive agent obtained in this example is shown in FIG. 2, and has a lamellar structure with a particle size D50 of 40-50nm and a specific surface area of 625m2(ii)/g, the conductivity is 12S/cm, and the oil absorption DBP is 305m L/100 g.
Claims (8)
1. A method for recycling a waste lithium ion battery cathode and co-producing a conductive agent is characterized by comprising the following steps:
crushing the negative pole pieces of the waste lithium ion batteries, placing the crushed negative pole pieces in water, and stirring to obtain mixed slurry;
step two, placing the mixed slurry in a vibration separation sieve for treatment, wherein oversize products are residual diaphragms or residual copper sheets; filtering the slurry under the sieve to obtain a filter cake, and performing the next step;
thirdly, removing impurities from the filter cake obtained in the second step by using concentrated sulfuric acid to obtain purified carbon powder;
step four, carrying out surface modification treatment on the purified carbon powder to obtain modified carbon powder;
step five: and reducing the modified carbon powder to obtain the conductive agent.
2. The method as claimed in claim 1, wherein in the step one, the liquid-solid ratio (m L/g) of the crushed negative electrode piece added into water is (3-5) 1, the stirring speed is 1000-5000rpm, the stirring time is 1-3h, and the temperature of the solution system in the stirring process is 60-90 ℃.
3. The method as claimed in claim 1, wherein the mesh size of the oscillating separating screen in step two is 240-400 mesh.
4. The method as claimed in claim 1, wherein the third step comprises mixing concentrated sulfuric acid with the filter cake obtained in the second step in a liquid-solid ratio (0.5-2):1, and treating in a closed furnace at 150-; then, the treated material is rinsed by deionized water until the pH value is 6.8-7, and then the material is filtered to obtain purified carbon powder.
5. The method of claim 3, wherein step four comprises the steps of:
step 1, slowly adding the purified filter cake obtained in the step three into concentrated sulfuric acid according to a liquid-solid ratio (m L/g) (10-40) of 1, uniformly stirring, transferring the solution into an ice bath (0 ℃), then adding sodium nitrate with the same mass as the filter cake, stirring for 1-1.5h, adding potassium permanganate with the weight being 3-5 times that of the filter cake, and continuously stirring for 1-1.5 h;
step 2, transferring the solution into a constant temperature water bath at 35-40 ℃, adding deionized water into a sulfuric acid solution at the speed of 1-2m L/min, wherein the adding amount of the deionized water is 1 time of the amount of the sulfuric acid, and then adding H with the volume of the sulfuric acid (1/8-1/10)2O2Obtaining a suspension;
step 3, slowly pouring the suspension into a dilute hydrochloric acid solution with the concentration of 5-10 percent and the volume of 5-10 times of the suspension, standing for 1-2 hours, pouring out supernatant liquid, and then adding deionized water until the pH value of the suspension reaches 6.8-7;
and 4, placing the suspension obtained in the previous step in a freeze drying box for freeze drying to obtain the modified carbon powder.
6. The method as claimed in claim 5, wherein in step five, the modified carbon powder is added in H2And under the protection of Ar atmosphere, heating to 600-800 ℃ at the speed of 1-5 ℃/min, and carrying out reduction treatment to obtain the conductive agent.
7. The method according to claim 1, wherein the particle size of the crushed negative electrode sheet is 1-10 mm.
8. The method according to any one of claims 1 to 7, wherein the D50 particle size of the prepared conductive agent is in the range of 5nm to 3.5 um; the specific surface area is 300-1000m2Per g, conductivity 1 × 104-1×105S/m。
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