CN115101842A - Method for recovering graphite from waste lithium ion battery mixture - Google Patents
Method for recovering graphite from waste lithium ion battery mixture Download PDFInfo
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- CN115101842A CN115101842A CN202210682300.7A CN202210682300A CN115101842A CN 115101842 A CN115101842 A CN 115101842A CN 202210682300 A CN202210682300 A CN 202210682300A CN 115101842 A CN115101842 A CN 115101842A
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- 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
Abstract
The invention relates to the field of lithium ion battery recovery, in particular to a method for recovering graphite from a waste lithium ion battery mixture. The method comprises the following steps: primary acid leaching: carrying out primary acid leaching on the heat-treated raw material by using a primary acid leaching reagent; secondary acid leaching: performing secondary acid leaching on the mixture subjected to the primary acid leaching treatment by using a secondary acid leaching agent; alkaline leaching: removing impurities from the mixture subjected to the secondary acid leaching treatment by adopting an alkali solution; the raw materials are anode and cathode mixture materials or cathode materials of the waste lithium ion battery; the primary acid leaching reagent is inorganic acid and/or an oxidizing agent; the secondary acid leaching reagent is an organic acid mixed solution added with a surfactant. The method for recovering the high-purity graphite from the anode and cathode mixed materials/cathode materials of the broken waste lithium ion batteries has the characteristics of high graphite recovery rate, high graphite purity, wide application range and the like.
Description
Technical Field
The invention relates to the field of lithium ion battery recovery, in particular to a method for recovering graphite from a waste lithium ion battery mixture.
Background
In recent years, the sales volume of new energy automobiles is steadily increased, and the development level of lithium ion batteries, which are used as core components influencing the endurance mileage and the safety performance of new energy automobiles, directly determines the industrial scale and the development level of new energy automobiles. The output of the current lithium ion power battery is frequently innovative. The service life of the lithium ion power battery is about 5-7 years, and the accumulated retirement amount of the power battery in the market in 2020 reaches 20 ten thousand tons. By 2025, the decommissioning amount of the lithium ion battery reaches 64 ten thousand tons, wherein the decommissioning amount of the power battery accounts for more than half of the total amount of the lithium ion battery, and the recycling of the lithium ion battery is gradually a research hotspot.
The invention discloses a method for recovering graphite from waste batteries with the publication number of CN101710632, which removes impurities from a battery material obtained by crushing and separating, washes and dries the battery material, and then recovers the recovered graphite at high temperature. At present, the research on graphite recovery in waste batteries is mainly to recover graphite on a negative electrode material, but the current industrial production cannot meet the requirement of separate separation of the negative electrode material of the waste batteries and only can recover a positive electrode mixed material and a negative electrode mixed material. At present, the recovery of high-purity graphite in a battery mixture is difficult, the purity of the recovered graphite is not high, the recovery rate is low, and the structure of the recovered graphite is poor. Therefore, there is a need in the art to provide a new method for recovering graphite from waste lithium batteries.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for recovering graphite from a waste lithium ion battery mixture.
The invention provides a method for recovering graphite from a waste lithium ion battery mixture, which comprises the following steps:
primary acid leaching: carrying out primary acid leaching on the heat-treated raw material by using a primary acid leaching reagent;
secondary acid leaching: performing secondary acid leaching on the mixture subjected to the primary acid leaching treatment by using a secondary acid leaching agent;
alkaline leaching: removing impurities from the mixture subjected to the secondary acid leaching treatment by adopting an alkali solution;
the raw materials are anode and cathode mixture materials or cathode materials of the waste lithium ion battery; the primary acid leaching reagent is inorganic acid and/or an oxidizing agent; the secondary acid leaching reagent is an organic acid mixed solution added with a surfactant. The method for recovering high-purity graphite from the anode and cathode mixed materials/cathode materials of the broken waste lithium ion batteries has the characteristics of high graphite recovery rate, high graphite purity, high extraction efficiency, wide application range and the like.
Preferably, the method for recovering graphite from the waste lithium ion battery mixture provided by the invention comprises the following steps:
1) and (3) heat treatment: carrying out heat treatment on the anode and cathode mixture or the cathode material of the waste lithium ion battery to obtain a heat-treated mixture;
2) primary acid leaching: carrying out primary acid leaching on the mixture after heat treatment by using a primary acid leaching reagent, wherein the primary acid leaching reagent is H 2 SO 4 And H 2 O 2 Mixed solution of (1), H 2 SO 4 With HNO 3 Mixed solution of (2) or HNO 3 Preferably, the liquid-solid ratio is 10-50: 1, and the mixture is filtered and washed to be neutral to obtain a mixture after primary acid leaching;
3) secondary acid leaching: carrying out secondary acid leaching on the mixture subjected to primary acid leaching by using a secondary acid leaching reagent, wherein the secondary acid leaching reagent is an organic acid mixed solution added with a surfactant, the liquid-solid ratio is preferably 100-300: 1, and filtering and washing the mixture to be neutral to obtain a mixture subjected to secondary acid leaching; the organic acid of the secondary acid leaching agent is preferably a mixed solution of methanesulfonic acid and citric acid, and the surfactant is preferably hexadecyl trimethyl ammonium bromide; in the invention, by adopting specific primary and secondary acid leaching reagents and conditions, the synergistic effect of the secondary acid leaching reagent and a surfactant (especially mixed acid of methanesulfonic acid and citric acid and hexadecyl trimethyl ammonium bromide) is better exerted, and the content of metal impurities in graphite is better reduced;
4) alkaline leaching: and soaking the mixture subjected to secondary acid leaching by using an alkaline leaching agent, wherein the liquid-solid ratio is preferably 50-150: 1, filtering, washing to be neutral, and drying to obtain recovered graphite;
preferably, in the step 1), the atmosphere of the heat treatment is air, the temperature is 450-700 ℃, and the time is 1-3 h.
More preferably, in the step 2), the primary acid leaching reagent adopts H 2 SO 4 And H 2 O 2 When they are mixed in solution, H 2 SO 4 Has a concentration of 2 to 5mol/L, H 2 O 2 The dosage of the composition is 4 to 12 vol percent. In the present invention, the pickling agent is mixed with an oxidizing agent at a preferable concentration to improve the effect of removing copper impurities.
Preferably, in the step 3), the organic acid of the secondary acid leaching agent is a mixed solution of methanesulfonic acid and citric acid, and the surfactant is cetyl trimethyl ammonium bromide. According to the invention, the specific organic acid mixed acid, the surfactant and the acid leaching reagent are adopted to act synergistically, so that impurity elements of nickel and cobalt can be removed well, and the purity of graphite is further improved.
Further preferably, in the step 3), the concentration of the methanesulfonic acid is 1-6 mol/L, the concentration of the citric acid is 0.5-3 mol/L, and the dosage of the surfactant is 5-100 mg/L.
Further preferably, in the step 2), the leaching time is 0.5-2 h, and the reaction temperature is 30-90 ℃.
Further preferably, in the step 3), the leaching time is 0.5-1.5 h, and the reaction temperature is 30-90 ℃.
Preferably, in the step 4), the alkaline leaching agent is a NaOH solution, and the concentration of the alkaline leaching agent is 0.5-3 mol/L.
Further preferably, in the step 4), the leaching time is 0.5-2 h, and the reaction temperature is 30-90 ℃.
More preferably, in steps 2) to 4), the reaction product is filtered, washed to neutrality and dried at 60 + -5 deg.C for 1 + -0.2 h.
The method for recovering graphite from the waste lithium ion battery mixture provided by the invention comprises the following steps:
1) and (3) heat treatment: carrying out heat treatment on the recycled battery anode and cathode mixture in the air atmosphere, wherein the heat treatment temperature is 450-700 ℃, and the time is 1-3 h;
2) primary acid leaching: by means of H 2 SO 4 And H 2 O 2 The mixed solution is used for leaching the mixture after alkaline leaching, filtering and washing the mixture to be neutral, drying the mixture to obtain the mixture after acid leaching, and H 2 SO 4 Has a concentration of 2 to 5mol/L, H 2 O 2 The dosage of the leaching agent is 4-12 vol%, the leaching time is 0.5-2 h, the reaction temperature is 30-90 ℃, and the liquid-solid ratio is 10-50: 1;
3) secondary acid leaching: adding hexadecyl trimethyl ammonium bromide into a mixed organic acid solution of 1-6 mol/L methanesulfonic acid and 0.5-3 mol/L citric acid, wherein the dosage of a surfactant is 5-100 mg/L, uniformly mixing the solution, performing secondary acid leaching on the mixture after acid leaching, filtering and washing to be neutral, drying, and leaching for 0.5-1.5 h at the reaction temperature of 30-90 ℃ in a liquid-solid ratio of 100-300: 1;
4) alkaline leaching: soaking the calcined positive and negative electrode mixture in NaOH solution, filtering and washing to be neutral, and drying to obtain the alkali-soaked mixture, wherein the concentration of the NaOH solution is 0.5-3 mol/L, the reaction time is 0.5-2 h, the reaction temperature is 30-90 ℃, and the liquid-solid ratio is 50-150: 1.
The invention has the beneficial effects that: according to the invention, the two-step acid leaching of inorganic acid/oxidant-organic acid/surfactant and the three-time leaching of alkaline leaching are combined, so that high-purity graphite can be better recovered from the anode and cathode mixed materials/cathode materials of the crushed waste lithium ion batteries, the impurity removal effect of the graphite is obviously improved, a new thought is provided for treating the waste batteries, and the resource circulation is better realized. The method can be used for extracting the high-purity graphite from the positive and negative electrode mixture of the waste lithium ion battery and can also be used for directly extracting the high-purity graphite from the negative electrode material in the waste lithium ion battery.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is an XRD chart of the raw material used in the examples of the present invention.
FIG. 2 is an XRD picture of the product obtained in example 1 of the present invention.
FIG. 3 is a SEM photograph of the product obtained in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The conditions in the examples may be further adjusted depending on the specific experimental conditions or plant conditions, and the conditions in the conventional experiments are not generally specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the following examples of the present invention, the content of C element in the used crushed mixture of positive and negative electrodes was 5.43%.
Example 1
And weighing 10g of the crushed mixture of the anode and the cathode, and calcining the mixture for 1 hour at the temperature of 600 ℃ to finish the heat treatment.
The heat-treated graphite is prepared by using 5mol/L H 2 SO 4 And 12 vot% H was added 2 O 2 Leaching with a liquid-solid ratio of 30:1, a leaching temperature of 90 ℃ and a leaching time of 1h, filtering, washing to neutrality and drying.
0.015g of cetyltrimethylammonium bromide was added to 300mL of pure water and mixed for 5 min. Adding methanesulfonic acid and citric acid into the solution to prepare a mixed solution with the concentration of the methanesulfonic acid being 3mol/L and the concentration of the citric acid being 0.5 mol/L. Adding the graphite subjected to acid leaching into the mixed solution, wherein the liquid-solid ratio is 150:1, adding magnetons, magnetically stirring for 1h at 90 ℃, then washing to neutrality by using pure water, and performing suction filtration and drying.
And (3) carrying out alkaline leaching on the graphite subjected to secondary acid leaching by using 100mL of 2mol/L NaOH solution, wherein the liquid-solid ratio is 150:1, the leaching temperature is 90 ℃, the alkaline leaching time is 1h, carrying out suction filtration after reaction, and washing to be neutral, wherein the washing frequency of the graphite subjected to alkaline leaching is 5 times, and 200mL of pure water is adopted each time.
The carbon content of the dried mixture can reach 82% by using a carbon-sulfur analyzer for the washed and dried graphite, and the recovery rate is 84.2%. As shown in fig. 3, the flake structure of graphite still remains good. In combination with XRD patterns 1-2, most of impurities are removed after the treatment by the method of the embodiment.
Example 2
10g of the broken mixture of the anode and the cathode is weighed and calcined for 1 hour at the temperature of 600 ℃, and the heat treatment is completed.
The heat-treated graphite is utilized to be 4mol/L H 2 SO 4 And 8 vot% H was added 2 O 2 Leaching at the liquid-solid ratio of 20:1 and the leaching temperature of 60 ℃ for 1h, filtering, washing to neutrality and drying.
0.025g of cetyltrimethylammonium bromide was added to 300mL of purified water and mixed for 5 min. Adding methanesulfonic acid and citric acid into the solution to prepare a mixed solution with the concentration of the methanesulfonic acid being 3mol/L and the concentration of the citric acid being 0.5 mol/L. Adding the graphite subjected to acid leaching into the mixed solution, wherein the liquid-solid ratio is 200:1, adding magnetons, magnetically stirring for 1h at 60 ℃, then washing to neutrality by using pure water, and performing suction filtration and drying.
And (3) carrying out alkaline leaching on the graphite subjected to secondary acid leaching by using 100mL of 1mol/L NaOH solution, wherein the liquid-solid ratio is 100:1, the leaching temperature is 60 ℃, the alkaline leaching time is 1h, carrying out suction filtration after reaction, and washing to be neutral, wherein the washing frequency of the graphite subjected to alkaline leaching is 5 times, and 200mL of pure water is adopted each time.
The carbon content in the dried mixture can reach 64.4% by using a carbon-sulfur analyzer after the graphite is washed and dried, and the recovery rate is 85.5%.
Example 3
And weighing 10g of the crushed mixture of the anode and the cathode, and calcining the mixture for 1 hour at the temperature of 600 ℃ to finish the heat treatment.
The heat-treated graphite is utilized to be 4mol/L H 2 SO 4 And 8 vot% H was added 2 O 2 The liquid-solid ratio is 30:1, the leaching temperature is 60 ℃, the leaching time is 1.5h, and the mixture is filtered, washed to be neutral and dried.
0.005g of cetyltrimethylammonium bromide was added to 300mL of pure water and mixed for 5 min. Adding methanesulfonic acid and citric acid into the solution to prepare a mixed solution with a methanesulfonic acid concentration of 5mol/L and a citric acid concentration of 0.5 mol/L. Adding the graphite subjected to acid leaching into the mixed solution, wherein the liquid-solid ratio is 200:1, adding magnetons, magnetically stirring for 1h at 60 ℃, then washing to neutrality by using pure water, and performing suction filtration and drying.
And (3) carrying out alkaline leaching on the graphite subjected to secondary acid leaching by using 100mL of 1mol/L NaOH solution, wherein the liquid-solid ratio is 100:1, the leaching temperature is 90 ℃, the alkaline leaching time is 1h, carrying out suction filtration after reaction, and washing to be neutral, wherein the washing frequency of the graphite subjected to alkaline leaching is 5 times, and 200mL of pure water is adopted each time.
The carbon content in the dried mixture can reach 80% by using a carbon-sulfur analyzer after the graphite is washed and dried, and the recovery rate is 79.5%.
Comparative example 1
10g of the broken mixture of the anode and the cathode is weighed and calcined for 1 hour at the temperature of 600 ℃, and the heat treatment is completed.
The heat-treated graphite is utilized to be 4mol/L H 2 SO 4 And 8 vot% H was added 2 O 2 Leaching with a liquid-solid ratio of 20:1, a leaching temperature of 90 ℃, a leaching time of 1h, filtering, washing to neutrality, and drying.
Preparing a mixed solution with the concentration of methanesulfonic acid of 3mol/L and the concentration of citric acid of 0.5mol/L, carrying out secondary leaching on the crushed material subjected to primary acid leaching by using organic mixed acid, wherein the liquid-solid ratio is 150:1, adding magnetons, carrying out magnetic stirring for 1h at 90 ℃, washing to be neutral by using pure water, and carrying out suction filtration and drying.
The carbon content in the dried mixture can reach 58.6% and the recovery rate is 68.7% by using a carbon-sulfur analyzer for the washed and dried graphite.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for recovering graphite from a waste lithium ion battery mixture is characterized by comprising the following steps:
primary acid leaching: carrying out primary acid leaching on the heat-treated raw material by using a primary acid leaching reagent;
secondary acid leaching: performing secondary acid leaching on the mixture subjected to the primary acid leaching treatment by using a secondary acid leaching agent;
alkaline leaching: removing impurities from the mixture subjected to the secondary acid leaching treatment by adopting an alkali solution;
the raw materials are anode and cathode mixture materials or cathode materials of the waste lithium ion battery; the primary acid leaching agent is inorganic acid and/or an oxidizing agent; the secondary acid leaching reagent is an organic acid mixed solution added with a surfactant.
2. The method for recovering graphite from the waste lithium ion battery mixture as claimed in claim 1, is characterized by comprising the following steps:
1) and (3) heat treatment: carrying out heat treatment on the anode and cathode mixture or the cathode material of the waste lithium ion battery to obtain a heat-treated mixture;
2) primary acid leaching: carrying out primary acid leaching on the mixture after the heat treatment by using a primary acid leaching reagent, wherein the primary acid leaching reagent is H 2 SO 4 And H 2 O 2 Mixed solution of (1), H 2 SO 4 With HNO 3 Mixed solution of (2) or HNO 3 The liquid-solid ratio is preferably 10-50: 1, the mixture is filtered and washed to be neutral,obtaining a mixture after primary acid leaching;
3) secondary acid leaching: performing secondary acid leaching on the mixture subjected to primary acid leaching by using a secondary acid leaching reagent, wherein the secondary acid leaching reagent is an organic acid mixed solution added with a surfactant, the liquid-solid ratio is preferably 100-300: 1, and filtering and washing to be neutral to obtain a mixture subjected to secondary acid leaching;
4) alkaline leaching: and soaking the mixture subjected to secondary acid leaching by using an alkaline leaching agent, wherein the liquid-solid ratio is preferably 50-150: 1, filtering, washing to be neutral, and drying to obtain the recovered graphite.
3. The method for recovering graphite from the waste lithium ion battery mixture according to claim 2, wherein in the step 1), the heat treatment atmosphere is air, the temperature is 450-700 ℃, and the time is 1-3 h.
4. The method for recovering graphite from waste lithium ion battery mixtures according to any one of claims 2 to 3, wherein in the step 2), the primary acid leaching agent is added with H 2 SO 4 And H 2 O 2 When they are mixed in solution, H 2 SO 4 Has a concentration of 2 to 5mol/L, H 2 O 2 The dosage of the composition is 4 to 12 vol percent.
5. The method for recovering graphite from waste lithium ion battery mixtures according to any one of claims 2 to 4, wherein in the step 3), the organic acids of the secondary acid leaching agent are methanesulfonic acid and citric acid, and the surfactant is cetyltrimethylammonium bromide.
6. The method for recycling graphite from waste lithium ion battery mixtures according to claim 5, wherein in the step 3), the concentration of methanesulfonic acid is 1-6 mol/L, the concentration of citric acid is 0.5-3 mol/L, and the dosage of the surfactant is 5-100 mg/L.
7. The method for recovering graphite from the waste lithium ion battery mixture according to any one of claims 4 to 6, wherein in the step 2), the leaching time is 0.5 to 2 hours, and the reaction temperature is 30 to 90 ℃; in the step 3), the leaching time is 0.5-1.5 h, and the reaction temperature is 30-90 ℃.
8. The method for recovering graphite from waste lithium ion battery mixtures according to any one of claims 2 to 7, wherein in the step 4), the alkaline leaching agent is NaOH solution, and the concentration of the alkaline leaching agent is 0.5-3 mol/L.
9. The method for recovering graphite from waste lithium ion batteries according to claim 8, wherein in the step 4), the leaching time is 0.5-2 hours, and the reaction temperature is 30-90 ℃.
10. The method for recovering graphite from waste lithium ion battery mixtures according to any one of claims 2 to 9, wherein in the steps 2) to 4), the reaction product is filtered, washed to be neutral, and dried at 60 ± 5 ℃ for 1 ± 0.2 h.
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