CN112886085B - Method for regenerating ternary lithium ion battery anode material by ion exchange method - Google Patents
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Abstract
The invention relates to a method for regenerating a ternary lithium ion battery anode material by an ion exchange method. Crushing and screening the waste lithium ion battery anode material, and roasting for 1-3 hours by microwave oxidation to obtain a pretreated waste electrode material; adding the pretreated waste electrode material into dilute hydrochloric acid to react for 3-5 h, controlling the pH value of a system by using ammonia water to precipitate aluminum, and performing solid-liquid separation to obtain an aluminum-removed filtrate; adding cation exchange resin into the aluminum-removed filtrate, performing ion exchange treatment, washing the cation exchange resin with deionized water, drying, adding metal carbonate to supplement lithium, nickel, cobalt and manganese elements, and grinding uniformly to obtain a mixture A; and placing the mixture A in a closed tubular microwave oven, continuously introducing air, uniformly heating the mixture A to 150-200 ℃ by microwave at a constant speed, preserving the heat for 20-30 min, uniformly heating the mixture A to 850-1000 ℃ at a constant speed, and preserving the heat for 4-6 h to obtain the ternary lithium ion battery anode material. The invention prepares the ternary lithium ion battery anode by directly regenerating the waste lithium ion battery, and can avoid a complex separation process.
Description
Technical Field
The invention relates to a method for regenerating a ternary lithium ion battery anode material by an ion exchange method, belonging to the technical field of lithium ion battery anode materials.
Background
With the development of new energy automobiles, the first electric automobiles are operated for more than 20 kilometers, which means that part of power batteries begin to enter a scrapping period. The arrival of the end-of-life also brings great market opportunity to the battery recycling industry. On one hand, the recovery of the power battery is in consideration of safety, the voltage of the power battery is high-voltage direct current, a passenger car reaches more than 300 volts, a bus reaches more than 600 volts, and safety accidents are easy to occur if the power battery is not recovered in time; on the other hand, battery recycling can extract valuable resources.
At present, in the known technology, the Luyao and the like are firstly treated with citric acid and H2O2Leaching of LiNi1/3Co1/3Mn1/3O2Then, thenBy addition of LiNO3、Ni(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO)3)2The metal ion ratio is adjusted to 3.05:1:1:1, the pH is adjusted to 8.0, transparent sol is obtained by heating in water bath at 80 ℃, then drying is carried out for 24h at 110 ℃, and finally the dried gel is calcined at 350 ℃ for 2h and at 750 ℃ for 12h to obtain the regenerated cathode material. The organic matter used by the method is harmful to health, the preparation period is long, the anode material is easy to shrink, and the quality is poor. Dissolving the positive electrode material in 1mol/L H2SO4And 1 vol% H2O2By adding NiSO4·6H2O，CoSO4·7H2O and MnSO4·H2And O, adjusting the molar ratio of Ni to Co to Mn in the leaching solution to be 1:1: 1. Then reacting for 12h under the conditions of pH 7.5 and 60 ℃, and precipitating Ni1/3Co1/ 3Mn1/3CO3Calcining at 500 ℃ for 5h to obtain (Ni)1/3Co1/3Mn1/3)3O4An intermediate. Then the metal oxide is reacted with Li2CO3Mixed well at a molar ratio of 1.06. Finally, preheating the mixture at 500 ℃ for 5h, and then sintering at 900 ℃ for 12h in an air atmosphere to obtain regenerated LiNi1/3Co1/3Mn1/3O2. The disadvantages of this method are that the addition of the precipitant may result in too high a local concentration, agglomeration or insufficiently uniform composition, and an excessively complex experimental procedure. Therefore, a new regeneration method with a short process route and environmental friendliness is continuously sought.
Disclosure of Invention
The invention provides a method for regenerating a ternary lithium ion battery anode material by an ion exchange method aiming at the problem of battery recovery in the prior art, wherein cation exchange resin is used for adsorption, drying and grinding, so that metals are directly and uniformly mixed without being respectively recovered; the microwave field is introduced, the unique energy transfer mode and the selective heating characteristic of the microwave are fully utilized, the raw material pyrolysis and the high-temperature solid sintering are carried out, and the time is greatly shortened.
A method for regenerating a ternary lithium ion battery anode material by an ion exchange method comprises the following specific steps:
(1) crushing and screening the waste lithium ion battery anode material, and then roasting for 1-3 h by microwave oxidation to obtain a pretreated waste electrode material;
(2) adding the waste electrode material pretreated in the step (1) into dilute hydrochloric acid, reacting for 3-5 hours at the temperature of 80-90 ℃ under the stirring condition, controlling the pH value of a system by adopting ammonia water to precipitate aluminum, performing solid-liquid separation to obtain an aluminum-removed filtrate, and adjusting the pH value of the aluminum-removed filtrate to 9.5-10.5;
(3) adding cation exchange resin into the aluminum-removed filtrate obtained in the step (2), performing ion exchange treatment under the stirring condition, flushing the cation exchange resin with deionized water, drying, adding metal carbonate to supplement one or more of lithium, nickel, cobalt and manganese elements, and uniformly grinding to obtain a mixture A;
(4) placing the mixture A in the step (3) in a closed tubular microwave oven, continuously introducing air, uniformly heating the microwave to 150-200 ℃ at a constant speed, preserving the heat for 20-30 min, uniformly heating to 850-1000 ℃ at a constant speed, preserving the heat for 4-6 h, cooling along with the oven, and grinding to obtain the ternary lithium ion battery anode material;
the anode material of the waste lithium ion battery in the step (1) is a waste nickel cobalt lithium manganate battery, a waste lithium manganate battery or a waste lithium cobaltate battery, and the temperature of microwave oxidation roasting is 550-700 ℃;
the concentration of the dilute hydrochloric acid in the step (2) is 5-6 mol/L, and the stirring speed is 500-800 r/min;
the pH value of the ammonia water control system in the step (2) is 4-4.5;
the cation exchange resin in the step (3) is strong-acid cation exchange resin, and the stirring speed is 500-800 r/min;
the molar ratio of nickel, cobalt and manganese in the mixture A is (1-5) to (1-3) to (1-8);
the air introducing speed in the step (4) is 500-1000 ml/min, and the microwave power for uniform temperature rise is 1000-1500W;
the microwave frequency adopted in the microwave heating-up stage and the heat preservation stage is 2450MHz, the furnace body of the tubular microwave oven is horizontally placed, the microwave generator irradiates materials from the bottom, and the furnace body drives the materials to do self-rotation motion in the vertical direction at the rotating speed of 5-8 r/min in the whole heating process, so that the materials are uniformly heated.
The invention has the beneficial effects that:
(1) the whole process of the invention is directly sintered to prepare the anode material, thereby saving the process of generating the precursor, saving energy and reducing consumption;
(2) the method has short process flow, the utilization rate of the nickel, cobalt, manganese and lithium is more than 80 percent, the aim of simply and effectively utilizing the valuable metals of nickel, cobalt, manganese and lithium in the waste nickel, cobalt and manganese ternary lithium ion battery is fulfilled, and the process time is greatly shortened by using microwave roasting.
Drawings
FIG. 1 is a process flow diagram of regeneration of ternary lithium ion battery positive electrode material by ion exchange method;
FIG. 2 is a microwave roasting process;
FIG. 3 is a graph of cycle performance of the regenerated ternary lithium ion battery positive electrode material of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a method for regenerating a ternary lithium ion battery cathode material by an ion exchange method (see figure 1) comprises the following steps:
(1) crushing and screening the positive electrode material of the waste lithium manganate battery (sieving with a 150-mesh sieve), screening out solid impurities such as plastics and the like, then carrying out microwave oxidation roasting for 1h in a microwave tube furnace at the temperature of 600 ℃, and removing organic matters contained in the raw material to obtain a pretreated waste electrode material;
(2) adding the waste electrode material pretreated in the step (1) into dilute hydrochloric acid with the concentration of 5mol/L, reacting at the temperature of 85 ℃ and the stirring speed of 600r/min for 3 hours at constant temperature to ensure that metals exist in an ionic state, controlling the pH value of a system to be 4 by adopting ammonia water to ensure that aluminum ions are precipitated in an aluminum hydroxide form, carrying out solid-liquid separation to obtain an aluminum-removed filtrate, adding the filtrate containing NH4Of ClAdjusting the pH value of the aluminum-removed filtrate to 9.5 so as to fully complex metal ions and ammonia;
(3) adding 0017 x (732) strong-acid styrene cation exchange resin into the aluminum-removed filtrate obtained in the step (2), performing ion exchange treatment at the stirring speed of 600r/min and at room temperature, washing the cation exchange resin with deionized water, performing microwave drying, adding metal carbonate to supplement one or more of lithium, nickel, cobalt and manganese elements, and grinding for 3 hours by using a vacuum planetary ball mill to obtain a mixture A; wherein the molar ratio of nickel, cobalt and manganese in the mixture A is 5:2: 3;
(4) placing the mixture A obtained in the step (3) in a closed tubular microwave oven, continuously introducing air with the flow rate of 600ml/min, uniformly heating the mixture to the temperature of 180 ℃ by microwave, preserving the heat for 20min to completely combust the resin, uniformly heating the mixture to the temperature of 900 ℃ and preserving the heat for 4h, cooling the mixture along with the oven, and grinding the mixture to obtain the ternary lithium ion battery anode material (the microwave roasting process is shown in figure 2);
the cycle performance curve of the regenerated ternary lithium ion battery anode material is shown in fig. 3, and fig. 3 shows that the capacity of the anode material is 145.33mAh/g under the multiplying power of 0.2C, after 30 cycles, the discharge capacity is 121.81mAh/g, the capacity retention rate is 83.82%, and the anode material has better multiplying power performance.
Example 2: a method for regenerating a ternary lithium ion battery cathode material by an ion exchange method (see figure 1) comprises the following steps:
(1) crushing and screening the positive electrode material of the waste nickel-cobalt lithium manganate battery (sieving with a 200-mesh sieve), screening out solid impurities such as plastics and the like, then carrying out microwave oxidation roasting for 2 hours in a microwave tube furnace at the temperature of 650 ℃, and removing organic matters contained in the raw material to obtain a pretreated waste electrode material;
(2) adding the waste electrode material pretreated in the step (1) into dilute hydrochloric acid with the concentration of 5.5mol/L, reacting at the temperature of 85 ℃ and the stirring speed of 700r/min for 3h at constant temperature to ensure that metals exist in an ionic state, controlling the pH value of a system to be 4 by adopting ammonia water to ensure that aluminum ions precipitate in an aluminum hydroxide form, carrying out solid-liquid separation to obtain an aluminum-removed filtrate, adding the filtrate containing NH4The pH value of the aluminum-removed filtrate is adjusted to be Cl by ammonia water solution10 to complex the metal ions with ammonia sufficiently;
(3) adding 0017 x (732) strong-acid styrene cation exchange resin into the aluminum-removed filtrate obtained in the step (2), performing ion exchange treatment at the stirring speed of 700r/min and at room temperature, washing the cation exchange resin with deionized water, performing microwave drying, adding metal carbonate to supplement one or more of lithium, nickel, cobalt and manganese elements, and grinding for 4 hours by using a vacuum planetary ball mill to obtain a mixture A; wherein the molar ratio of nickel, cobalt and manganese in the mixture A is 1:1: 1; want to
(4) Placing the mixture A obtained in the step (3) in a closed tubular microwave oven, continuously introducing air with the flow of 800ml/min, uniformly heating the mixture to 190 ℃ by microwave, preserving the temperature for 25min to completely combust the resin, uniformly heating the mixture to 950 ℃ and preserving the temperature for 5h, cooling the mixture along with the oven, and grinding the mixture to obtain the ternary lithium ion battery anode material (the microwave roasting process is shown in figure 2);
the capacity of the anode material is 140.38mAh/g under the multiplying power of 0.2C, after 30 times of circulation, the discharge capacity is 113.25mAh/g, the capacity retention rate is 80.67%, and the anode material has better multiplying power performance.
Example 3: a method for regenerating a ternary lithium ion battery cathode material by an ion exchange method (see figure 1) comprises the following steps:
(1) crushing and screening the waste lithium cobalt oxide battery positive electrode material (sieving with a 300-mesh sieve), screening out solid impurities such as plastics and the like, then carrying out microwave oxidation roasting for 1h in a microwave tube furnace at the temperature of 700 ℃, and removing organic matters contained in the raw material to obtain a pretreated waste electrode material;
(2) adding the waste electrode material pretreated in the step (1) into dilute hydrochloric acid with the concentration of 6mol/L, reacting at the temperature of 85 ℃ and the stirring speed of 800r/min for 3 hours at constant temperature to ensure that metals exist in an ionic state, controlling the pH value of a system to be 4 by adopting ammonia water to ensure that aluminum ions are precipitated in an aluminum hydroxide form, carrying out solid-liquid separation to obtain an aluminum-removed filtrate, adding the filtrate containing NH4Adjusting the pH value of the aluminum-removing filtrate to 10.5 to fully complex metal ions and ammonia by using the ammonia water solution of Cl;
(3) adding 0017 x (732) strong-acid styrene cation exchange resin into the aluminum-removed filtrate obtained in the step (2), performing ion exchange treatment at the stirring speed of 800r/min and at room temperature, washing the cation exchange resin with deionized water, performing microwave drying, adding metal carbonate to supplement one or more of lithium, nickel, cobalt and manganese elements, and grinding for 5 hours by using a vacuum planetary ball mill to obtain a mixture A; wherein the molar ratio of nickel, cobalt and manganese in the mixture A is 1:1: 1;
(4) placing the mixture A in the step (3) in a closed tubular microwave oven, continuously introducing air with the flow rate of 1000ml/min, uniformly heating the microwave to the temperature of 200 ℃ and preserving the heat for 30min to completely combust the resin, uniformly heating to the temperature of 1000 ℃ and preserving the heat for 4.5h, cooling along with the oven, and grinding to obtain the ternary lithium ion battery anode material (the microwave roasting process is shown in figure 2);
the capacity of the positive electrode material is 148.52mAh/g under the multiplying power of 0.2C, after 30 times of circulation, the discharge capacity is 127.86mAh/g, the capacity retention rate is 86.09%, and the positive electrode material has excellent multiplying power performance.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (7)
1. A method for regenerating a ternary lithium ion battery anode material by an ion exchange method is characterized by comprising the following specific steps:
(1) crushing and screening the waste lithium ion battery anode material, and then roasting for 1-3 h by microwave oxidation to obtain a pretreated waste electrode material; wherein the temperature of microwave oxidizing roasting is 550-700 ℃;
(2) adding the pretreated waste electrode material obtained in the step (1) into dilute hydrochloric acid, reacting for 3-5 hours at the temperature of 80-90 ℃ under the stirring condition, controlling the pH value of a system by adopting ammonia water to precipitate aluminum, performing solid-liquid separation to obtain an aluminum-removed filtrate, and adjusting the pH value of the aluminum-removed filtrate to 9.5-10.5;
(3) adding cation exchange resin into the aluminum-removed filtrate obtained in the step (2), performing ion exchange treatment under the stirring condition, flushing the cation exchange resin with deionized water, drying, adding metal carbonate to supplement one or more of lithium, nickel, cobalt and manganese elements, and uniformly grinding to obtain a mixture A;
(4) and (3) placing the mixture A obtained in the step (3) in a closed tubular microwave oven, continuously introducing air, uniformly heating the microwave to 150-200 ℃ and preserving the heat for 20-30 min, uniformly heating to 850-1000 ℃ and preserving the heat for 4-6 h, cooling along with the oven, and grinding to obtain the ternary lithium ion battery anode material.
2. The method for regenerating the ternary lithium ion battery cathode material by the ion exchange method according to claim 1, is characterized in that: the waste lithium ion battery in the step (1) is a waste nickel cobalt lithium manganate battery, a waste lithium manganate battery or a waste lithium cobaltate battery.
3. The method for regenerating the ternary lithium ion battery cathode material by the ion exchange method according to claim 1, is characterized in that: the concentration of the dilute hydrochloric acid in the step (2) is 5-6 mol/L, and the stirring speed is 500-800 r/min.
4. The method for regenerating the ternary lithium ion battery cathode material by the ion exchange method according to claim 1 or 3, is characterized in that: and (3) controlling the pH value of the system to be 4-4.5 by using ammonia water in the step (2).
5. The method for regenerating the ternary lithium ion battery cathode material by the ion exchange method according to claim 1, is characterized in that: the cation exchange resin in the step (3) is strong-acid cation exchange resin, and the stirring speed is 500-800 r/min.
6. The method for regenerating the ternary lithium ion battery cathode material by the ion exchange method according to claim 1, is characterized in that: the molar ratio of nickel, cobalt and manganese in the mixture A is (1-5) to (1-3) to (1-8).
7. The method for regenerating the ternary lithium ion battery cathode material by the ion exchange method according to claim 1, is characterized in that: and (4) introducing the air at a speed of 500-1000 ml/min, and raising the temperature at a constant speed with the microwave power of 1000-1500W.
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| CN103035977A (en) * | 2013-01-05 | 2013-04-10 | 深圳市泰力废旧电池回收技术有限公司 | Method for separating and recovering lithium from waste lithium ion battery |
| CN106785159A (en) * | 2016-11-18 | 2017-05-31 | 池州西恩新材料科技有限公司 | A kind of recovery method of nickel and cobalt containing anode material of lithium battery |
| CN107978816A (en) * | 2017-12-28 | 2018-05-01 | 中南大学 | Method for regenerating and repairing anode material of waste lithium ion battery |
| CN110527836A (en) * | 2019-09-12 | 2019-12-03 | 金川集团股份有限公司 | A kind of method that ion-exchange recycles valuable metal in waste and old nickel cobalt manganese lithium ion battery |
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| CN111697282B (en) * | 2020-06-18 | 2021-11-02 | 中国科学院宁波材料技术与工程研究所 | Method for extracting lithium from dilute solution recovered from waste battery positive electrode material |
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| CN103035977A (en) * | 2013-01-05 | 2013-04-10 | 深圳市泰力废旧电池回收技术有限公司 | Method for separating and recovering lithium from waste lithium ion battery |
| CN106785159A (en) * | 2016-11-18 | 2017-05-31 | 池州西恩新材料科技有限公司 | A kind of recovery method of nickel and cobalt containing anode material of lithium battery |
| CN107978816A (en) * | 2017-12-28 | 2018-05-01 | 中南大学 | Method for regenerating and repairing anode material of waste lithium ion battery |
| CN110527836A (en) * | 2019-09-12 | 2019-12-03 | 金川集团股份有限公司 | A kind of method that ion-exchange recycles valuable metal in waste and old nickel cobalt manganese lithium ion battery |
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