CN112670614B - Physical sorting method for positive and negative electrode materials of waste lithium iron phosphate batteries - Google Patents
Physical sorting method for positive and negative electrode materials of waste lithium iron phosphate batteries Download PDFInfo
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention relates to the technical field of recycling of waste power lithium ion batteries, and particularly discloses a physical sorting method of positive and negative electrode materials of waste lithium iron phosphate batteries. According to the method, firstly, the mixed material of the positive electrode and the negative electrode of the lithium iron phosphate battery is pyrolyzed, so that the organic matters are removed, physical separation becomes possible, the adhesion between the positive electrode material and graphite is eliminated through the scrubbing action of a rod mill, and favorable conditions are created for recovering the graphite step by step through subsequent flotation and magnetic separation. The method has the advantages of cleanness, high efficiency, high product purity, simple operation, easy industrialization and the like, realizes the effective separation of the positive and negative mixed electrode powder, and improves the utilization rate of resources.
Description
Technical Field
The invention relates to the technical field of recycling of waste power lithium ion batteries, in particular to a physical sorting method of positive and negative electrode materials of waste lithium iron phosphate batteries.
Background
In recent years, lithium ion power batteries are widely applied in the field of new energy automobiles, and the lithium ion power batteries are about to enter a batch scrapping stage. Because the waste lithium ion battery has the characteristics of harmfulness and resource, the increasingly serious resource circulation problem and the environmental pollution problem are gradually caused. The resource and harmless treatment of the waste lithium battery becomes a hotspot of research in the field of resources and environment.
The waste power battery is recycled by performing pretreatment such as disassembly, discharge, crushing, screening, magnetic separation and the like on the waste power battery to obtain a plastic shell, a diaphragm, copper foil, aluminum foil and anode-cathode mixed electrode powder (mainly comprising an anode material, a cathode material and a binder). The anode material of the lithium ion power battery is mainly ternary material and lithium iron phosphate, the ternary material is rich in high-value metals such as lithium, cobalt, nickel and the like and is recycled, but the lithium iron phosphate has low metal value, the traditional chemical and metallurgical processes have the defects of high energy consumption, high cost, easy generation of secondary pollution and the like, and the poor economic benefit of disposal becomes a main problem which hinders the recycling of the lithium iron power battery. Therefore, the method for separating the lithium iron phosphate anode and cathode materials, which is green, environment-friendly, simple, efficient and good in sorting index, has important significance.
Disclosure of Invention
The invention mainly solves the technical problem of providing a physical sorting method for positive and negative electrode materials of waste lithium iron phosphate batteries, and provides a physical sorting method capable of cleanly and efficiently separating positive electrode powder and negative electrode powder aiming at the current situations that the chemical separation and disposal cost of the positive and negative electrode materials of the existing waste lithium iron phosphate batteries is high, the secondary pollution is serious, and graphite is not effectively recovered.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A physical sorting method of positive and negative electrode materials of waste lithium iron phosphate batteries comprises the following steps:
s1: pyrolysis of volatile organic compounds
Putting the mixed material of the positive electrode and the negative electrode of the waste lithium iron phosphate battery into a pyrolysis furnace, heating and pyrolyzing the mixed material at 350-450 ℃ in an inert atmosphere or under a low-pressure condition for 1.5-2 h, and condensing and collecting to obtain a pyrolyzed electrode material;
s2: rod mill dissociation
Adding water into the pyrolyzed electrode material to prepare slurry with the mass percentage concentration of 65-70%, and placing the slurry into a rod mill for rod milling treatment;
s3: flotation column separation graphite
Introducing the slurry subjected to rod milling in the step S2 into a stirring barrel, adding water to prepare the slurry with the mass percentage concentration of 10-15%, adding a regulator, an inhibitor and a foaming agent into the slurry, stirring, and then performing flotation in a flotation column to obtain flotation foam and flotation tailings;
s4: high-gradient magnetic separation graphite
Carrying out magnetic separation on the flotation tailings in the step S3 by using a high-gradient magnetic separator to obtain a magnetic product and a non-magnetic product; then, carrying out filter pressing on the magnetic product to obtain a positive electrode material of the lithium iron phosphate battery; and (4) merging the non-magnetic product and the flotation foam in the step (S3) and performing filter pressing to obtain a negative electrode material mainly comprising graphite.
In a preferred embodiment of the present invention, in step S2, the filling rate of the rod mill is 30-35%, the rotation speed is 60-65% of the critical speed of the rod mill, the rotation speed is generally 30-40 r/min, and the rod milling time is 10-20 min.
As a preferred embodiment of the present invention, in step S3, the adjusting agent is water glass, and the amount of the adjusting agent is 1000 to 1500g per ton of the mixed material of the positive electrode and the negative electrode of the waste lithium iron phosphate battery.
The inhibitor is a mixed medicament formed by carboxymethyl cellulose (CMC) or tannin and sodium hexametaphosphate, and the dosage of the inhibitor is 500-800 g added to each ton of mixed material of positive and negative electrodes of the waste lithium iron phosphate battery.
The foaming agent is methyl isobutyl carbinol (MIBC) or terpineol, and the dosage of the foaming agent is 10-20 g of the mixed material of the positive electrode and the negative electrode of each ton of the waste lithium iron phosphate batteries.
In a preferred embodiment of the present invention, the inhibitor is a mixed agent of carboxymethyl cellulose and sodium hexametaphosphate or a mixed agent of tannin and sodium hexametaphosphate.
Preferably, the mass ratio of the carboxymethyl cellulose to the sodium hexametaphosphate is 1 (4-6), and more preferably 1.
Preferably, the mass ratio of the tannin to the sodium hexametaphosphate is 1 (3-6), and more preferably 1.
As a preferred embodiment of the present invention, in step S3, the flotation includes primary flotation roughing and primary flotation concentrating.
In a preferred embodiment of the present invention, in step S3, the aeration rate of the flotation column is 0.10-0.20 m 3 /(min.m 2 )。
In a preferred embodiment of the present invention, in step S4, the background field strength of the high gradient magnetic separator is 0.4 to 0.8T, and the pulse size is 100 to 200 times/min.
The invention provides a physical sorting method of positive and negative electrode materials of waste lithium iron phosphate batteries, which is research and development designed aiming at the separation of positive and negative electrode mixtures of the lithium iron phosphate batteries. Through the pyrolysis of the positive and negative electrode material powder, organic impurities (mainly binder) on the particle surface are removed, and the graphite particle surface has hydrophobicity again, so that favorable conditions are created for the physical separation of graphite and positive electrode materials. And then, the characteristics of uniform grinding material products and reduction of over crushing of the rod mill are utilized to perform rod milling dissociation on the electrode powder, so that the adhesion effect between the positive electrode material and graphite is eliminated, the dissociation of the graphite and the positive electrode material is promoted, and the flotation separation and the magnetic separation are possible. The flotation environment of slurry is improved through the regulator and the inhibitor, the floatability difference between graphite and a positive electrode material is enlarged, flotation is carried out by utilizing a flotation column with better fine-fraction flotation separation effect under the condition of not adding a collecting agent, the flotation and easy-to-float graphite pre-separation are realized, and the influence of the flotation column on the subsequent magnetic separation is avoided. The subsequent high-gradient magnetic separation utilizes the characteristic that the positive electrode material has weak magnetism and graphite is non-magnetic, and further realizes the high-efficiency separation of the graphite and the positive electrode material through strong magnetic separation. By adopting the method, the purity of the obtained positive electrode material lithium iron phosphate is more than 95 percent, the graphite content is less than 3 percent, the recovery rate of the lithium iron phosphate is more than 92 percent, the graphite grade of the obtained negative electrode material is more than 85 percent, and the recovery rate of the graphite is more than 92 percent.
The invention provides a physical separation method of positive and negative electrode materials of waste lithium iron phosphate batteries, which is designed mainly for solving the problems of high cost, serious secondary pollution and the like of the existing chemical separation treatment of the positive and negative electrode materials. According to the invention, the mixed material of the positive electrode and the negative electrode of the lithium iron phosphate battery is pyrolyzed, so that physical separation is possible while organic matters are removed, the adhesion between the positive electrode material and graphite is eliminated through the scrubbing action of the rod mill, and favorable conditions are created for recovering the graphite step by step through subsequent flotation and magnetic separation. The method has the advantages of cleanness, high efficiency, high product purity, simple operation, easy industrialization and the like, realizes the effective separation of the positive and negative mixed electrode powder, and improves the utilization rate of resources.
Drawings
Fig. 1 is a process flow chart of the physical sorting method of the positive and negative electrode materials of the waste lithium iron phosphate battery provided by the invention.
Detailed Description
The technical solution of the present invention will be described in detail by specific examples.
In the following examples, the drugs used are all commercially available products unless otherwise specified. The concentrations or contents in each example are mass percentages.
Example 1
The physical sorting and recovering method for the positive and negative electrode materials of the waste lithium iron phosphate batteries of the embodiment is shown in a process flow chart of fig. 1. Sorting the anode and cathode mixtures of a certain lithium iron phosphate battery of Guangdong Shenzhen, which is carried out according to the following steps:
(1) And (3) placing the mixture of the positive electrode and the negative electrode of the waste lithium iron phosphate battery in a pyrolysis furnace, heating for 1.8h at the temperature of 400 ℃ under the inert atmosphere, and condensing and collecting to obtain pyrolyzed electrode powder.
(2) Adding water into the pyrolyzed electrode powder to prepare slurry with the mass percent concentration of 70%, and placing the slurry into a rod mill, wherein the filling rate of the rod mill is adjusted to be 32%, the rotating speed of the rod mill is 35r/min, and the rod milling time is 18min.
(3) Introducing the slurry after rod milling into a stirring barrel, adding water to prepare the slurry with the mass percentage concentration of 12%, and sequentially adding a water glass regulator, a combined inhibitor of CMC and sodium hexametaphosphate, and an MIBC foaming agent into the slurry, wherein the mass ratio of the regulator to the CMC to the sodium hexametaphosphate is 1. After stirring for 5min, the aeration rate of the flotation column is adjusted to 0.12m 3 /(min.m 2 ) And performing flotation roughing 1 time and flotation fine selection 1 time to obtain flotation foam and flotation tailings.
(4) Adjusting the background field intensity of the magnetic separator to be 0.6T, and the pulse size to be 120 times/min, performing high-gradient magnetic separation on the flotation tailings obtained in the step (3) to obtain a magnetic product and a non-magnetic product, and performing filter pressing on the magnetic product to obtain a lithium iron phosphate battery positive electrode material; and (4) combining the nonmagnetic product with the flotation foam in the step (3) and then performing pressure filtration to obtain a negative electrode material graphite.
The purity of the positive electrode material lithium iron phosphate obtained in the step (4) is 96.45%, the graphite content is 1.12%, the recovery rate of the lithium iron phosphate is 94.61%, the graphite grade of the obtained negative electrode powder is 86.12%, and the recovery rate of the graphite is 93.45%.
Example 2
The physical sorting and recovering method for the positive and negative electrode materials of the waste lithium iron phosphate batteries of the embodiment is shown in a process flow chart of fig. 1. Sorting the positive and negative electrode mixture of a certain lithium iron phosphate battery in Guangdong Jiangmen according to the following steps:
(1) And (3) placing the mixture of the positive electrode and the negative electrode of the waste lithium iron phosphate battery in a pyrolysis furnace, heating for 2.0 hours at the temperature of 350 ℃ under the inert atmosphere condition, and condensing and collecting to obtain pyrolyzed electrode powder.
(2) Adding water into the pyrolyzed electrode powder to prepare slurry with the mass percent concentration of 65%, and placing the slurry into a rod mill, wherein the filling rate of the rod mill is adjusted to be 30%, the rotating speed of the rod mill is 32r/min, and the rod milling time is 15min.
(3) Introducing the slurry after rod milling into a stirring barrel, adding water to prepare the slurry with the mass percentage concentration of 15%, and sequentially adding a water glass regulator, a combined inhibitor of CMC and sodium hexametaphosphate in a mass ratio of 1. After stirring for 5min, the aeration rate of the flotation column is adjusted to 0.12m 3 /(min.m 2 ) And performing flotation roughing 1 time and flotation fine selection 1 time to obtain flotation foam and flotation tailings.
(4) Adjusting the background field intensity of the magnetic separator to be 0.5T, and the pulse size to be 125 times/min, performing high-gradient magnetic separation on the flotation tailings obtained in the step (3) to obtain a magnetic product and a non-magnetic product, and performing filter pressing on the magnetic product to obtain a lithium iron phosphate battery positive electrode material; and (4) combining the nonmagnetic product with the flotation foam in the step (3) and then performing pressure filtration to obtain a negative electrode material graphite.
The purity of the positive electrode material lithium iron phosphate obtained in the step (4) is 95.72%, the graphite content is 1.68%, the recovery rate of the lithium iron phosphate is 95.72%, the graphite grade of the obtained negative electrode powder is 85.31%, and the recovery rate of the graphite is 94.21%.
Example 3
The physical sorting and recovering method for the positive and negative electrode materials of the waste lithium iron phosphate batteries of the embodiment is shown in a process flow chart of fig. 1. Sorting the positive and negative electrode mixtures of a certain lithium iron phosphate battery in Guangdong Dongguan, and performing the following steps:
(1) And (3) placing the mixture of the positive electrode and the negative electrode of the waste lithium iron phosphate battery in a pyrolysis furnace, heating for 1.5h at the temperature of 450 ℃ under the inert atmosphere, and condensing and collecting to obtain pyrolyzed electrode powder.
(2) Adding water into the pyrolyzed electrode powder to prepare slurry with the mass percent concentration of 70%, placing the slurry into a rod mill, adjusting the filling rate of the rod mill to be 35%, the rotating speed of the rod mill to be 30r/min, and the rod milling time to be 12min.
(3) Introducing the ground slurry into a stirring barrel, adding water to prepare the productThe method comprises the following steps of adding a water glass regulator, a combined inhibitor of tannin and sodium hexametaphosphate in a mass ratio of 1 to 5 and an MIBC foaming agent into slurry with a percentage concentration of 10%, wherein the dosages of the regulator, the inhibitor and the foaming agent are respectively 1500g, 500g and 10g added to each ton of waste lithium iron phosphate battery positive and negative electrode mixture. After stirring for 5min, the aeration rate of the flotation column is adjusted to 0.20m 3 /(min.m 2 ) And performing 1-time rough flotation and 1-time fine flotation to obtain flotation froth and flotation tailings.
(4) Adjusting the background field intensity of the magnetic separator to be 0.8T, and the pulse size to be 100 times/min, performing high-gradient magnetic separation on the flotation tailings obtained in the step (3) to obtain a magnetic product and a non-magnetic product, and performing filter pressing on the magnetic product to obtain a lithium iron phosphate battery positive electrode material; and (4) combining the nonmagnetic product with the flotation foam in the step (3) and then performing pressure filtration to obtain a negative electrode material graphite.
The purity of the positive electrode material lithium iron phosphate obtained in the step (4) is 95.37%, the graphite content is 2.01%, the recovery rate of the lithium iron phosphate is 95.37%, the graphite grade of the obtained negative electrode powder is 86.31%, and the recovery rate of the graphite is 95.83%.
Example 4
The process flow chart of the physical separation and recovery method of the positive and negative electrode materials of the waste lithium iron phosphate batteries is shown in fig. 1. The method comprises the following steps of sorting a positive-negative electrode mixture of a certain lithium iron phosphate battery in Guangdong Guangzhou:
(1) And (3) placing the mixture of the positive electrode and the negative electrode of the waste lithium iron phosphate battery in a pyrolysis furnace, heating for 1.6h at the temperature of 380 ℃ under the inert atmosphere, and condensing and collecting to obtain pyrolyzed electrode powder.
(2) Adding water into the pyrolyzed electrode powder to prepare slurry with the mass percent concentration of 68%, and placing the slurry into a rod mill, wherein the filling rate of the rod mill is adjusted to be 32%, the rotating speed of the rod mill is 40r/min, and the rod milling time is 15min.
(3) Introducing the slurry after rod milling into a stirring barrel, adding water to prepare the slurry with the mass percentage concentration of 15%, sequentially adding a water glass regulator, a combined inhibitor of CMC and sodium hexametaphosphate with the mass ratio of 1 and an MIBC foaming agent into the slurry,the dosage of the regulator, the inhibitor and the foaming agent is respectively 1000g, 800g and 10g added to each ton of waste lithium iron phosphate battery positive and negative electrode mixture. After stirring for 5min, the aeration rate of the flotation column is adjusted to 0.15m 3 /(min.m 2 ) And performing flotation roughing 1 time and flotation fine selection 1 time to obtain flotation foam and flotation tailings.
(4) Adjusting the background field intensity of the magnetic separator to be 0.6T, and the pulse size to be 200 times/min, carrying out high-gradient magnetic separation on the flotation tailings obtained in the step (3) to obtain a magnetic product and a non-magnetic product, and carrying out filter pressing on the magnetic product to obtain a lithium iron phosphate battery positive electrode material; and (4) combining the nonmagnetic product with the flotation foam in the step (3) and then performing pressure filtration to obtain a negative electrode material graphite.
The purity of the positive electrode material lithium iron phosphate obtained in the step (4) is 96.53%, the graphite content is 1.09%, the recovery rate of the lithium iron phosphate is 95.12%, the graphite grade of the obtained negative electrode powder is 85.67%, and the recovery rate of the graphite is 96.42%.
Example 5
The physical sorting and recovering method for the positive and negative electrode materials of the waste lithium iron phosphate batteries of the embodiment is shown in a process flow chart of fig. 1. Sorting the anode and cathode mixtures of a certain lithium iron phosphate battery of Guangdong Shenzhen, which is carried out according to the following steps:
(1) And (3) placing the mixture of the positive electrode and the negative electrode of the waste lithium iron phosphate battery in a pyrolysis furnace, heating for 1.5h at the temperature of 400 ℃ under the inert atmosphere, and condensing and collecting to obtain pyrolyzed electrode powder.
(2) Adding water into the pyrolyzed electrode powder to prepare slurry with the mass percentage concentration of 65%, placing the slurry into a rod mill, adjusting the filling rate of the rod mill to be 35%, the rotating speed of the rod mill to be 35r/min, and the rod milling time to be 10min.
(3) Introducing the slurry after rod milling into a stirring barrel, adding water to prepare the slurry with the mass percentage concentration of 12%, and sequentially adding a water glass regulator, a combined inhibitor of CMC and sodium hexametaphosphate in a mass ratio of 1. Stirring for 5min, and regulating buoyancyThe aeration quantity of the selected column is 0.17m 3 /(min.m 2 ) And performing flotation roughing 1 time and flotation fine selection 1 time to obtain flotation foam and flotation tailings.
(4) Adjusting the background field intensity of the magnetic separator to be 0.4T, and the pulse size to be 160 times/min, carrying out high-gradient magnetic separation on the flotation tailings obtained in the step (3) to obtain a magnetic product and a non-magnetic product, and carrying out filter pressing on the magnetic product to obtain a lithium iron phosphate battery positive electrode material; and (4) combining the nonmagnetic product with the flotation foam in the step (3) and then performing pressure filtration to obtain a negative electrode material graphite.
The purity of the positive electrode material lithium iron phosphate obtained in the step (4) is 95.17%, the graphite content is 2.35%, the recovery rate of the lithium iron phosphate is 96.73%, the graphite grade of the obtained negative electrode powder is 87.67%, and the recovery rate of the graphite is 97.67%.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can 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 (7)
1. A physical separation method for positive and negative electrode materials of waste lithium iron phosphate batteries is characterized by comprising the following steps:
s1: pyrolysis of volatile organic compounds
Placing the mixed material of the positive electrode and the negative electrode of the waste lithium iron phosphate battery in a pyrolysis furnace, heating and pyrolyzing the mixed material at 350-450 ℃ in an inert atmosphere, and condensing and collecting to obtain a pyrolyzed electrode material;
s2: bar mill dissociation
Adding water into the pyrolyzed electrode material to prepare slurry with the mass percentage concentration of 65-70%, and placing the slurry into a rod mill for rod milling treatment;
s3: flotation column separation graphite
Introducing the slurry subjected to rod milling in the step S2 into a stirring barrel, adding water to prepare the slurry with the mass percentage concentration of 10-15%, adding a regulator, an inhibitor and a foaming agent into the slurry, and then performing flotation in a flotation column to obtain flotation foam and flotation tailings; the regulator is water glass, and the dosage of the regulator is 1000-1500 g of the regulator added to each ton of the mixed material of the positive electrode and the negative electrode of the waste lithium iron phosphate battery; the inhibitor is a mixed medicament formed by carboxymethyl cellulose or tannin and sodium hexametaphosphate, and the dosage of the inhibitor is 500-800 g added to each ton of mixed material of positive and negative electrodes of the waste lithium iron phosphate battery; the foaming agent is methyl isobutyl carbinol or terpineol oil, and the dosage of the foaming agent is 10-20 g of the mixed material of the positive electrode and the negative electrode of each ton of waste lithium iron phosphate batteries;
s4: high-gradient magnetic separation graphite
Carrying out magnetic separation on the flotation tailings in the step S3 by using a high-gradient magnetic separator to obtain a magnetic product and a non-magnetic product; then, carrying out filter pressing on the magnetic product to obtain a positive electrode material of the lithium iron phosphate battery; and combining the non-magnetic product with the flotation foam in the step S3, and performing filter pressing to obtain the negative electrode material.
2. The physical sorting method according to claim 1, wherein the filling rate of the rod mill in step S2 is 30 to 35% and the rotation speed is 30 to 40r/min.
3. The physical sorting method according to claim 1, wherein the inhibitor is a mixed medicament of carboxymethylcellulose and sodium hexametaphosphate or a mixed medicament of tannin and sodium hexametaphosphate, and the mass ratio of the carboxymethylcellulose to the sodium hexametaphosphate is 1 (4-6); the mass ratio of the tannin to the sodium hexametaphosphate is 1 (3-6).
4. The physical sorting method according to claim 2 or 3, wherein in step S3, the flotation comprises primary flotation rougher flotation and primary flotation cleaner flotation.
5. The physical separation method of claim 4, wherein the aeration amount in the flotation column flotation in the step S3 is 0.10-0.20 m 3 /(min.m 2 )。
6. The physical sorting method of claim 1, wherein in step S4, the background field strength of the high gradient magnetic separator is 0.4-0.8T, and the pulse size is 100-200 times/min.
7. The physical sorting method according to claim 1, wherein the purity of the lithium iron phosphate of the positive electrode material obtained in step S4 is more than 95%, the graphite content is less than 3%, and the recovery rate of the lithium iron phosphate is more than 92%; and/or the obtained cathode material has a graphite grade of more than 85 percent and a graphite recovery rate of more than 92 percent.
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