CN108134154B - Safe disassembly method for waste lithium ion battery - Google Patents
Safe disassembly method for waste lithium ion battery Download PDFInfo
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- CN108134154B CN108134154B CN201810031605.5A CN201810031605A CN108134154B CN 108134154 B CN108134154 B CN 108134154B CN 201810031605 A CN201810031605 A CN 201810031605A CN 108134154 B CN108134154 B CN 108134154B
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention discloses a safe disassembly method of waste lithium ion batteries, which comprises the following steps: discharging to a voltage below 0.6V before disassembly; the discharging method comprises the following steps: mixing a waste lithium ion battery into conductive powder, wherein the conductive powder comprises conductive mica powder, the granularity range of the conductive powder is 0.1-5 mu m, the resistivity is less than 100 omega-cm, the conductive powder also comprises an auxiliary discharge component, and the auxiliary discharge component is mixed powder comprising calcium carbonate and graphite. According to the invention, the conductive powder including the conductive mica powder is used as a discharge medium, under the condition that the waste lithium ion battery and the conductive powder are fully mixed, the waste lithium ion battery can be rapidly and efficiently discharged, the voltage of the waste lithium ion battery can be rapidly reduced to be below 0.6V, and the safety of the waste lithium ion battery in the subsequent disassembly process can be ensured.
Description
Technical Field
The invention belongs to the field of waste lithium ion battery recovery, and particularly relates to a safe disassembly method of a waste lithium ion battery.
Background
With the wide promotion of the application of lithium ion batteries in the field of power vehicles, the problem of recycling waste power lithium ion batteries is increasingly remarkable. With the prosperity of the new energy automobile market, the power lithium ion battery market also keeps a strong growth situation, and the problem of scrapping and processing a large number of power batteries is faced within 3-5 years in the future. Although with the expansion of the lithium ion battery market for electronic equipment, large-scale recycling enterprises have appeared.
At present, in the waste lithium ion battery recovery process, most enterprises are concentrated on recycling the positive and negative electrode plates and the active materials, and some enterprises also make corresponding researches on the recovery of the electrolyte, but only little attention is paid to the adaptive disassembly process in the recovery process. The first step after the waste lithium ion battery is recovered is disassembly, i.e. the lithium ion battery is disassembled into different components according to the components contained in the preparation process, typically, the lithium ion battery is disassembled into a shell, a positive plate, a negative plate and a diaphragm.
The disassembly of the waste lithium ion battery is not only realized by simply separating each component by external force, but also relates to how to separate each component without damage, and the safety of the whole disassembly process needs to be considered. The first step of the recovery processing of the waste lithium ion battery is to discharge the residual electric quantity in the battery safely and efficiently, and then subsequent processes such as disassembling and crushing can be carried out, otherwise, the battery is discharged in a large amount due to short circuit in the disassembling process, and even dangerous conditions such as explosion and the like can occur, so that accidents are caused. At present, two methods are mainly used for safe discharge of waste lithium ion batteries, one method is physical discharge, and the other method is mainly used for discharging electricity through an external load, namely, the battery is connected with a resistor, and the electric quantity in the battery is consumed through heat release, but the method is only a laboratory test and is not feasible for large-scale discharge; the other is chemical discharging, that is, the residual electricity in the battery is consumed in the solution through the electrolysis process by using the anode and cathode metals of the battery as the cathode and the anode, and at present, the slow discharging is mainly performed by using the aqueous solution containing salt as the electrolyte. However, the method has slow discharge rate, affects production efficiency, is easy to generate hydrogen, oxygen and the like in electrolyzed water, has potential safety hazard, and is difficult to treat used water due to pollution of organic electrolyte flowing out from a damaged old battery. The prior art does not provide any efficient and safe discharge process aiming at the disassembly process of the waste lithium ion battery.
Disclosure of Invention
in order to overcome the defects of the prior art, the invention provides a high-efficiency, safe, simple-operation and low-cost method for discharging the waste lithium ion battery. According to the invention, the conductive powder including the conductive mica powder is used as a discharge medium, under the condition that the waste lithium ion battery and the conductive powder are fully mixed, the waste lithium ion battery can be rapidly and efficiently discharged, the voltage of the waste lithium ion battery can be rapidly reduced to be below 0.6V, and the safety of the waste lithium ion battery in the subsequent disassembly process can be ensured.
The technical effect to be achieved by the invention is realized by the following scheme:
The invention provides a safe disassembly method of waste lithium ion batteries, which comprises the following steps:
Discharging the waste lithium ion battery until the voltage is lower than 0.6V before disassembling;
the discharging method comprises the following steps: mixing the waste lithium ion battery into conductive powder, wherein the conductive powder comprises conductive mica powder.
furthermore, the granularity range of the conductive powder is 0.1-5 mu m, and the resistivity is less than 100 omega cm.
Compared with the prior art that the battery is rapidly discharged by using the saline solution, the battery is rapidly discharged by using the conductive powder containing the conductive mica powder as a discharge medium. The conductive mica powder is in a scale shape, generally is grey white or light grey powder in appearance, is resistant to acid, alkali and organic solvents, has no oxidability, is stable at a temperature of below 800 ℃ and is flame retardant. The resistivity of the conductive mica powder is less than 100 omega cm, and the conductive mica powder can be used alone or mixed with other powder.
Further, the conductive powder also comprises an auxiliary discharge component, the auxiliary discharge component is mixed powder comprising calcium carbonate and graphite, and the preparation method comprises the following steps:
S01: mixing calcium carbonate and silicon dioxide aerogel in a mass ratio of 1: (0.2-0.3) adding the mixture into absolute ethyl alcohol, uniformly stirring, adjusting the pH to 8-9 by using ammonia water and the viscosity to 4-8cP, then adding a TEOS reagent with the mass of 3-5wt% of calcium carbonate, stirring and reacting for 8-12h, naturally cooling, filtering, washing a solid product until no residue is left on the surface, and finally drying;
S02: dispersing the solid product prepared in the S01 in absolute ethyl alcohol, and marking as a solution A; dispersing the graphite powder into absolute ethyl alcohol, adding 1-3% by mass of silane coupling agent, heating to 90-95 ℃, mechanically stirring and refluxing for 6-8h at constant temperature, naturally cooling, washing the solid product until no residue is left on the surface, and drying to obtain modified graphite powder B;
S03: and putting the powder B into the solution A, and carrying out wet grinding until the powder B is uniformly dispersed to finally obtain the required auxiliary discharge component.
The electric conductivity can be increased by mixing the conductive mica powder with the powder with better electric conductivity, and the electric conductivity can be reduced by mixing the conductive mica powder with the powder with poorer electric conductivity, so that the discharge rate of the waste battery in the powder can be adjusted, and safe and efficient discharge is realized. Because the surface energy of the conductive mica powder is low, the adhesion performance of the conductive mica powder to the surface of the battery is general in the discharging process of the battery, and in order to improve the contact performance of the conductive powder and the battery (the poor contact can cause the slowing of the discharging process), the conductive powder in the invention is added with an auxiliary discharging component besides the conductive mica powder, and the auxiliary discharging component mainly comprises modified powder of calcium carbonate and graphite.
According to the invention, the surface of calcium carbonate is coated with a layer of silica aerogel by using a modification method, and then the sub-graphite powder with good conductivity and adhesiveness and the calcium carbonate powder form a uniform mixture by using the pores and the adsorption performance of the silica aerogel. On one hand, the calcium carbonate powder has good mixing performance and high bulk density, can effectively improve the contact performance between the conductive powder and the battery when being used in cooperation with the conductive mica powder, has low price and easily obtained raw materials, and is beneficial to reducing the discharge cost. On the other hand, the addition of the sub-graphite powder improves the conductivity of the calcium carbonate powder, so that the discharge process of the battery is not influenced by the addition of the auxiliary discharge component.
The excellent electric conductivity of the conductive mica powder ensures that the electron transmission efficiency is high, the discharge efficiency is greatly improved, and the potential safety hazard is reduced due to the excellent flame retardant property of the conductive mica powder and the auxiliary discharge components. The chemical stability of the conductive powder enables the conductive powder to be repeatedly utilized after use, so that the discharging process has both economical efficiency and environmental protection. The integrity of the battery can be kept after the waste lithium ion battery is discharged, and the waste lithium ion battery with good integrity can be obtained after the filtering sieve, so that the subsequent disassembly is convenient. According to the technical scheme, the waste lithium ion batteries are discharged safely and efficiently, and the adverse factors that hydrogen and oxygen are easily generated by discharging in an aqueous solution and a large amount of heat is released to cause water boiling, easy explosion and the like are avoided.
Further, in S01, the reaction temperature was 40 to 55 ℃. The reaction temperature should be slightly higher than room temperature, but should not be too high, which affects the coating uniformity of the silica aerogel.
further, in S01, the drying temperature is 80-90 ℃, and the drying time is 8-12 h.
Further, in S01, the porosity of the silica aerogel is 88-95%, the specific surface area is 550-600 square meters per gram, and the pore size is 100-200 nm. The porosity, specific surface area and pore size of the silica aerogel determine the mixing performance between the calcium carbonate powder and the sub-graphite powder.
Further, in S02, the addition amount of absolute ethyl alcohol in the solution A is such that the S01 solid product and the modified graphite powder B can be immersed; the addition amount of the absolute ethyl alcohol in the preparation process of the modified graphite powder B is 20-30 times of the volume of the graphite powder.
Further, in S02, the ratio of the mass of the graphite powder to the mass of the solid product in S01 was (1.2-1.3): 1.
Further, in S03, in order to improve the dispersion efficiency, the wet milling apparatus is a planetary ball mill.
Further, preferably, the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and auxiliary discharge components in a mass ratio (1.5-2): 1 are mixed and ground to a particle size range of 0.1-5 μm. The proportion of the conductive mica powder and the auxiliary discharge component needs to be controlled moderately, the cost is increased and the contact performance of the conductive powder and the battery is influenced when the amount of the conductive mica powder is too much, and the discharge speed of the battery is influenced when the amount of the auxiliary discharge component is too much. The particle size range of the conductive powder also directly influences the discharge speed of the battery and the difficulty of sieving the battery after the battery is discharged.
The invention has the following advantages:
The invention provides a discharge method of waste lithium ion batteries, which is efficient, safe, simple to operate and low in cost. According to the invention, the conductive powder including the conductive mica powder is used as a discharge medium, under the condition that the waste lithium ion battery and the conductive powder are fully mixed, the waste lithium ion battery can be rapidly and efficiently discharged, the voltage of the waste lithium ion battery can be rapidly reduced to be below 0.6V, and the safety of the waste lithium ion battery in the subsequent disassembly process can be ensured.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
The preparation method of the auxiliary discharge component comprises the following specific steps:
S01: mixing calcium carbonate and silicon dioxide aerogel in a mass ratio of 1: 0.2 is added into absolute ethyl alcohol, the pH value is adjusted to 8-9 by ammonia water after the mixture is evenly stirred, the viscosity is 5.26cP, then TEOS reagent with the calcium carbonate mass of 3wt% is added, the mixture is stirred and reacts for 8 hours (the reaction temperature is 45 ℃) and then is naturally cooled, the solid product is washed after the filtration until no residue is left on the surface, and finally the solid product is dried for 12 hours at the temperature of 80 ℃.
The silica aerogel used in the step has the porosity of 92 percent, the specific surface area of 584 square meters per gram and the average size of holes of 155 nm.
S02: dispersing the solid product prepared in the S01 in absolute ethyl alcohol, and marking as a solution A; and (2) dispersing the graphite powder into absolute ethyl alcohol, adding 1% by mass of silane coupling agent, heating to 90 ℃, mechanically stirring and refluxing for 8 hours at a constant temperature, naturally cooling, washing the solid product until no residue is left on the surface, and drying to obtain modified graphite powder B.
The addition amount of the absolute ethyl alcohol in the solution A is that the S01 solid product and the modified graphite powder B can be immersed; the addition amount of the absolute ethyl alcohol in the preparation process of the modified graphite powder B is 20 times of the volume of the graphite powder. The ratio of the mass of the graphite powder to the mass of the solid product in S01 was 1.2: 1.
s03: and putting the powder B into the solution A, and carrying out wet grinding by using a planetary ball mill until the powder B is uniformly dispersed to finally obtain the required auxiliary discharge component.
Preparing conductive powder:
Mixing conductive mica powder and the auxiliary discharge component prepared in the above step in a mass ratio of 1.5: 1 were mixed and ground to an average particle size of 1 μm.
Example 2
Other conditions of this example are the same as those of example 1, except that: preparation of auxiliary discharge components in step S01, calcium carbonate and silica aerogel are mixed in a mass ratio of 1: 0.22 to absolute ethanol.
Example 3
other conditions of this example are the same as those of example 1, except that: preparation of auxiliary discharge components in step S01, calcium carbonate and silica aerogel are mixed in a mass ratio of 1: 0.25 to absolute ethanol.
example 4
Other conditions of this example are the same as those of example 1, except that: preparation of auxiliary discharge components in step S01, calcium carbonate and silica aerogel are mixed in a mass ratio of 1: 0.28 to absolute ethanol.
example 5
other conditions of this example are the same as those of example 1, except that: preparation of auxiliary discharge components in step S01, calcium carbonate and silica aerogel are mixed in a mass ratio of 1: 0.30 to absolute ethanol.
Example 6
Other conditions of this example are the same as those of example 1, except that: in the specific step S02 of preparing the auxiliary discharge component, the amount of absolute ethanol added during the preparation of the modified graphite powder B is 30 times the volume of the graphite powder B.
Example 7
Other conditions of this example are the same as those of example 1, except that: in the preparation of the auxiliary discharge component, in step S02, the ratio of the mass of the graphite powder to the mass of the solid product in step S01 was 1.25: 1.
Example 8
Other conditions of this example are the same as those of example 1, except that: in the preparation of the auxiliary discharge component, in step S02, the ratio of the mass of the graphite powder to the mass of the solid product in step S01 was 1.3: 1.
Example 9
other conditions of this example are the same as those of example 1, except that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and an auxiliary discharge component in a mass ratio of 1.6: 1 are mixed and ground to an average particle size of 1 μm.
Example 10
other conditions of this example are the same as those of example 1, except that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and an auxiliary discharge component in a mass ratio of 1.8: 1 are mixed and ground to an average particle size of 1 μm.
Example 11
Other conditions of this example are the same as those of example 1, except that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and auxiliary discharge components in a mass ratio of 2:1 are mixed and ground to an average particle size of 1 μm.
Example 12
other conditions of this example are the same as those of example 1, except that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and the auxiliary discharge component prepared in the above step in a mass ratio of 1.5: 1 were mixed and ground to an average particle size of 0.1. mu.m.
Example 13
Other conditions of this example are the same as those of example 1, except that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and the auxiliary discharge component prepared in the above step in a mass ratio of 1.5: 1 were mixed and ground to an average particle size of 2 μm.
Example 14
Other conditions of this example are the same as those of example 1, except that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and the auxiliary discharge component prepared in the above step in a mass ratio of 1.5: 1 were mixed and ground to an average particle size of 5 μm.
The electrical resistivity of the conductive powder prepared in examples 1 to 14 was tested, and meanwhile, the waste lithium ion battery was mixed into the conductive powder and discharged until the voltage was less than 0.6V, and then disassembled. The positive current collector and the negative current collector of the waste lithium ion battery used in the embodiment are aluminum foils and copper foils respectively, active substances are coated on the positive surface and the negative surface of the positive current collector aluminum foil and the negative current collector copper foil, the diaphragm is Celgard 2500, and the electrolyte component is 1MLiPF6Dissolved in an organic solution of ethylene carbonate, diethyl carbonate =1:1 (volume ratio).
The conductive powder resistivity test results are as follows:
The discharging speed of the method in the embodiment is improved by more than 60% compared with the discharging speed of the traditional salt solution, the electron transmission efficiency is high due to the excellent conductivity of the conductive powder, the discharging efficiency is greatly improved, the potential safety hazard is reduced due to the excellent flame retardant property of the conductive powder, and the conductive powder can be recycled due to the chemical stability of the conductive powder. The integrity of the battery can be kept after the waste lithium ion battery is discharged, and the waste lithium ion battery with good integrity can be obtained after the filtering sieve, so that the subsequent disassembly is convenient.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the embodiments of the present invention and not for limiting the same, and although the embodiments of the present invention are described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the embodiments of the present invention, and these modifications or equivalent substitutions cannot make the modified technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A safe disassembly method of waste lithium ion batteries is characterized in that:
Discharging the waste lithium ion battery until the voltage is lower than 0.6V before disassembling;
The discharging method comprises the following steps: mixing a waste lithium ion battery into conductive powder, wherein the conductive powder comprises conductive mica powder;
The conductive powder also comprises an auxiliary discharge component, the auxiliary discharge component is mixed powder comprising calcium carbonate and graphite, and the preparation method comprises the following steps:
S01: mixing calcium carbonate and silicon dioxide aerogel in a mass ratio of 1: (0.2-0.3) adding the mixture into absolute ethyl alcohol, uniformly stirring, adjusting the pH to 8-9 by using ammonia water and the viscosity to 4-8cP, then adding a TEOS reagent with the mass of 3-5wt% of calcium carbonate, stirring and reacting for 8-12h, naturally cooling, filtering, washing a solid product until no residue is left on the surface, and finally drying;
S02: dispersing the solid product prepared in the S01 in absolute ethyl alcohol, and marking as a solution A; dispersing the graphite powder into absolute ethyl alcohol, adding 1-3% by mass of silane coupling agent, heating to 90-95 ℃, mechanically stirring and refluxing for 6-8h at constant temperature, naturally cooling, washing the solid product until no residue is left on the surface, and drying to obtain modified graphite powder B;
s03: and putting the powder B into the solution A, and carrying out wet grinding until the powder B is uniformly dispersed to finally obtain the required auxiliary discharge component.
2. the safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: the granularity range of the conductive powder is 0.1-5 mu m, and the resistivity is less than 100 omega cm.
3. The safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: in S01, the reaction temperature is 40-55 ℃.
4. the safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: in S01, the drying temperature is 80-90 ℃, and the drying time is 8-12 h.
5. The safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: in S01, the silica aerogel adopted has a porosity of 88-95%, a specific surface area of 550-200 nm and a pore size of 100-200nm, and is used for treating 600 square meters per gram.
6. The safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: in the S02, the addition amount of the absolute ethyl alcohol in the solution A is that the S01 solid product and the modified graphite powder B can be immersed; the addition amount of the absolute ethyl alcohol in the preparation process of the modified graphite powder B is 20-30 times of the volume of the graphite powder.
7. The safe disassembly method of the waste lithium ion battery as claimed in claim 3, characterized in that: in S02, the ratio of the mass of the graphite powder to the mass of the solid product in S01 is (1.2-1.3): 1.
8. The safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: in S03, the wet grinding equipment is a planetary ball mill.
9. The safe disassembly method of the waste lithium ion battery as claimed in claim 1, characterized in that: the preparation method of the conductive powder comprises the following steps: mixing conductive mica powder and auxiliary discharge components in a mass ratio (1.5-2): 1 are mixed and ground to a particle size range of 0.1-5 μm.
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| CN109004308B (en) * | 2018-08-27 | 2020-06-12 | 惠州亿纬锂能股份有限公司 | Waste lithium ion battery discharging method |
| US11121418B2 (en) * | 2019-12-31 | 2021-09-14 | Omega Harvested Metallurgical, Inc. | Coke powder as a discharging agent for waste battery recycling and method thereof |
| CN111370794A (en) * | 2020-03-19 | 2020-07-03 | 河南小威环境科技有限公司 | Method for releasing electric quantity of lithium ion battery |
| CN112201872B (en) * | 2020-10-22 | 2021-12-21 | 中国科学院宁波材料技术与工程研究所 | Safe discharge method and wet physical sorting method for retired batteries |
| CN112687974B (en) * | 2021-03-16 | 2021-06-18 | 嘉兴模度新能源有限公司 | Chemical disassembling method applied to battery adhesive module |
| CN114335768A (en) * | 2021-11-23 | 2022-04-12 | 深圳供电局有限公司 | Waste lithium iron phosphate battery discharging device, discharging method and application |
| CN115084700A (en) * | 2022-06-27 | 2022-09-20 | 中南大学 | Thermosensitive discharge particles and safe discharge method of waste lithium ion battery |
| CN116706287B (en) * | 2023-08-08 | 2024-01-12 | 宁德时代新能源科技股份有限公司 | Battery capacity sorting device and sorting method |
| CN116885329B (en) * | 2023-09-07 | 2023-12-29 | 深圳市杰成镍钴新能源科技有限公司 | Battery discharging device and battery discharging control method |
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| CN106816663B (en) * | 2017-02-24 | 2020-09-08 | 中南大学 | Method for efficiently and safely discharging waste lithium ion batteries |
| CN106834703B (en) * | 2017-03-30 | 2019-04-26 | 中南大学 | A kind of leaching method of waste lithium ion cell anode active material |
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