Method for preparing pretreated product for recovering valuable metals of lithium secondary battery
US-2023420761-A1 · Dec 28, 2023 · US
US11920213B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11920213-B2 |
| Application number | US-202118246671-A |
| Country | US |
| Kind code | B2 |
| Filing date | Apr 30, 2021 |
| Priority date | Oct 29, 2020 |
| Publication date | Mar 5, 2024 |
| Grant date | Mar 5, 2024 |
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Disclosed is an incomplete extraction method for recycling batteries, which may include: introducing a pretreatment gas into a device loaded with a waste battery powder, and bringing a gas outlet into communication with absorption liquid A and absorption liquid B in order; raising the temperature and introducing the pretreatment gas; reducing the temperature and introducing a reaction gas; raising the temperature, introducing the reaction gas, and then introducing the pretreatment gas; and reducing the temperature, and turning off the pretreatment gas; adding an extractant to absorption liquid A, mixing the mixture, taking organic phase A, adding a stripping agent, and taking aqueous phase A; and adjusting the pH to acidity, then adding an extractant, taking organic phase B, adding a stripping agent to obtain a stock solution enriched in Li, Mn, Ni and Co.
Opening claim text (preview).
The invention claimed is: 1. A method for recycling a battery by incomplete extraction, characterized by comprising: (1) subjecting waste batteries to discharging, crushing, and pyrolysis to obtain a waste battery powder; (2) introducing a pretreatment gas into a device loaded with the waste battery powder, and bringing a gas outlet of the device into communication with absorption liquid A and absorption liquid B in order; (3) performing the following operations on the device loaded with the waste battery powder: raising the temperature and continuing to introduce the pretreatment gas; reducing the temperature and introducing a reaction gas; raising the temperature, introducing the reaction gas, and then introducing the pretreatment gas; and reducing the temperature, and turning off the pretreatment gas; (4) adding a first extractant to absorption liquid A, mixing the mixture, carrying out liquid separation, taking organic phase A, adding a first stripping agent for liquid separation, and taking aqueous phase A; and (5) adjusting the pH of aqueous phase A to acidity, then adding a second extractant for liquid separation, taking organic phase B, adding a second stripping agent for liquid separation to obtain a stock solution enriched in Li, Mn, Ni and Co; wherein the pretreatment gas is at least one of nitrogen, helium, argon or neon; the reaction gas is one of chlorine gas, fluorine gas or bromine gas; absorption liquid A is an acid solution, the acid solution is HCl; and absorption liquid B is an alkaline solution, the alkaline solution is a NaOH or KOH solution; wherein, in step (4), the first extractant is [(CH 3 ) 3 C(CH 2 ) 5 CH(CH 3 )CH 2 ]HPO 2 and the first stripping agent is diethylenetriamine pentaacetic acid; in step (5), the second extractant is [CH 3 (CH 2 ) 4 CH(CH 3 )CH 2 ] 2 HPO 2 and the second stripping agent is triethylenetetraamine hexaacetic acid. 2. The method of claim 1 , wherein, in step (2), the introduced pretreatment gas has a flow rate of 10-30 mL/min and a temperature of 20-40° C. 3. The method of claim 1 , wherein, the specific operation of step (3) involves: raising the temperature to 300-400° C. at a ramp rate of 3-5° C./min, maintaining the flow rate, continuing to introduce the pretreatment gas for 20-60 min, and maintaining the gas flow rate; reducing the temperature to 20-40° C. and then introducing the reaction gas at a flow rate of 10-50 mL/min; raising the temperature to 200-240° C. at a ramp rate of 3-5° C./min, maintaining the temperature and introducing the reaction gas for 1-3 h; raising the temperature to 280-320° C. at a ramp rate of 3-5° C./min, maintaining the temperature and introducing the reaction gas for 2-3 h; further raising the temperature to 360-380° C. at a ramp rate of 3-5° C./min, maintaining the temperature and introducing the reaction gas for 1-3 h; and finally raising the temperature to 450-470° C. at a ramp rate of 3-5° C./min, maintaining the temperature, introducing the reaction gas for 2-4 h, turning off the reaction gas, introducing the pretreatment gas, and reducing the temperature to 20-35° C. 4. The method of claim 1 , wherein, in step (4), the volume ratio of absorption liquid A to the first extractant is 1:(1-5); and in step (4), the volume ratio of organic phase A to the first stripping agent is 1:(1-5). 5. The method of claim 1 , wherein, in step (5), the volume ratio of organic phase B to the second stripping agent is 1:(1-5). 6. Use of the method of claim 1 in metal recovery.
Phosphinic acid, e.g. H2P(O)(OH) · CPC title
Roasting processes (C22B1/16 takes precedence) · CPC title
Binding; Briquetting {; Granulating} · CPC title
Wet processes · CPC title
Treatment or purification of solutions, e.g. obtained by leaching (C22B23/0407 takes precedence) · CPC title
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