A kind of impurity removal and treatment method in the recycling process of lithium battery scrap positive electrode materials

A cathode material, lithium battery technology, applied in battery recycling, lithium storage battery, waste collector recycling, etc., can solve problems affecting the stability of co-precipitation process, lithium ion poisoning, etc.

Active Publication Date: 2021-03-09
SICHUAN ENERGY INTERNET RES INST TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The applicant's research aims to solve the problem that the online pH meter is prone to lithium ion poisoning in a solution with high lithium ion concentration and affects the stability of the co-precipitation process

Method used

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  • A kind of impurity removal and treatment method in the recycling process of lithium battery scrap positive electrode materials
  • A kind of impurity removal and treatment method in the recycling process of lithium battery scrap positive electrode materials
  • A kind of impurity removal and treatment method in the recycling process of lithium battery scrap positive electrode materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Step 1: At room temperature, add 30 L of lithium battery scrap cathode material leaching solution into the 50 L first reaction kettle.

[0083] Step 2: Use a pH meter to control the peristaltic pump online to pump 2 mol / L lithium hydroxide solution into the first reaction kettle until the pH value is stable at 5.5, stop pumping the lithium hydroxide solution, and allow the mixture to react for 1 hour. The reaction consumed a total of 4.2 L of lithium hydroxide solution.

[0084]Step 3: filter the reacted mixture with a filter press of 200 mesh filter cloths, and use 0.6 MPa high-pressure air to blow-wash the filter cake until no filtrate flows out. During the filtration process, if the internal pressure of the filter press rises rapidly, for example, when it rises to the pressure upper limit of 0.5MPa within 2 minutes, the filtration needs to be stopped, indicating that the filterability of the precipitate is poor. Wait until the pressure drops to 0MPa, and then contin...

Embodiment 2

[0089] Step 1: Add 10 L of the filtrate in Example 1 to the 50 L first reaction kettle as the first bottom liquid, so that the electrode of the pH meter is located below the liquid level, and heat the first reaction kettle to keep the reaction temperature at 70°C.

[0090] Step 2: Use a peristaltic pump to pump the leaching solution of the scrapped positive electrode material of the lithium battery and the 2 mol / L lithium hydroxide solution into the first reaction kettle respectively. The pumping speed of lithium battery scrap cathode material leaching liquid is controlled at 200 ml / min, and the pumping speed of lithium hydroxide is controlled by an online pH meter, and the pumping speed of lithium hydroxide is controlled so that the pH of the mixture is 5.5. After fully reacting for 3 h, the mixture overflowed from the overflow port of the first reaction kettle and entered the first aging kettle. During this process, a total of 36 L of lithium battery scrap positive electrode...

Embodiment 3

[0132] Step 1: Add 10L of deionized water and 300mL of 23.5% ammonia water into the 50L second reaction kettle as the second bottom liquid, maintain the reaction temperature at 50°C, and pass nitrogen gas as the protective gas.

[0133] Step 2: The first filtrate obtained in Example 2 was pumped into the second reactor at a flow rate of 60 mL / min, and 12% ammonia water was pumped into the second reactor at a flow rate of 5 mL / min. Use a pH meter to control the flow rate of the pumped 4mol / L lithium hydroxide solution in real time, and control the flow rate of the lithium hydroxide solution so that the pH of the mixture is between 10.7-11.2. After fully reacting for 5 hours, the mixture overflowed from the overflow port of the second reaction kettle and flowed into the second aging kettle.

[0134] Step 3: heating the second aging tank to keep the aging temperature at 50° C., and aging the mixture in the second aging tank for 1 hour.

[0135] Step 4: filter the aged mixture wi...

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Abstract

The embodiment of the present application discloses a method for removing impurities and treating waste positive electrode materials of lithium batteries during the recovery process. Including at a first temperature higher than room temperature and a fixed first pH value, controlling the flow rate of the lithium battery scrap positive electrode material leaching solution and the first alkaline solution to precipitate and remove iron ions, aluminum ions and at least part of the copper ions to obtain the first filtrate; Under the second temperature higher than room temperature and the fixed first pH range, control the flow velocity of the first filtrate, complexing agent and the second alkaline solution to separate the second filtrate containing lithium ions to obtain the precipitation of the target substance; carry out the precipitation of the target substance Dissolving to obtain a first solution; at a third temperature higher than room temperature and a fixed fluoride ion concentration, controlling the flow rate of the first solution and a fluorine-containing precipitant to precipitate and remove calcium ions, magnesium ions and at least part of lead ions to obtain a target solution. Through the method of the present application, a precipitate with large particle size, high crystallinity and low water content can be obtained, which is convenient for washing and improves the recovery rate of nickel-cobalt-manganese, the scrap positive electrode material of lithium batteries.

Description

technical field [0001] The present application relates to the technical field of material recycling, in particular to a method for removing impurities and treating waste positive electrode materials of lithium batteries during the recycling process. Background technique [0002] In the recycling process of lithium battery scrap positive electrode materials, the dissolved nickel-cobalt-manganese solution often contains a variety of metal impurities (for example, Fe, Al, Cu, Ca, Mg or Pb, etc.), if the impurities are not removed, the above impurities will be harmful to the The quality and performance of the lithium battery cathode material synthesized after recycling the scrap cathode material of the lithium battery will be affected. [0003] The impurity removal method for metal impurities such as Fe, Al, Ca, Mg, etc. in the prior art has the problem that the precipitate is difficult to filter and wash, resulting in the impurity precipitate that cannot be filtered in the actu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/54H01M10/052H01M6/52H01M6/14B01D36/04
CPCH01M10/54H01M10/052H01M6/52H01M6/14B01D36/04Y02E60/10Y02W30/84Y02P10/20B01D21/01H01M2004/028C22B3/22C22B3/42C22B7/007C22B15/0089C22B21/0023C22B23/0461C22B26/12C22B26/20C22B47/00
Inventor 容忠言张久俊戴林杉隋邦杰时一方
Owner SICHUAN ENERGY INTERNET RES INST TSINGHUA UNIV
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