Closed-loop recovery method of lithium-containing molten salt

A recycling method and molten salt technology, applied in chemical instruments and methods, inorganic chemistry, electrical components, etc., can solve the problems of excessive use of electrode materials, inability to achieve large-scale production and preparation, and waste of molten salt.

Active Publication Date: 2021-01-26
HUNAN UNIV OF HUMANITIES SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a closed-loop recovery method for lithium-containing molten salt to solve the technical problems of excessive use of electrode materials prepared by the existing molten salt method, waste of molten salt, and inability to realize large-scale production and preparation

Method used

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  • Closed-loop recovery method of lithium-containing molten salt
  • Closed-loop recovery method of lithium-containing molten salt
  • Closed-loop recovery method of lithium-containing molten salt

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Configure the lithium-containing molten salt system, the lithium-containing molten salt system is a mixed system of the first lithium salt and the second lithium salt, the first lithium salt is LiCl, the second lithium salt is LiOH, the amount of LiOH substance is 86mmol, and the amount of LiCl substance The amount is 50.7mmol;

[0063] Will LiNi 0.5 co 0.2 mn 0.3 o 2 Precursor mixed with lithium-containing molten salt system, LiNi 0.5 co 0.2 mn 0.3 o 2 The molar ratio of the precursor to the lithium-containing molten salt system is 1:5, and the mixture is obtained. The mixture is transferred to a high-temperature kiln and fed with oxygen. First, it is preheated at 300°C for 2 hours, and then heated to 850°C. , keep the temperature for 6h for sintering, cool after sintering, wash with water three times, and collect the filtrate and sediment;

[0064] Introduce oxygen into the precipitate and heat it to 850°C, keep it warm for 2 hours to dry, and obtain the lithi...

Embodiment 2

[0067] Titration analysis

[0068] Obtain after the filtrate of recovery is dried and reclaim lithium-containing molten salt, carry out titration test:

[0069] The titration of LiOH: take methyl red-bromocresol green as indicator, titrate the total alkalinity in the sample filtrate with a certain concentration of hydrochloric acid standard titration solution, calculate the content of lithium hydroxide with the amount of consumption of hydrochloric acid standard titration solution, 3 Group parallel.

[0070] Titration of LiCl: with standard AgNO 3 Solution titration of Cl in sample filtrate － Form AgCl precipitate, with potassium chromate as indicator, when Cl － After precipitation, the Ag + with CrO 4 2- Formation of red precipitate 2Ag + +CrO 4 2- =Ag 2 CrO 4 ↓(red) indicates the arrival of the end point. According to AgNO 3 The amount of (Ag needs to be deducted + The amount consumed by the hydroxide precipitation reaction with LiOH) can be calculated as Cl －...

Embodiment 3

[0072] For the LiNi of Example 1 0.5 co 0.2 mn 0.3 o 2 The mixture obtained after the precursor was mixed with the lithium-containing molten salt system was tested by in-situ XRD.

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Abstract

The invention discloses a closed-loop recovery method of lithium-containing molten salt, and the method comprises the following steps: preparing a lithium-containing molten salt system which is a mixed system of a first lithium salt and a second lithium salt; mixing the lithium battery electrode material precursor with a lithium-containing molten salt system to obtain a mixture, transferring the mixture into a high-temperature kiln, performing preheating, heating and sintering, performing cooling and washing after sintering, and collecting filtrate and precipitate; heating and drying the precipitate to obtain a lithium battery electrode material named as NCM-P; and supplementing the second lithium salt into the filtrate until the amount of substance required for preparing the NCM-P is reached, adding a lithium battery electrode material precursor with the amount of substance the same as that of the NCM-P, performing uniform mixing, performing drying to obtain a mixture, and repeating the preparation method to obtain the NCM-1,..., NCM-n. According to the closed-loop recovery method of the lithium-containing molten salt, closed-loop reutilization can be realized without separating out residual lithium-containing molten salt or titrating and analyzing filtrate components.

Description

technical field [0001] The invention relates to the field of lithium-containing materials, in particular to a closed-loop recovery method for lithium-containing molten salt. Background technique [0002] At present, the preparation of lithium-ion battery electrode materials mainly adopts solid-state method, that is, after mixing the precursor and lithium salt according to the stoichiometric ratio, at high temperature, the reactants diffuse in the crystal lattice through the particle contact surface to form the final electrode material. The advantage of this method is that the process is simple and easy to industrialize. But the defects are also very obvious: 1) The reaction process is mainly determined by the rate at which the reactant molecules or ions diffuse into the lattice under the action of thermal motion. Generally, the higher the reaction temperature, the more intense the thermal motion. Therefore, in order to quickly To obtain the product, the preparation temperat...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/525H01M10/0525C01G53/00
CPCH01M4/505H01M4/525H01M10/0525C01G53/50Y02E60/10
Inventor 陈占军郭军钟洪彬胡传跃付小宁朱杰彭秧锡
Owner HUNAN UNIV OF HUMANITIES SCI & TECH
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