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Closed-loop recovery method for lithium-containing molten salt

A recovery method and technology of molten salt, applied in the direction of chemical instruments and methods, nickel compounds, structural parts, etc., can solve problems such as waste of molten salt, inability to realize large-scale production preparation, and excessive use of electrode materials, so as to save time and reduce Effects of energy consumption and production cost reduction

Active Publication Date: 2022-02-15
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 for lithium-containing molten salt
  • Closed-loop recovery method for lithium-containing molten salt
  • Closed-loop recovery method for lithium-containing molten salt

Examples

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, which comprises a lithium-containing molten salt system, which is a mixed system of a first lithium salt and a second lithium salt; The lithium molten salt system is mixed to obtain a mixture, and the mixture is transferred to a high-temperature kiln, preheated first, then heated and sintered, cooled after sintered, washed with water, and the filtrate and precipitate are collected; the precipitate is heated and dried to obtain a lithium battery electrode material, Named as NCM‑P; add the second lithium salt to the filtrate to the amount required for the preparation of NCM‑P, and add the same amount of lithium battery electrode material precursor for the preparation of NCM‑P, mix evenly and dry The mixture is obtained, and the above preparation method is repeated to obtain NCM‑1, ..., NCM‑n. The above-mentioned closed-loop recovery method of lithium-containing molten salt can realize closed-loop reuse without separating the residual lithium-containing molten salt or titrating and analyzing the 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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Patent Type & Authority Patents(China)
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