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A method for preparing lithium battery electrode materials by using waste slag extracted from vanadium

A technology for extracting vanadium slag and electrode materials, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of low utilization rate of Ti resources, low added value, hidden dangers of disasters, etc., and achieve high utilization rate of added value, The effect of improving electrochemical performance and avoiding environmental pollution

Active Publication Date: 2018-02-02
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above utilization methods are overall utilization, in fact, they only use part of the components in the waste slag, and the added value is not high, especially the utilization rate of Ti resources is very low.
However, if it is dumped randomly, the dissociation and diffusion of toxic ions of heavy metals such as vanadium and chromium will inevitably cause direct pollution and major disaster hazards to the environment.

Method used

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  • A method for preparing lithium battery electrode materials by using waste slag extracted from vanadium
  • A method for preparing lithium battery electrode materials by using waste slag extracted from vanadium
  • A method for preparing lithium battery electrode materials by using waste slag extracted from vanadium

Examples

Experimental program
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Effect test

Embodiment 1

[0052] (1) Separation of iron and titanium:

[0053] After the vanadium extraction waste slag is mechanically crushed, the vanadium extraction waste slag is roasted with ammonium sulfate. The ammonium sulfate extraction vanadium waste slag ratio is 4:1. Ionized water was leached at 80°C for 60 minutes, and filtered to obtain iron-rich filtrate and titanium-rich filter residue;

[0054] (2) Preparation of yellow ammonium jarosite:

[0055] Add hydrogen peroxide to the iron-rich filtrate gained in step (1), the Fe in the iron-rich filtrate 2+ Oxidized to Fe 3+ . Afterwards, heat the iron-rich filtrate under stirring conditions, the temperature is 80°C, add ammonia water at the same time to adjust the pH value of the filtrate to 2.0, and then start timing. The reaction time is 8 hours. During the reaction process, continuously add ammonia water to the filtrate to neutralize the of sulfuric acid. After the reaction is finished, the feed liquid is filtered, and the filter resi...

Embodiment 2

[0064] (1) Separation of iron and titanium:

[0065] After the vanadium extraction waste slag is mechanically crushed, the vanadium extraction waste slag is roasted with ammonium sulfate. The ammonium sulfate extraction vanadium waste slag ratio is 4:1. Ionized water was leached at 85°C for 120 minutes, and filtered to obtain iron-rich filtrate and titanium-rich filter residue

[0066] (2) Preparation of yellow ammonium jarosite:

[0067] Add hydrogen peroxide to the iron-rich filtrate gained in step (1), the Fe in the iron-rich filtrate 2+ Oxidized to Fe 3+ . Afterwards, the iron-rich filtrate was heated with stirring at a temperature of 85° C., and ammonia water was added to adjust the pH value of the solution while the temperature was raised. The pH of the solution is 1.5. When the set condition is reached, the timing starts. The reaction time is 6 hours. During the reaction, ammonia water is continuously added to the solution to neutralize the sulfuric acid produced. ...

Embodiment 3

[0076] (1) Separation of iron and titanium:

[0077] After the vanadium extraction waste slag is mechanically crushed, the vanadium extraction waste slag is roasted with ammonium sulfate. The ammonium sulfate extraction vanadium waste slag ratio is 4:1. Ionized water was leached at 90°C for 180 minutes, and filtered to obtain iron-rich filtrate and titanium-rich filter residue

[0078] (2) Preparation of yellow ammonium jarosite:

[0079] Add hydrogen peroxide to the iron-rich filtrate gained in step (1), the Fe in the iron-rich filtrate 2+ oxidized to Fe 3+ . Afterwards, the iron-rich filtrate was heated under the condition of stirring, and the temperature was 90° C., and ammonia water was added to adjust the pH value of the solution while the temperature was raised. The pH of the solution is 2.5. When the set condition is reached, the timing starts. The reaction time is 8 hours. During the reaction, ammonia water is continuously added to the solution to neutralize the sulf...

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Abstract

The invention discloses a method for preparing lithium battery electrode materials by utilizing vanadium extraction waste residue, which belongs to the technical field of lithium ion battery electrode material preparation; including: (1) separation of iron and titanium: (2) preparation of xanthoferrite: (3) preparation of LiFePO4 Lithium secondary battery cathode material: (4) Preparation of lithium titanate precursor: (5) Preparation of Li4Ti5O12 lithium secondary battery anode material: This invention uses the difficult-to-process multiple water leaching vanadium waste residues as raw materials and uses selective precipitation Technology to prepare lithium ion battery negative electrode material lithium titanate and positive electrode material lithium iron phosphate precursor, and then prepare these two lithium ion battery positive and negative electrode materials - LiFePO4 and Li4Ti5O12 at low cost, to realize the analysis of various valuable elements in the vanadium extraction waste residue To achieve recycling and high value-added utilization; realize solid waste resource utilization and environmental friendliness, and protect the environment.

Description

[0001] The invention belongs to the technical field of preparation of lithium ion battery electrode materials, and in particular relates to a method for preparing lithium battery electrode materials (lithium iron phosphate and lithium titanate) by using vanadium extraction waste slag. Background technique [0002] In recent years, lithium iron phosphate with olivine structure has a high theoretical specific capacity (170mAh·g -1 ), good cycle performance, good thermal stability, low price, and environmental friendliness, it has become one of the most promising cathode materials for lithium-ion batteries. Lithium titanate with a spinel structure has excellent structural stability ("zero strain" in the lithium ion intercalation process) and safety performance (Li 4 Ti 5 o 12 : relative to Li / Li 十 The reduction potential is 1.5V, which can avoid the precipitation of metal lithium), and is considered to be a good anode material for high-power lithium-ion batteries and asymmetri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485H01M4/58H01M10/0525
CPCH01M4/485H01M4/5825H01M10/0525Y02E60/10
Inventor 罗绍华王志远吕方包硕张俊杨司楠郭克石杨悦刘东芳孙梅竹
Owner NORTHEASTERN UNIV LIAONING
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