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Method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag

A technology for extracting vanadium waste slag and lithium iron phosphate, applied in chemical instruments and methods, phosphorus compounds, titanium compounds, etc., can solve the problems of low utilization rate of Ti resources, low added value, hidden dangers of disasters, etc., and achieve added value utilization. High rate, improve electrochemical performance, avoid environmental pollution

Active Publication Date: 2015-07-29
NORTHEASTERN UNIV LIAONING
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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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  • Method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag
  • Method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag
  • Method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag

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preparation example Construction

[0057] (2) Preparation of lithium iron phosphate precursor - iron phosphate: using leachate as raw material, using H 3 PO 4 Preparation of ferric phosphate by selective precipitation. A certain molar proportion of H 3 PO 4 Add the solution into the effluent, stir vigorously, add a certain amount of hydrogen peroxide to oxidize Fe(II) to Fe(III), and finally adjust the pH value with ammonia water, react at constant temperature, filter the obtained precipitate, wash and dry, and obtain phosphoric acid Iron powder.

[0058] (3) Preparation of lithium iron phosphate: using iron phosphate as raw material, LiFePO is synthesized by carbothermal reduction method 4 / C Lithium secondary battery cathode material. Weigh Li according to the stoichiometric ratio 2 CO 3 , precursors and organic carbon sources, mixed evenly, calcined under the protection of inert gas in the atmosphere furnace, and taken out after cooling to obtain LiFePO with a small amount of metal doping 4 / C cathod...

Embodiment 1

[0065] (1) Separation of iron and titanium:

[0066] After the vanadium extraction waste slag is mechanically crushed, the vanadium extraction waste slag is leached with hydrochloric acid with a mass concentration of 15% under normal pressure, the mass ratio of hydrochloric acid to vanadium extraction waste slag is 2.125, the leaching temperature is 70°C, and the leaching time is 2h; the leaching is completed Afterwards, the resulting slurry was cooled to room temperature, and filtered to obtain iron-rich leaching filtrate and titanium-rich leaching filter residue.

[0067] (2) Preparation of lithium iron phosphate precursor - iron phosphate:

[0068] The free HCl in the leaching solution obtained in step (1) is subjected to acid steam recovery treatment to obtain a concentrated leaching solution, which is prepared into an iron-rich leaching solution with a molar concentration of 0.265. According to the Fe / P molar ratio of 0.75, phosphoric acid H 3 PO 4 Add it to the iron-r...

Embodiment 2

[0077] (1) Separation of iron and titanium:

[0078] After the vanadium extraction waste slag is mechanically crushed, the vanadium extraction waste slag is leached under normal pressure with hydrochloric acid with a mass concentration of 20%, the mass ratio of hydrochloric acid to vanadium extraction waste slag is 1.75, the leaching temperature is 90°C, and the leaching time is 5h; the leaching is completed Afterwards, the resulting slurry was cooled to room temperature, and filtered to obtain iron-rich leaching filtrate and titanium-rich leaching filter residue.

[0079] (2) Preparation of lithium iron phosphate precursor - iron phosphate:

[0080] The free HCl in the leaching solution obtained in step (1) is subjected to recovery treatment by steaming acid to obtain a concentrated leaching solution, which is prepared into an iron-rich leaching solution with a molar concentration of 0.528. According to the Fe / P molar ratio of 0.87, phosphoric acid H 3 PO 4 Add it to the i...

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Abstract

The invention discloses a method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag. The method comprises the following steps: (1), iron and titanium separation: the vanadium extraction slag is leached with hydrochloric acid and filtered to obtain iron-rich leached filtrate and titanium-rich leached residues; (2), preparation of a LiFePO4 precursor: phosphoric acid is added to the iron-rich leached filtrate, H2O2 and ammonia water are added, and the mixture is precipitated, filtered and dried to obtain FePO4 powder; (3) preparation of a LiFePO4 lithium secondary battery cathode material: the FePO4 precursor, Li2CO3 and an organic carbon source are mixed and calcined to obtain LiFePO4 / C; (4) preparation of a Li4Ti5O12 precursor: NH3*H2O is added to the titanium-rich leached residues, the mixture is heated, then H2O2, ammonia water and concentrated H2SO4 are added, and filtrate is subjected to heating reaction and evaporated to dryness to obtain a titanium peroxide compound; (5), preparation of Li4Ti5O12 lithium secondary battery anode material: the titanium peroxide compound is calcined to obtain TiO2, and TiO2 and Li2CO3 are mixed and calcined to obtain Li4Ti5O12. Valuable elements of the vanadium extraction slag are wholly used to acquire a high added-value product, and efficient vanadium extraction slag utilization and environmental protection are realized.

Description

technical field [0001] The invention relates to a precursor method for lithium ion battery electrode materials, in particular to a method for preparing lithium battery electrode materials lithium iron phosphate and lithium titanate by extracting vanadium waste residue. Background technique [0002] In recent years, lithium iron phosphate of olivine structure has 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 asymmetric hybrid batterie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/04C01B25/45C01G23/00
CPCY02P10/20
Inventor 罗绍华郭克石陈东辉艾志宏滕飞吕方包硕杨悦刘东芳
Owner NORTHEASTERN UNIV LIAONING
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