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Method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite

A technology of lithium iron phosphate and ilmenite, which is applied in the direction of chemical instruments and methods, phosphorus compounds, titanium compounds, etc., can solve the problems of unseen precursors, etc., and achieve the effects of improving electrochemical performance, simple process flow, and low cost

Inactive Publication Date: 2010-05-19
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, there is no report on the comprehensive utilization of ilmenite to simultaneously prepare two kinds of electrode material precursors

Method used

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  • Method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite
  • Method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite
  • Method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Separation of ferro-titanium

[0037] The ilmenite is crushed to a particle size below 5 microns, and the ilmenite is leached with hydrochloric acid with a mass concentration of 25% under normal pressure. The mass ratio of the hydrochloric acid to the ilmenite is 1.8, the leaching temperature is 120°C, and the leaching time is 0.5 hours. After the leaching is completed, the slurry is cooled to room temperature and filtered to obtain filter residue and filtrate.

[0038] (2) Preparation of lithium titanate precursor

[0039] The filter residue obtained in step (1) was washed twice with hydrochloric acid with a mass concentration of 5%, and then placed in a sodium hydroxide solution with a concentration of 250g / L, cooked at 80°C for 3 hours, cooled to room temperature, and filtered to obtain a filter residue ; Then the filter residue is placed in hydrochloric acid with a mass concentration of 20%, steamed at 100 ℃ for 1 hour, cooled to room temperature, filtered, the filter...

Embodiment 2

[0043] (1) Separation of ferro-titanium

[0044] The ilmenite is crushed to a particle size of less than 5 microns, and the ilmenite is leached with hydrochloric acid with a mass concentration of 15% under normal pressure. The mass ratio of the hydrochloric acid to the ilmenite is 0.9, the leaching temperature is 100°C, and the leaching time is 5 hours. After the leaching is completed, the slurry is cooled to room temperature and filtered to obtain filter residue and filtrate.

[0045] (2) Preparation of lithium titanate precursor

[0046] The filter residue obtained in step (1) was washed twice with hydrochloric acid with a mass concentration of 10%, and then placed in a potassium hydroxide solution with a concentration of 170g / L, cooked at 150°C for 5 hours, cooled to room temperature, and filtered to obtain a filter residue ; Then the filter residue is placed in hydrochloric acid with a mass concentration of 30%, steamed at 120 ℃ for 10 minutes, cooled to room temperature, filter...

Embodiment 3

[0050] (1) Separation of ferro-titanium

[0051] The ilmenite was crushed to a particle size below 5 microns, and the ilmenite was leached with hydrochloric acid with a mass concentration of 35% under normal pressure. The mass ratio of hydrochloric acid to the ilmenite was 1.5, the leaching temperature was 80°C, and the leaching time was 3 hours. After the leaching is completed, the slurry is cooled to room temperature and filtered to obtain filter residue and filtrate.

[0052] (2) Preparation of lithium titanate precursor

[0053] The filter residue obtained in step (1) was washed twice with hydrochloric acid with a mass concentration of 2%, and then placed in a potassium hydroxide solution with a concentration of 20g / L, cooked at 120°C for 1 hour, cooled to room temperature, and filtered to obtain a filter residue ; Then the filter residue is placed in hydrochloric acid with a mass concentration of 10%, steamed at 90 ℃ for 4 hours, cooled to room temperature, filtered, the filter...

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Abstract

The invention discloses a method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite, which comprises the following steps of: 1) separating the ilmenite, namely crushing the ilmenite, leaching the ilmenite with hydrochloric acid, filtering the ilmenite to obtain a residue and a filtrate; 2) preparing the precursor of the lithium titanate, namely washing the residue prepared by step 1) with the hydrochloric acid, adding the washed residue in aqueous alkali, cooking the mixture, filtering the mixture after cooling, and then adding the obtained filter residue in the hydrochloric acid, cooking the mixture, and filtering, washing, drying and calcining the mixture after cooling to obtain the precursor of the lithium titanate; and 3) preparing the precursor of the lithium iron phosphate, namely taking the filtrate prepared by step 1) as a raw material, adding iron powder to reduce ferric iron, diluting the reduced filtrate, adding a complexing agent and a precipitant into the diluted mixture, controlling the pH value of the system, reacting the mixture at 30 to 80 DEG C, aging the reacted mixture, and filtering, washing and drying the obtained precipitate to obtain the precursor of the lithium iron phosphate. The method is wide in raw material source, simple in process flow, good and stable in product quality, low in cost and comprehensive and full in use of the ilmenite.

Description

Technical field [0001] The invention belongs to the field of lithium ion battery materials and preparation methods thereof, and relates to a method for preparing lithium titanate and lithium iron phosphate precursors by comprehensively utilizing ilmenite. Background technique [0002] In recent years, lithium titanate with a spinel structure has excellent structural stability (de-intercalation process of lithium ions) and safety performance (Li 4 Ti 5 O 12 Relative Li / Li + The reduction potential is 1.5V, which can avoid the precipitation of lithium metal). It is considered to be a good anode material for high-power lithium-ion batteries and asymmetric hybrid batteries. Lithium iron phosphate with olivine structure has become one of the most promising cathode materials for lithium-ion batteries due to its high theoretical specific capacity (170mAh / g), good cycle performance, good thermal stability, low price, and environmental friendliness. One. [0003] However, as the main raw m...

Claims

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Application Information

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IPC IPC(8): C22B3/10C01G23/00C01G23/053C01B25/45H01M4/58
CPCY02E60/12Y02E60/10Y02P10/20
Inventor 李新海伍凌王志兴郭华军王小娟彭文杰胡启阳张云河
Owner CENT SOUTH UNIV
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