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Method for preparing lithium titanate precursor and lithium iron phosphate precursor by comprehensively utilizing ilmenite

A lithium iron phosphate and precursor technology is applied in the field of comprehensively utilizing ilmenite to prepare lithium titanate and lithium iron phosphate precursors, and achieves the effects of simple process flow, excellent electrochemical performance and stable product quality.

Inactive Publication Date: 2010-11-03
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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 lithium titanate precursor and lithium iron phosphate precursor by comprehensively utilizing ilmenite
  • Method for preparing lithium titanate precursor and lithium iron phosphate precursor by comprehensively utilizing ilmenite
  • Method for preparing lithium titanate precursor and lithium iron phosphate precursor by comprehensively utilizing ilmenite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Separation of ferro-ilmenite: the ilmenite is ball-milled until the particle size is below 5 microns, and the ilmenite is leached under normal pressure with sulfuric acid with a mass concentration of 5%, the mass ratio of sulfuric acid to ilmenite is 1.8, and the leaching temperature is 100 degrees Celsius , The leaching time is 10 hours. After the leaching is completed, the slurry is cooled to room temperature, and filtered to obtain a filter residue and a filtrate.

[0032] (2) Preparation of lithium titanate precursor: the filter residue obtained in step (1) was washed twice with sulfuric acid with a mass concentration of 5%, and then dissolved with sulfuric acid with a mass concentration of 85%, and the molar ratio of sulfuric acid to titanium was 1.5: 1. Add deionized water to dilute until the molar concentration of titanium is 0.5mol / L, add ammonium oxalate, the molar ratio of ammonium oxalate to titanium is 2:1, react for 1 hour, cool to 3 degrees Celsius, le...

Embodiment 2

[0035] (1) Ferro-ilmenite separation: the ilmenite is ball-milled to a particle size of less than 5 microns, and the ilmenite is leached under normal pressure with sulfuric acid with a mass concentration of 15%. The mass ratio of sulfuric acid to ilmenite is 2.5, and the leaching temperature is 120 Celsius, the leaching time is 0.5 hours. After the leaching is completed, the slurry is cooled to room temperature, and filtered to obtain a filter residue and a filtrate.

[0036] (2) Preparation of lithium titanate precursor: the filter residue obtained in step (1) was washed twice with sulfuric acid with a mass concentration of 10%, and then dissolved with sulfuric acid with a mass concentration of 90%, and the molar ratio of sulfuric acid to titanium was 3: 1. Dilute with deionized water until the molar concentration of titanium is 2 mol / L, add oxalic acid, the molar ratio of oxalic acid and titanium is 1:1, react for 4 hours, cool to 1 degree Celsius, let stand for 0.5 hours, f...

Embodiment 3

[0040] (1) Separation of ferro-ilmenite: the ilmenite is ball-milled to a particle size of less than 5 microns, and the ilmenite is leached under normal pressure with sulfuric acid with a mass concentration of 25%. The mass ratio of sulfuric acid to ilmenite is 1.2, and the leaching temperature is 80 Celsius, the leaching time is 20 hours. After the leaching is completed, the slurry is cooled to room temperature, and filtered to obtain a filter residue and a filtrate.

[0041] (2) Preparation of lithium titanate precursor: the filter residue obtained in step (1) was washed twice with sulfuric acid with a mass concentration of 1%, and then dissolved with sulfuric acid with a mass concentration of 75%, and the molar ratio of sulfuric acid to titanium was 1: 1. Dilute with deionized water until the molar concentration of titanium is 0.1mol / L, add sodium oxalate, the molar ratio of sodium oxalate and titanium is 4:1, react for 10 minutes, cool to 5 degrees Celsius, let stand for 1...

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Abstract

The invention discloses a method for preparing a lithium titanate precursor and a lithium iron phosphate precursor by comprehensively utilizing ilmenite. The method is characterized by comprising the following steps of: 1) separating ferrotitanium: performing ball milling on the ilmenite, leaching the ilmenite with sulfuric acid, cooling and filtering the leached ilmenite to obtain filter residue and filtrate; 2) preparing a lithium titanate precursor: washing the obtained filter residue with dilute sulfuric acid, dissolving the filter residue in 75 to 90 percent sulfuric acid, diluting the mixture, adding a precipitator into the mixture for reaction, cooling, standing and filtering the mixture, and drying the filter residue to obtain the precursor of the lithium titanate; and 3) preparing the lithium iron phosphate precursor: diluting the filtrate, adding oxidant and precipitator into the solution, controlling the pH value of the system with aqueous solution of alkali, and washing, filtering and drying the precipitate after the reaction to obtain the precursor of the lithium iron phosphate, namely ferric phosphate. The method has the advantages of wide raw material source, simple process flow, high and stable product quality, and low cost and comprehensive and full utilization of the ilmenite.

Description

technical field [0001] The invention relates to a method for preparing a lithium titanate precursor for negative electrode materials and a lithium iron phosphate precursor for positive electrode materials, in particular to a method for preparing lithium titanate and lithium iron phosphate precursors from ilmenite. technical background [0002] In recent years, lithium titanate with a spinel structure has been widely used due to its excellent structural stability (Li-ion deintercalation process) and safety performance (Li 4 Tu 5 o 12 Relative to Li / Li + 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 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 sta...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01G23/00
Inventor 王志兴伍凌李新海郭华军李灵均彭文杰张云河胡启阳吴飞翔
Owner CENT SOUTH UNIV
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