Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite

A technology of lithium iron phosphate and ilmenite, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., to achieve simple process flow, stable product quality, and good product quality

Inactive Publication Date: 2009-12-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been no reports on the comprehensive utilization of ilmenite to prepare lithium iron phosphate precursors for lithium-ion battery cathode materials

Method used

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  • Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite
  • Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 500 grams of ilmenite are leached with sulfuric acid, filtered, and a certain amount of hematite and ferric sulfate are dissolved in the filtrate, so that the concentration of Fe in the mixed solution is 0.1mol / L, and the molar ratio of Ti to Fe is 0.3; Add a sufficient amount of sodium peroxide solution (1mol / L), then add phosphoric acid (1mol / L) that is equimolar to Fe, and adjust the pH to 2.5±0.1 with sodium hydroxide solution (0.5mol / L). React in a stirred reactor for 5 minutes, wash and filter the resulting precipitate, and dry it at 100°C to obtain a mixture of iron phosphate and doped phosphate, the precursor of lithium iron phosphate, the cathode material for lithium ion batteries.

Embodiment 2

[0025] Leach 500 grams of ilmenite with hydrochloric acid, filter, and dissolve a certain amount of ferric chloride in the filtrate, so that the concentration of Fe in the mixed solution is 1mol / L, and the molar ratio of Ti to Fe is 0.2; add a sufficient amount of Sodium hypochlorite solution (3mol / L), then add ammonium dihydrogen phosphate solution (0.1mol / L) equimolar to Fe, adjust pH=3.5±0.1 with lithium hydroxide solution (2mol / L), and stir at 60°C After reacting in the reactor for 24 hours, the resulting precipitate was washed, filtered, and dried at 50°C to obtain a mixture of iron phosphate and doped phosphate, which is the precursor of lithium iron phosphate, the positive electrode material of lithium ion batteries.

Embodiment 3

[0027] 500 grams of ilmenite are leached with sulfuric acid, filtered, and a certain amount of ferrous sulfate and ferrous chloride are dissolved in the filtrate, so that the concentration of Fe in the mixed solution is 2mol / L, and the molar ratio of Ti to Fe is 0.1; Add a sufficient amount of potassium chlorate solution (0.1mol / L) to the solution, then add an ammonium dihydrogen phosphate solution (3mol / L) equimolar to Fe, and adjust the pH to 4.5±0.1 with ammonia water (3mol / L). React in a stirred reactor for 10 hours, wash and filter the resulting precipitate, and dry it at 200°C to obtain a mixture of iron phosphate and doped phosphate, which is the precursor of lithium iron phosphate, the cathode material for lithium ion batteries.

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Abstract

The invention discloses a method for comprehensively utilizing titanic iron ore to prepare a precursor of the lithium iron phosphate, which is characterized in that titanium iron ore is immerged into an acid, filtering, a quantitative other ore resource is dissolved in the filtered solution, making the Fe concentration in the mixed solution to be from 0.01 to 3 mol / L and the molar ration of Ti to Fe to be from 0.0005 to 0.3; an oxidant and a sedimentation agent are put into the solution, wherein the concentration of the oxidant and the sedimentation agent is from 0.01 to 3 mol / L, using an alkaline solution from 0.01 to 6 mol / L to control pH value of the system between 1.5 and 6.0, reacting for from 5 minutes to 24 hours in an agitating reactor at a temperature of between 20 and 90 degree centigrade, the attained sedimentation is rinsed and filtered, the precursor of the lithium iron phosphate for the anode material of a lithium-ion battery is got after the attained sedimentation continues to be dried at a temperature of between 50 and 200 degree centigrade, and the precursor is a mixture of ferric phosphate and doped phosphate. The method for comprehensively utilizing titanic iron ore to prepare the precursor of the lithium iron phosphate has the advantages of wide raw material resource, simple process procedure, good and stable product quality, and low cost, which is particularly applicable to provide the high quality iron resource for the volume production of the lithium iron phosphate for the anode material of the lithium-ion battery and comprehensively utilize the titanic iron ore resource as well.

Description

technical field [0001] The invention relates to a preparation method of a lithium iron phosphate precursor, a cathode material of a lithium ion battery, in particular to a method for comprehensively utilizing ilmenite to prepare a lithium iron phosphate precursor, a cathode material of a lithium ion battery. technical background [0002] Lithium iron phosphate with an 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. . However, as the main raw material for the production of lithium iron phosphate-iron salt, the large-scale industrial production of lithium iron phosphate is seriously restricted due to shortcomings such as unstable product quality, low density, and low purity. [0003] At present, most of the iron sources for preparing lithium iron phosphate are chemically pure or ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 王志兴伍凌李新海郭华军彭文杰胡启阳张云河刘久清郑俊超李灵均
Owner CENT SOUTH UNIV
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