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Process for producing iron phosphate for producing iron lithium phosphate material

A technology of lithium iron phosphate and iron phosphate, applied in the field of preparation of iron phosphate, can solve the problems of low reactivity, difficulty in diffusion of lithium ions, etc.

Inactive Publication Date: 2008-05-07
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ferric phosphate material with two crystal waters produced by the method of the present invention has a crystal structure similar to lithium iron phosphate, which overcomes the problem that commercially available ferric phosphate products have a complete grain structure, low reactivity, and lithium ion It is very difficult to diffuse in it, and it is difficult to insert lithium ions in the subsequent sintering process to form the shortcomings of lithium iron phosphate crystals suitable for lithium-ion battery cathode materials, thereby improving the performance of lithium iron phosphate materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve analytically pure ferric chloride in distilled water, prepare a 0.05 M aqueous solution, and add 0.01% by mass of ferric chloride sodium dodecylbenzene sulfonate to make the iron ions form surfactant-encapsulated micelles , And then according to the molar ratio as Fe 3+ : PO 4 3- Add analytically pure phosphoric acid at a ratio of 1:0.8 and stir evenly. Slowly add 1M NaOH aqueous solution under stirring. The addition time is longer than 1 hour until the pH value of the solution reaches 6, and the resulting iron phosphate precipitates are filtered and filtered out The ferric phosphate is washed 3 times with distilled water twice its weight, and dried at 60°C under vacuum to obtain FePO 4 ·2H 2 O powder.

Embodiment 2

[0021] The analytical pure ferric nitrate is dissolved in distilled water to prepare a 5 M aqueous solution, and sodium alkenyl sulfonate with a mass of 3% by mass of ferric nitrate is added to make the iron ions form surfactant-encapsulated micelles, and then the molar ratio is Fe 3+ : PO 4 3- Add analytical pure phosphoric acid at a ratio of 1:1.2 and stir evenly. Slowly add 9M KOH aqueous solution under stirring. The addition time is longer than 1 hour until the pH value of the solution reaches 7. The precipitated iron phosphate material is filtered and filtered out. Iron phosphate is washed with 5 times its weight in distilled water for 5 times, and dried at 90°C under vacuum to obtain FePO product 4 ·2H 2 O powder.

Embodiment 3

[0023] The analytically pure iron sulfate is dissolved in distilled water to prepare a 0.5M aqueous solution, and sodium lauryl sulfate with a mass of 0.1% by mass of ferric sulfate is added to make the iron ions form surfactant-encapsulated micelles, and then the molar ratio is Fe 3+ : PO 4 3- Add analytical pure phosphoric acid at a ratio of 1:1.0 and stir evenly. Slowly add 3M ammonia solution under stirring. The addition time is longer than 1 hour until the pH value of the solution reaches 6. The precipitated iron phosphate material is filtered and filtered out. Iron phosphate was washed 4 times with 3 times its weight in distilled water and dried at 80°C under vacuum to obtain FePO product 4 ·2H 2 O powder.

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Abstract

The preparation method of iron phosphate used for preparing lithium iron phosphate material in the present invention relates to heavy metal phosphate, and the steps are: dissolving analytically pure soluble iron salt in distilled water to prepare a 0.05-5M aqueous solution, and the added mass is the iron salt mass 0.01~3% of anionic surfactant, then add analytically pure phosphoric acid according to the molar ratio of Fe3+:PO43-=1:0.8~1.2 and stir evenly, and slowly add alkaline solution with a concentration of 1~9M under stirring , the feeding time is more than 1 hour, until the pH value of the solution reaches 6-7, the iron phosphate precipitate is filtered, and the filtered iron phosphate is washed 3-5 times with distilled water 2-5 times its weight. Dry at ~90°C to obtain the product FePO4·2H2O powder. The iron phosphate product with two crystal waters prepared by the method of the invention has high reactivity, and the performance of the lithium iron phosphate material made by using it is better than that of the lithium iron phosphate material made by commercially available iron phosphate products.

Description

Technical field [0001] The technical scheme of the present invention relates to heavy metal phosphates, in particular to a method for preparing iron phosphate for preparing lithium iron phosphate materials. Background technique [0002] Lithium iron phosphate has high theoretical capacity (170mAh / g), high working voltage (voltage platform around 3.5V), and appropriate mass density (3.64g / cm 3 ), small self-discharge, LiFePO at low current density 4 Li in + Almost 100% embedding / de-embedding, long cycle life, good cycle performance, no memory effect, low price, good thermal stability, environmental friendliness, etc. It is expected to replace the higher-cost LiCoO 2 Become a new generation of lithium-ion battery cathode material. [0003] At present, the solid-phase reaction method is the main method for the synthesis of lithium iron phosphate materials. In the preparation methods of lithium iron phosphate materials disclosed in CN 1581537, CN 1753216, CN 1958440, CN 1958441 and C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37C01B25/45
Inventor 梁广川欧秀芹王丽郅晓科崔军燕
Owner HEBEI UNIV OF TECH
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