Production method of battery-grade iron phosphate

A production method, ferric phosphate technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as complex process and large alkali consumption, achieve fine and uniform particle size, simplify production process, and reduce production cost Effect

Inactive Publication Date: 2011-05-11
易玲 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this method is more complicated, and the alkali consumption is larger when adjusting the pH value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] First put the solid polyferric sulfate into the dissolution kettle, add water to dissolve it into a solution with an iron ion concentration of 0.1-0.3M, let the polyferric sulfate solution stand still, and after the solution is clarified, take the supernatant liquid into the reaction kettle and mix with Phosphate solution reaction, the reaction temperature is controlled at 40-75°C, and the reaction time is 30-70 minutes to obtain basic ferric phosphate slurry, which is press-filtered; and then treated with 0.4-0.7M phosphoric acid solution. For basic ferric phosphate, adjust the pH value of the solution to 1-3, the reaction temperature is 50-90°C, and the reaction time is 1-4 hours to obtain white ferric phosphate slurry, which is separated from solid and liquid, filtered, washed, dried, Pulverize to obtain battery grade iron phosphate, the Fe content of the product is 29.32%, and the purity is 99.4%.

Embodiment 2

[0012] Put the solid polyferric sulfate into the dissolution kettle, add water to make a solution with an iron ion concentration of 0.15M, let it stand, and after the solution is clarified, take the supernatant liquid into the reaction kettle;

[0013] Dissolve diammonium hydrogen phosphate into a solution with a concentration of 0.14M, add it into the reaction kettle to react with polyferric sulfate, control the temperature at 55°C, and keep it warm for 30 minutes to obtain basic ferric phosphate slurry, and press filter the slurry;

[0014] Make phosphoric acid into a 0.5M solution in the treatment kettle, then put the filtered basic ferric phosphate material into the treatment kettle, adjust the pH value of the solution to 2 with ammonia water, keep the temperature at 65°C, and react for 4 hours to obtain white iron phosphate slurry, filtered, washed, and dried to obtain battery-grade iron phosphate. The Fe content of the obtained product is 29.41%, and the purity is 99.5%....

Embodiment 3

[0016] Add solid polyferric sulfate into the dissolution kettle, add water to make a solution with an iron ion concentration of 0.12M, let it stand, and after the solution is clarified, take the supernatant liquid into the reaction kettle;

[0017] Dissolve ammonium dihydrogen phosphate into a solution with a concentration of 0.12M, add it to the reaction kettle to react with polyferric sulfate, control the temperature at 75°C, and keep it warm for 30 minutes to obtain basic ferric phosphate slurry, and press filter the slurry;

[0018] Make phosphoric acid into a 0.5M solution in the treatment kettle, then add the basic ferric phosphate material after pressure filtration into the treatment kettle, adjust the pH value of the solution to 2 with ammonia water, keep the temperature at 75°C, and react for 3 hours to obtain white iron phosphate slurry, filtered, washed, and dried to obtain battery-grade iron phosphate. The Fe content of the product is 29.52%, and the purity is 99.5...

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Abstract

The invention relates to a production method of battery-grade iron phosphate, comprising the following steps of: dissolving polymeric iron sulfate into a solution with the iron ion concentration of 0.03-0.3 M; then adding a phosphate solution to generate an alkali iron phosphate sizing agent; then carrying out solid-liquid separation on the alkali iron phosphate sizing agent; adding separated alkali iron phosphate to a phosphoric acid solution for processing, and regulating a pH value; and then filtering, washing and drying to obtain the battery-grade iron phosphate. The invention reduces theusing amount of alkali in the producing process by utilizing the polymeric iron sulfate as ferric iron ions and the characteristics of lower acidity of the polymeric iron sulfate compared with iron salt, i.e. iron sulfate and the like, has the advantages of simple process flow, low production cost, high product purity, Fe content higher than 29 percent, purity higher than 99 percent and small anduniform grain diameter and is especially suitable for producing lithium iron phosphate, i.e. a positive pole material, of a lithium ion battery.

Description

technical field [0001] The invention belongs to a method for manufacturing electrode materials, in particular to a method for producing battery-grade iron phosphate. technical background [0002] Ferric phosphate has important application value as the raw material of producing lithium ion battery cathode material lithium ferrous phosphate, and the production method of ferric phosphate also has multiple, checks Chinese patent document and knows: CN1635648 and CN101172594 provide a kind of by ferric iron It is formed by the reaction of salt and phosphate, and the iron salts are mainly ferric chloride, ferric nitrate, ferric sulfate, etc. In the reaction process of this method, a large amount of alkali is needed to adjust the pH due to the strong acidity of the iron salt, and the iron phosphate generated after the reaction of the iron salt and phosphoric acid contains basic iron phosphate, thereby affecting the purity of the product. CN101209819 and CN101190785 provide a metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCY02E60/10
Inventor 易玲易佑华蒋新月
Owner 易玲
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