Preparation method of ferric phosphate

A technology of iron phosphate and phosphoric acid, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of difficult filtration, low capacity, and harm the quality of iron phosphate, and achieve the effect of stable iron content and high purity

Inactive Publication Date: 2015-01-14
徐越峰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In most of these preparation methods, when the pH regulator is mixed with iron phosphate, an irreversible side reaction occurs to generate hydroxide precipitation. As everyone knows, iron hydroxide is a typical hard-to-filter colloid, which endangers the quality of iron phosphate. After processing this type of iron phosphate into lithium iron phosphate batteries, there are generally problems such as low capacity and large self-discharge.

Method used

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  • Preparation method of ferric phosphate
  • Preparation method of ferric phosphate
  • Preparation method of ferric phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Dissolve ferrous sulfate (280.8g, 99-101%) in 1L of deionized water, add 6g of sulfuric acid, stir evenly, and filter the solution to remove insoluble matter.

[0026] Diammonium hydrogen phosphate (133.4 g, 99%) was dissolved in 0.5 L of deionized water, stirred evenly, and the solution was filtered to remove insoluble matter.

[0027] The above two solutions were mixed under rapid stirring, and the solution did not precipitate.

[0028] Hydrogen peroxide (78 g, 30%) was slowly added to the above mixture, the pH increased during the oxidation process, and a suspension of yellow-white precipitate was obtained.

[0029] Slowly raise the temperature of the solution to 80° C., keep it warm for 2.5 hours, wash and filter to obtain a light powdery white filter cake.

[0030] The filter cake was sintered in a muffle furnace at 350°C for 6 hours to obtain 140.2 grams of dry powder, which was ferric phosphate.

[0031] Material analysis is: Fe / P molar ratio 0.995, sulfur cont...

Embodiment 2

[0039] Dissolve ferrous sulfate (224.6g, 99-101%) in 1L of deionized water, stir evenly, and filter the solution to remove insoluble matter.

[0040] Dissolve trisodium phosphate (132.5 g, 99%) in 1 L of deionized water, stir evenly, and filter the solution to remove insoluble matter.

[0041] The above two solutions were mixed under rapid stirring; a blue ferrous phosphate precipitate was obtained.

[0042] Take hydrogen peroxide (92g, 30%) and slowly add the mixed solution.

[0043] Slowly add hydrogen peroxide to the ferrous phosphate suspension, and continue to stir rapidly to gradually oxidize to obtain pure ferric phosphate precipitation.

[0044] Add 12 g of sulfuric acid to this suspension and mix well.

[0045]After stirring slowly for 60 minutes, slowly raise the solution temperature to 85°, keep the temperature for 2.5 hours, filter and wash to obtain light pink dihydrate crystalline ferric phosphate.

[0046] The filter cake was sintered in a muffle furnace at 3...

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Abstract

The invention provides a preparation method of ferric phosphate. The preparation method comprises the following steps of: firstly adding acid to a ferrous salt solution to regulate a pH value; then uniformly mixing with a phosphate solution or/and a mixture of phosphoric acid and a phosphate; then adding an oxidizing agent to react to generate ferric phosphate. The preparation method of ferric phosphate, disclosed by the invention, well overcomes the defects of the traditional preparation method of ferric phosphate; the pH of an iron source is regulated before the iron source and a phosphorus source are mixed, so that a pre-estimated pH range can be reached without adding a pH regulating agent after the mixing, and the problem that impurities, such as Fe(OH)3, are generated because the alkaline pH regulating agent is locally excessive in the traditional method is prevented; no iron hydroxide is generated in the technical process, the obtained ferric phosphate is high in purity; high-quality ferric phosphate can be obtained after impurity ions are further removed subsequently, the purity exceeds 99.8%, the iron content is stabilized at 36.8%-37.2%, and the phosphate radical content is stabilized at 62.8%-63.2%.

Description

technical field [0001] The invention relates to a method for preparing iron phosphate, and the prepared material is mainly used for making battery materials. Background technique [0002] As a precursor of lithium iron phosphate, the positive electrode material of batteries, iron phosphate has obvious advantages and its usage continues to expand. The traditional method for preparing battery-grade iron phosphate is to use Fe 2+ After salt solution oxidation or directly with Fe 3+ The solution is mixed with phosphate, the pH of the solution is adjusted, a precipitate is formed, and the ferric phosphate product is obtained by washing, filtering and drying. In most of these preparation methods, when the pH regulator is mixed with iron phosphate, an irreversible side reaction occurs to generate hydroxide precipitation. As everyone knows, iron hydroxide is a typical hard-to-filter colloid, which endangers the quality of iron phosphate. After processing this type of iron phospha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 徐越峰宋海申张宝
Owner 徐越峰
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