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Preparation of high pure ferric phosphate

A technology of iron orthophosphate and iron phosphate, which is applied in the direction of phosphate, phosphorus oxyacid, etc., can solve the problems of low product purity, yellowish color of iron phosphate, and high production cost, and achieve simple process operation, white product color, The effect of low production cost

Active Publication Date: 2008-12-24
湖南海利锂电科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that it has strict requirements on production equipment and serious pollution.
Another method is to acidify ferrous sulfate with phosphoric acid and react with sodium chlorate to generate ferric dihydrogen phosphate solution, then use sodium hydroxide to adjust the pH value to about 2, and ferric phosphate will precipitate out. The disadvantage of this method is that phosphoric acid and hydrogen The consumption of sodium oxide is large, and the production cost is very high
In addition, there is a direct reaction between sodium phosphate and ferric sulfate to generate ferric phosphate under the condition that the pH value is less than 2. The ferric phosphate produced by this method is yellowish in color, obviously has iron hydroxide impurities, and the product purity is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Dissolve 142.5g of ferrous sulfate heptahydrate with water to make about 400ml of solution, add 27g of concentrated sulfuric acid, add 40g of hydrogen peroxide at 25°C, and oxidize for 30 minutes to obtain ferric sulfate solution for later use.

[0008] Dissolve 190g of trisodium phosphate dodecahydrate in water to make about 800ml of solution. Stir the above ferric sulfate solution and raise the temperature to 75°C, then add the sodium phosphate solution dropwise into the ferric sulfate solution, and keep it warm for 30 minutes after the addition is complete. Filter and wash to pH 4-5.

[0009] Weigh 60g of phosphoric acid with water to make about 800ml of phosphoric acid solution, beat and stir the above-mentioned filtered and washed materials evenly, and react at 90°C for 0.5 hours. Filter and wash until the pH value is about 5, and dry to obtain a white powder product with a Fe content of 28.91% and a purity of 99.62% (dry basis).

Embodiment 2

[0011] Dissolve 100g of ferrous chloride tetrahydrate with water to make about 400ml of solution, add 60g of concentrated hydrochloric acid, add 40g of hydrogen peroxide at 10°C, and oxidize for 120 minutes to obtain ferric chloride solution, which is set aside.

[0012] Dissolve 180g of disodium hydrogen phosphate dodecahydrate in water to make about 800ml of solution. Stir the above ferric chloride solution and raise the temperature to 30°C, then add the disodium hydrogen phosphate solution dropwise into the ferric chloride solution, and keep the reaction for 120 minutes after the addition is completed. Filter and wash to pH 4-5.

[0013] Weigh 60g of phosphoric acid with water to make about 800ml of phosphoric acid solution, beat and stir the above-mentioned filtered and washed materials evenly, and react at 60°C for 8 hours. Filter and wash to about pH 5, and dry to obtain a white powder product with a Fe content of 28.73% and a purity of 99.57% (dry basis).

Embodiment 3

[0015] Dissolve 142.5g of ferrous sulfate heptahydrate in water to make about 400ml of solution, add 27g of concentrated sulfuric acid, add 12g of sodium chlorate at 90°C, and oxidize for 10 minutes to obtain ferric sulfate solution for later use.

[0016] Dissolve 135g of potassium phosphate trihydrate in water to make about 800ml of solution. Stir the above ferric sulfate solution and maintain the temperature at about 10°C, then add the potassium phosphate solution dropwise into the ferric sulfate solution, and keep it warm for 60 minutes after the addition is complete. Filter and wash to pH 4-5.

[0017] Weigh 60g of phosphoric acid water to make about 800ml of phosphoric acid solution, beat and stir the above-mentioned filtered and washed materials evenly, and react at 40°C for 10 hours. Filter and wash to about pH 5, and dry to obtain a white powder product with an Fe content of 28.85% and a purity of 99.53% (dry basis).

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PUM

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Abstract

The invention discloses a preparation method of ferric orthophosphate which is characterized by oxidizing the ferrite solution into ferric salt solution by oxidant under acid condition, then reacting the phosphate or monohydric phosphate with the ferric salt to obtain basic ferric phosphate containing ferric hydroxide, treating the crude product of basic ferric phosphate using phosphoric acid with a concentration of 0.65 M so as to convert the ferric hydroxide thereof into ferric orthophosphate, then separating the solid and liquid of the product and washing, drying the product to obtain white product of ferric orthophosphate with a purity lager than 99%. The preparation method can be widely used in the preparation of paint, pigment, feed additive, catalyst and new battery materials, especially for the production of lithium iron phosphate for lithium ion battery anode material.

Description

technical field [0001] The invention relates to the technical field of preparing ferric orthophosphate. Background technique [0002] Ferric orthophosphate is a non-toxic white antirust pigment, which can replace toxic red lead, lead chrome yellow, zinc chrome yellow, etc. in paints. It is also a very good feed and food additive, catalyst, and can also be used as a new battery positive electrode material, and is also an excellent raw material for preparing lithium iron phosphate, a lithium ion battery positive electrode material. [0003] There are many ways to synthesize ferric orthophosphate, the most traditional one is to react ferric nitrate with phosphoric acid, then decompose the reaction solution at high temperature to decompose nitric acid to obtain white ferric orthophosphate product. The disadvantage of this method is that it has strict requirements on production equipment and serious pollution. Another method is to acidify ferrous sulfate with phosphoric acid an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/26
Inventor 彭爱国贺周初余长艳肖伟刘昱霖
Owner 湖南海利锂电科技有限公司
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