Method for preparing high purity ferric phosphate using ferrous sulfate as by-product of white titanium pigment

A technology of high-purity phosphoric acid and ferrous sulfate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of unseen high-purity ferric phosphate, and achieve the effect of solving environmental pollution

Inactive Publication Date: 2009-09-16
GUANGXI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, no relevant literature and patents have been seen on the preparation of high-purity ferric phosphate with ferrous sulfate, a by-product of titanium dioxide.

Method used

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  • Method for preparing high purity ferric phosphate using ferrous sulfate as by-product of white titanium pigment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1 1. 1. 139g titanium dioxide byproduct ferrous sulfate heptahydrate is dissolved in 1kg water (equivalent to about 0.5mol L of ferrous sulfate concentration -1 ), filter to remove water-insoluble solid impurities such as sand and stones, then add 2.78g powdery sodium sulfide while stirring in the filtrate, continue to stir for 10 minutes after black precipitates appear in the solution, filter to remove black precipitates, and obtain pure ferrous sulfate solution. ②Add 60g of concentrated phosphoric acid to the pure ferrous sulfate solution, stir evenly, adjust the pH of the solution to 2 with ammonia water, add 60g of 30% hydrogen peroxide dropwise to the solution under stirring, react at 25°C for 6 hours, after the reaction is complete, filter , washed the filter cake with water for 3 times, and dried the filter cake at 105° C. to obtain white iron phosphate powder. The Fe content of the obtained product is 29.42%, and the purity is 99.5%.

Embodiment 2

[0020] Embodiment 2 1. 278g titanium dioxide by-product ferrous sulfate heptahydrate is dissolved in 1kg water (equivalent to about 1mol L of ferrous sulfate concentration -1 ), filter to remove water-insoluble solid impurities such as sand and stones, then add 5.56g powdery sodium sulfide while stirring in the filtrate, continue to stir for 10 minutes after black precipitates appear in the solution, filter to remove black precipitates, and obtain pure ferrous sulfate solution. ②Add 120g of concentrated phosphoric acid to the pure ferrous sulfate solution, stir evenly, adjust the pH of the solution to 1.8 with sodium hydroxide, feed oxygen into the solution while stirring, and react at 40°C for 10 hours. After the reaction is complete, filter, The filter cake was washed with water for 3 times, and the filter cake was dried at 105° C. to obtain white iron phosphate powder. The Fe content of the product obtained is 29.43%, and the purity is 99.5%.

Embodiment 3

[0021] Embodiment 3 1. 834g titanium dioxide by-product ferrous sulfate heptahydrate is dissolved in 1kg water (equivalent to about 3mol L of ferrous sulfate concentration -1), filter to remove water-insoluble solid impurities such as sand and stones, then add 8.34g powdery sodium sulfide while stirring in the filtrate, continue to stir for 10 minutes after black precipitates appear in the solution, filter to remove black precipitates, and obtain pure ferrous sulfate solution. ②Add 350g of concentrated phosphoric acid to the pure ferrous sulfate solution, stir evenly, adjust the pH of the solution to 2.5 with potassium hydroxide aqueous solution, pass air into the solution while stirring, and react at 70°C for 10 hours, after the reaction is complete, filter , washed the filter cake with water for 3 times, and dried the filter cake at 105° C. to obtain white iron phosphate powder. The Fe content of the product obtained is 29.38%, and the purity is 99.5%.

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Abstract

The invention relates to a preparation method of pure ferric phosphate, characterized in that: iron vitriol, phosphorus source as by-product of white titanium pigment are used as reactant and purificant and oxidant are added into the reactant and the reaction temperature is controlled at 25-100 DEG C and the reaction time is 0.5-10 hours, thus white ferric phosphate powder (FePO[4]2-4H[2]O) with 2-4 crystal water is obtained. The technological process has features of simple process, low production cost, high product purity, increased added value of ferrous sulfate as by-product of white titanium pigment and the product can be used as ceramic metal glaze-color glaze material and raw material for producing lithium iron phosphate as lithium ionization cell anode material.

Description

Technical field: [0001] The invention relates to a production method of ferric phosphate, in particular to a method for preparing high-purity ferric phosphate from titanium dioxide by-product ferrous sulfate, belonging to the field of inorganic materials. Background technique: [0002] In the process of producing titanium dioxide by the sulfuric acid method, about 3.5 to 4 tons of by-product green vitriol (ferrous sulfate heptahydrate, molecular formula FeSO 4 ·7H 2 O). At present, the production of titanium dioxide in my country mainly adopts the sulfuric acid method, which produces a large amount of by-products vitriol every year. Some of these by-products are used for feed additives, water purifiers, and agricultural fertilizers, and some of them are used for the production of iron oxide pigments (such as iron red, iron yellow, Iron blue, iron black), etc., but still a large part cannot be effectively utilized. In the open literature about titanium dioxide by-product fe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 龚福忠阮恒徐运贵周立亚
Owner GUANGXI UNIV
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