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Technology for preparing iron phosphate through hydrolytic method

A technology of iron phosphate and hydrolysis method, applied in phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high energy consumption, ammonia nitrogen pollution, etc. Effect

Active Publication Date: 2015-09-30
徐源庆
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technology of the present invention aims to solve the problems of high energy consumption and ammonia nitrogen pollution in the above-mentioned prior art. It does not use alkaline substances such as sodium hydroxide or ammonia to adjust the pH value so that phosphate and ferric iron are precipitated, but Use the dilution method combined with the temperature control of the solution to combine the ferric iron with the phosphate to precipitate the primary ferric phosphate precipitate (the hydrolyzate containing a certain amount of iron), and then convert the impurities in the primary ferric phosphate into pure ferric phosphate in the phosphoric acid solution. ferric phosphate

Method used

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  • Technology for preparing iron phosphate through hydrolytic method

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Experimental program
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Effect test

Embodiment 1

[0021] The first step is oxidation. Get 278g (1mol) ferrous sulfate heptahydrate (100%) into a beaker, add 600ml of water to dissolve, then take 115.3g (1mol) of phosphoric acid with a mass percentage of 85%, add it to the ferrous sulfate solution, stir evenly, and , 90ml (0.8mol) of 27.5% hydrogen peroxide was added dropwise in ten minutes to oxidize ferrous iron into ferric iron. After adding the hydrogen peroxide, add water to make the volume of the solution 1 L. Heat the above materials to 90-95°C;

[0022] The second step is hydrolysis. In a reaction kettle with a capacity of 20L, add 10L of deionized water and heat to 90-95°C. The solution obtained in the first step is quickly added into the hot water in the second step under stirring, and the concentration of the hydrolyzate is 0.09 mol / L (calculated as Fe). Due to the rapid decrease in pH value, hydrolysis occurs, resulting in iron phosphate precipitation;

[0023] The third step is separation. Immediately while ...

Embodiment 2

[0027] The second step hydrolysis water consumption in embodiment 1 is brought up to 15L, and the concentration of hydrolyzate is 0.03mol / L (calculated as Fe), other is with embodiment 1. The results are shown in Table 1.

Embodiment 3

[0029] The volume of the water of the dissolved material in the first step in Example 1 is doubled. After adding the hydrogen peroxide, add water to make the volume of the solution 2L, that is, the amount of raw materials remains unchanged and the volume increases to 2L. Others are the same as in Example 1. . The concentration of the hydrolyzate is 0.08mol / L (calculated as Fe), and the results are shown in Table 1.

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Abstract

The invention provides a technology for preparing iron phosphate through a hydrolytic method. The technology for preparing the iron phosphate through the hydrolytic method comprises the steps that 1 aqueous solution of the iron phosphate and phosphoric acid are added, an oxidizing agent is added while stirring is conducted, and the temperature is heated to 90 to 95 DEG C; 2 deionized water is added in a hydrolyzing tank, then the temperature is heated to 90 to 95 DEG C, the solution obtained in the step 1 is totally added into the hot water while stirring is conducted, and sediment of the iron phosphate is generated; 3 the mixing solution obtained in the step 2 is filtered immediately, and primary iron phosphate product sediment A and mother solution A are obtained; 4 according to inversion, all the sediment A obtained in the step 3 are added into 0.5 mol / L iron phosphate solution and is stirred, the temperature is heated to 90 to 95 DEG C, the temperature is maintained for 1 hour, filtering is conducted, and sediment B and mother solution B are obtained. The mother solution B acts on the step 4 of a product in a next batch, a filter cake is pulped and washed by the deionized water in the normal temperature, drying in 100 to 120 DEG C is conducted, and the product is obtained. The technology for preparing the iron phosphate through the hydrolytic method has the advantages that water treatment in the technology is simplified and circulative, and lowering the cost is facilitated.

Description

technical field [0001] The invention relates to a production process method of iron phosphate, in particular to a preparation method of iron phosphate used for synthesizing lithium iron phosphate, a positive electrode material of a lithium ion battery. technical background [0002] Iron phosphate (FePO 4 2H 2 O) is a precursor for the manufacture of lithium iron phosphate, the cathode material for lithium-ion batteries. Cost reduction, energy saving and consumption reduction are the key to the popularization and application of iron phosphate and lithium iron phosphate in the fields of electric vehicles and energy storage. The main raw materials for industrial production of ferric phosphate are iron source (ferric salt or ferric salt obtained by oxidation of ferrous salt), phosphorus source (phosphoric acid) and alkaline substance (sodium hydroxide or ammonia water). The iron source (ferric iron salt or ferrous iron source) can be a raw material of analytically pure grade,...

Claims

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Application Information

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IPC IPC(8): C01B25/37
Inventor 欧秀芹郅晓科时志翔赵南南梁广川
Owner 徐源庆
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