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Preparation method of high-purity battery-grade anhydrous iron phosphate

An anhydrous phosphoric acid, battery-level technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of sulfuric acid environmental pollution, environmental protection requirements, unsafe production process, etc., to achieve recyclable products Utilization, stable response, and low input cost

Inactive Publication Date: 2016-10-26
HEBEI ANZ NEW ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are basically two types of methods for preparing iron phosphate in the industry. One is to use elemental iron powder and sulfuric acid to react.
The second type is to use ferrous solution to oxidize and react with ammonium hydrogen phosphate or phosphoric acid and ammonia water for heating. During the reaction, ammonia gas is released, and there are ammonia nitrogen substances in the discharge, which also faces environmental problems.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Dissolve 38.44g of industrial 85% concentrated phosphoric acid in 0.8kg of water to make an acid solution, adjust the amount of water appropriately and control the pH range of the acid solution to 1.2-1.8;

[0027] 2. Add 278g of ferrous sulfate heptahydrate to the above acid solution, stir evenly, slowly add 56.67g of 30% hydrogen peroxide into the solution for oxidation, and the temperature range is 35°C to 50°C;

[0028] 3. Add 253g of sodium phosphate dodecahydrate to 1.4kg of water to form a sodium phosphate solution, and slowly add it to the above solution, white precipitate will appear in the reaction, and continue to heat up to 50-90°C for 2-4 hours;

[0029] 4. After washing and filtering the above white precipitate, put it into an atmosphere furnace and heat it to 550°C±10°C for dehydration. The precipitate after dehydration is iron phosphate powder, and the cleaning liquid crystallizes and is reused.

Embodiment 2

[0031] 1. Dissolve 19.22g of industrial 85% phosphoric acid in 0.4kg of water to make an acid solution, adjust the amount of water appropriately and control the pH range of the acid solution to 1.2-1.8;

[0032] 2. Add 139g ferrous sulfate heptahydrate to the above acid solution and stir evenly;

[0033] 3. Add 126.67g of sodium phosphate dodecahydrate to 0.7kg of water to form a sodium phosphate solution, and slowly add it to the above solution;

[0034] 4. Then slowly add 28.3g of 30% hydrogen peroxide to the solution for oxidation, and a white precipitate will appear in the reaction, and heat up to 50-90°C for 2-4 hours;

[0035] 5. After cleaning and filtering the above white precipitate, put it into an atmosphere furnace and heat it to 550°C±10°C for dehydration. The precipitate after dehydration is iron phosphate powder, and the cleaning liquid crystallizes and is reused.

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Abstract

The invention discloses a preparation method of high-purity battery-grade anhydrous iron phosphate; the method includes the following steps: firstly, preparing a phosphoric acid solution, dissolving ferrous salt slowly in an acid solution, then adding an oxidant, carrying out oxidation, and finally, slowly adding a sodium phosphate solution, or firstly adding the sodium phosphate solution, then slowly adding the oxidant, carrying out oxidation, then heating, and carrying out a reaction to obtain a precipitate, namely iron phosphate dihydrate; and cleaning the iron phosphate dihydrate, filtering, dehydrating, and thus obtaining anhydrous ferric phosphate. The washing discharge solution is a sodium sulfate (mirabilite) solution, and is recycled and crystallized to form an additional solid product.

Description

technical field [0001] The invention belongs to the field of new energy battery materials, and in particular relates to a method for preparing battery-grade anhydrous iron phosphate. Background technique [0002] With the vigorous development of the new energy industry and power batteries, the industrialization of the cathode material lithium iron phosphate and the upstream material iron phosphate is also very hot. The stable industrial production of iron phosphate shows better electrochemical performance as lithium iron phosphate cathode material is gradually replacing ferrous oxalate and becoming the mainstream framework material. At present, there are basically two types of methods for preparing iron phosphate in the industry. One is to use elemental iron powder and sulfuric acid to react. . The second type is to use ferrous solution to oxidize and react with ammonium hydrogen phosphate or phosphoric acid and ammonia water for heating. During the reaction, ammonia gas i...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/375C01P2006/80
Inventor 吕霄李民吕宏白皓吴晓鹏
Owner HEBEI ANZ NEW ENERGY TECH