Method for synthesizing ferric phosphate material

A technology of ferric orthophosphate and synthesis method, which is applied in the direction of phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of nanometer ferric phosphate growth, responsible synthesis process, large specific surface area, etc., and achieve batch stability and sintering Short time, the effect of overcoming capacity reduction

Inactive Publication Date: 2011-08-17
天津恒普科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as CN101693531A, CN101837966A, etc., which cause problems such as large specific surface area, difficult processing, and responsible synthesis process
In particular, there are problems such as nano-iron phosphate will still grow into micron-sized materials during subsequent thermal processing.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The synthetic method of ferric orthophosphate material, after mixing with 1 kilogram of 20# machine oils and 1 kilogram of dodecylbenzenesulfonic acid, dissolve in 8 kilograms of distilled water. At this point the weight of oil and surfactant accounts for 5% of the total weight of the solution. Stir with a mixer at 1000 rpm for 1 hour to form an emulsion. Sulfuric acid was added to adjust the pH value of the solution to less than 1. Then add 0.115 kg of monoammonium phosphate (0.1M), and then add 0.243 kg of ferric chloride (0.15M), and stir well. At this time, the molar ratio of phosphorus to iron atoms is 1:1.5. Gradually add sodium hydroxide to adjust the pH to around 4. At this point a large amount of precipitate appeared. The precipitate was filtered out, dried at 120°C for 1 hour, and then calcined at 800°C for 1 hour to obtain iron phosphate microspheres with a hollow / shell structure. The average diameter is about 10 microns.

Embodiment 2

[0029] The synthetic method of ferric orthophosphate material, after mixing with 1g of oleic acid and 9g of Tween 80, dissolve in 990g of distilled water. At this point the weight of oil and surfactant accounts for 0.1% of the total weight of the solution. Stir with a mixer at 1000 rpm for 10 hours to form an emulsion. Sulfuric acid was added to adjust the pH value of the solution to less than 1. Then add 0.82 kg of sodium phosphate (5M), and then add 0.605 kg of ferric nitrate (2.5M), and stir well. At this time, the molar ratio of phosphorus to iron atoms is 1:0.5. Add ammonia gradually to adjust the pH to around 4. At this point a large amount of precipitate appeared. The precipitate was filtered out, dried at 100°C for 10 hours, and calcined at 400°C for 10 hours to obtain iron phosphate microspheres with a hollow / shell structure. The average diameter of iron orthophosphate microspheres is about 3 microns.

Embodiment 3

[0031] The synthetic method of ferric orthophosphate material, after mixing with 10g oleic acid and 50g flat plus O, dissolve in 5.94 kg of distilled water. At this point the weight of oil and surfactant accounts for 1% of the total weight of the solution. Stir with a mixer at 1500 rpm for 2 hours to form an emulsion. Sulfuric acid was added to adjust the pH value of the solution to less than 1. Then add 1.212 kg of potassium phosphate (1M), then add 1.169 kg of iron sulfate (1M), and stir well. At this time, the molar ratio of phosphorus and iron atoms is 1:1, and gradually add lithium hydroxide to adjust the pH value to about 4.5. At this point a large amount of precipitate appeared. The precipitate was filtered out, dried at 110°C for 2 hours, and then calcined at 550°C for 4 hours to obtain iron phosphate microspheres with a hollow / shell structure. The average diameter of iron orthophosphate microspheres is about 8 microns.

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Abstract

The invention relates to a method for synthesizing a ferric phosphate material, belonging to the technical field of lithium ion cathode materials. The method for synthesizing the ferric phosphate material comprises the following steps of: (1) manufacturing a hollow spherical template: stirring oil with carbon hydrogen bonds and a water-soluble surfactant free of metal ions for 0.1-10 h in a water solution to form an emulsion, wherein the weight ratio of the oil to the surfactant is 1:(1-9), and the total weight of the oil and the surfactant accounts for 0.1-5% of the solution; (2) precipitating ferric phosphate: adjusting the pH value of an acid solution containing phosphates and ferric salts by using the emulsion to form ferric phosphate precipitate, wherein the precipitate is adhered to an emulsion microsphere to form a structure of which the exterior is ferric phosphate and the kernel is the emulsion microsphere; and (3) processing the ferric phosphate microsphere: filtering and drying the ferric phosphate microsphere, calcining the ferric phosphate microsphere at high temperature to form a hollow/shell structure microsphere ferric phosphate material. The method provided by the invention has the advantages of simple process, operation convenience, stable ferric phosphate microsphere, large rate discharge capacity and low temperature capacity and the like.

Description

technical field [0001] The invention belongs to the technical field of lithium ion cathode materials, in particular to a method for synthesizing ferric orthophosphate materials. Background technique [0002] Currently, iron orthophosphate (FePO 4 ) is a commonly used phosphate, which can be used in food additives, ceramic additives and other fields. High-purity ferric orthophosphate can be used to manufacture cathode materials for lithium-ion batteries, greatly enhancing its application value. [0003] Traditional iron phosphate materials are synthesized by chemical precipitation by reacting phosphate and iron salt in solution. The material manufactured by the traditional process is formed by direct precipitation, and the subsequent precipitation is attached to the surface of the previous precipitation to form a dense structure. Patent CN100588611C prepares iron phosphate by reacting soluble iron salt and phosphoric acid. Highly active iron phosphate materials can be pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 胡学仁
Owner 天津恒普科技发展有限公司
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