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Method for preparing iron phosphate with micro/nano structure

A micro-nano structure, iron phosphate technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of large particle size, equipment requirements, low reactivity, etc. The effect of control and simple process

Active Publication Date: 2011-04-13
河南省净寰新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned two kinds of iron phosphate industrial production methods all need to react at high temperature, have requirements for equipment, and high energy consumption, high production cost, and the iron phosphate obtained by the above-mentioned method has the following disadvantages: one is completely or partially crystalline, The reaction activity is not high; the second is that the particle size is large and the distribution is uneven, resulting in difficulties in the insertion and diffusion of lithium ions in the lattice, and poor electrochemical performance
There is no report on the preparation method of ferric phosphate with micro-nano structure

Method used

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  • Method for preparing iron phosphate with micro/nano structure
  • Method for preparing iron phosphate with micro/nano structure

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Measure 1000 grams of 10wt% ferrous sulfate solution and 80 grams of 85wt% phosphoric acid solution respectively, add them to the reactor, add 27wt% hydrogen peroxide, and after 3 hours, add 86 grams of polyvinyl alcohol PVA1788, heat up to 50 ° C, turbulent flow After circulating for 20 minutes, add 5wt% sodium hydroxide solution within 15 minutes and control the pH value to 2.1; after adding alkali, continue to circulate in turbulent flow for 30 minutes, and then stand and age for 120 minutes. Filter, wash with deionized water at 50°C for 3 times, dry at 120°C for 10 hours, and then process at 300°C to obtain 2 micron iron phosphate clusters.

Embodiment 2

[0019] Measure 500 grams of 20wt% ferrous sulfate solution and 80 grams of 85wt% phosphoric acid solution respectively, add them to the reactor, and let air flow in until the solution turns brown. After 5 hours, add 17 grams of polyoxyethylene ether AEO-9 , the temperature was raised to 90°C, after turbulent circulation for 60 minutes, 15wt% sodium hydroxide solution was added within 40 minutes and the pH value was controlled to 3.0; after adding alkali, the turbulent circulation was continued for 60 minutes, and then left to age for 200 minutes. Filter, wash with deionized water at 50°C for three times, dry at 120°C for 10 hours, and then process at 500°C to obtain iron phosphate clusters with a diameter of 500 nm.

Embodiment 3

[0021] Measure 1000 grams of 25wt% ferrous sulfate solution and 190 grams of 85wt% phosphoric acid solution respectively, add them to the reactor, and feed oxygen until the solution turns brown. After 4 hours, add 95 grams of polyoxyethylene ether AEO-9 , heat up to 70°C, after turbulent circulation for 40 minutes, add 20wt% sodium hydroxide solution within 90 minutes and control the pH value to 3.5; Filter, wash with deionized water at 50°C for three times, dry at 120°C for 10 hours, and then process at 600°C to obtain 200nm iron phosphate clusters.

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Abstract

The invention discloses a method for preparing iron phosphate with a micro / nano structure. The method comprises the following steps of: guiding solution of ferrous sulfate, phosphoric acid and an oxidant into a reaction container respectively; performing oxidation reaction for 2 to 5 hours and then adding a water-soluble nonionic surfactant in an amount which is 10 to 0.05 weight percent of the total amount of the ferrous sulfate and the phosphoric acid; heating to the temperature of between 50 and 100 DEG C; performing turbulent circulation for 20 to 60 minutes, then adding 5 to 20 weight percent of solution of sodium hydroxide and controlling pH of a reaction system to be 2.0 to 4.5 on line; after alkali is added, continuously performing the turbulent circulation for 20 to 60 minutes, standing and aging for 120 to 600 minutes and separating; and washing a product with pure water until the pH is 5 to 7, drying the product and performing heat treatment on the surface of the product. By the method, a near-spherical iron phosphate nanocluster with high fluidity and dispersibility and controllable specific surface area is prepared; the size of the primary particles is less than 100nm; the size of cluster particles is regulated and controlled within a range of between 200nm and 2 microns; and the product can be used for preparing lithium iron phosphate serving as a positive material of a lithium ion battery and used in the fields such as food additives, biomedicine and the like.

Description

technical field [0001] The invention relates to a method for preparing iron phosphate with a micro-nano structure, belonging to the technical field of inorganic materials. Background technique [0002] In order to meet the huge demand for mobile new energy, the development of secondary batteries with excellent performance, safety, low price, and environmental friendliness has attracted widespread attention. Currently LiFePO 4 and FePO 4 As a positive electrode material for power lithium-ion batteries, it is recognized as the best choice. Studies have shown that as a synthetic LiFePO 4 The main raw material FePO 4 , its structure, morphology and particle size will directly affect the product LiFePO 4 structure and performance. [0003] At present, most of the industrial production methods of ferric phosphate are synthesized by high-temperature reaction of ferrite and phosphate, or by reaction of ferric chloride and phosphoric acid at a certain temperature. The above-men...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 袁良杰艾常春何必寅蒋昌忠孙聚堂
Owner 河南省净寰新能源科技有限公司
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