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Preparation method of anhydrous iron phosphate nanoparticles

A nanoparticle, iron phosphate technology, applied in the preparation/purification of carbon, nanotechnology, nanotechnology, etc., can solve the problems of high energy consumption and excessive excess

Active Publication Date: 2020-07-07
黄冈林立新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, in this process, the molar ratio of phosphoric acid and iron powder is 2.5-3:1, and the excessive amount will bring about a long subsequent washing process; moreover, the reaction aqueous solution needs to be crystallized at 80-98°C, and the energy consumption is relatively high. big

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  • Preparation method of anhydrous iron phosphate nanoparticles
  • Preparation method of anhydrous iron phosphate nanoparticles
  • Preparation method of anhydrous iron phosphate nanoparticles

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 14.4236g concentration of 85wt% H 3 PO 4 The solution was added to 20 ml of deionized water and stirred to form a phosphoric acid solution. Add 2.7926g of Fe powder to the phosphoric acid solution, raise the temperature to 40°C, and stir for 0.5h. Add 2.5ml concentration of 30wt% H 2 o 2 (density 1.11g / ml) solution, continue stirring for 0.5h. Filter to obtain a tan filtrate. The obtained filter residue was dried and weighed, and the mass of the filter residue was 0.0514g, so the reaction degree of the iron powder in the first step was 98.15%. Add 70 ml of deionized water and 2.5 ml of 30 wt% H to the tan solution 2 o 2 The solution was stirred at room temperature for 1 h. Filter, wash, and dry to obtain light yellow powder. Make the SEM image of the light yellow powder, such as figure 1. The light yellow powder was placed in a muffle furnace, kept at 600°C for 6 hours, and 7.2480 g of light yellow powder was obtained after cooling. The calculated overall re...

Embodiment 2

[0036] 7.9553g concentration of 85wt% H 3 PO 4 The solution was added to 20 ml of deionized water and stirred to form a phosphoric acid solution. Add 1.6754g of Fe powder to the phosphoric acid solution, raise the temperature to 40°C, and stir for 0.5h. Add 1.5ml of 30wt% H 2 o 2 Solution, continue to stir for 0.5h. Filter to obtain a tan filtrate. Add 75 ml of deionized water and 1.5 ml of 30% HO to the tan solution 2 o 2 The solution was stirred at room temperature for 1 h. Filter, wash, and dry to obtain light yellow powder. Place the light yellow powder in a muffle furnace at 700°C for 6 hours, and obtain a light yellow powder after cooling. The X-ray diffraction pattern of the powder proved to be pure phase FePO in crystalline state (PDF NO.29-0715) 4 .

Embodiment 3

[0038] 20.2917g concentration of 85wt% H 3 PO 4 The solution was added to 20 ml of deionized water and stirred to form a phosphoric acid solution. Add 4.4680g Fe powder to the phosphoric acid solution, raise the temperature to 40°C, and stir for 0.5h. Add 1.6ml of 30wt% H 2 o 2 Solution, continue to stir for 0.5h. Filter to obtain a tan filtrate. Add 68 ml of deionized water and 4.1 ml of 30% HO to the tan solution 2 o 2 The solution was stirred at room temperature for 1 h. Filter, wash, and dry to obtain light yellow powder. Place the light yellow powder in a muffle furnace at 600°C for 6 hours, and obtain a light yellow powder after cooling. The X-ray diffraction pattern of the powder proved to be pure phase FePO in crystalline state (PDF NO.29-0715) 4 .

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Abstract

The invention provides a preparation method of anhydrous iron phosphate nanoparticles, which belongs to the technical field of inorganic synthesis. The preparation method comprises the following stepsof adding iron powder into a phosphoric acid solution, heating to about 40 DEG C, preserving heat, adding an oxidant, continuously preserving heat, and filtering to obtain a dark brown filtrate, adding an oxidant into the filtrate, and stirring at normal temperature, filtering, washing and drying to obtain faint yellow powder, and carrying out high-temperature treatment on the powder at 500-700 DEG C to obtain the anhydrous iron phosphate nanoparticles. In the preparation method, the oxidation of ferrous ions is completed at normal temperature, and iron phosphate does not need to be crystallized and aged, so that the cost for preparing iron phosphate is further reduced. In addition, the anhydrous iron phosphate obtained by the preparation method is of a micron secondary structure formed by agglomeration of nanoparticles, and the lithium iron phosphate obtained by lithiation of the anhydrous iron phosphate with the morphology is large in capacity and high in compaction density.

Description

technical field [0001] The invention relates to a method for preparing anhydrous iron phosphate nanoparticles, which belongs to the technical field of inorganic materials and also belongs to the technical field of energy materials. Background technique [0002] As a cathode material for lithium-ion batteries, lithium iron phosphate has high specific capacity, good safety, long cycle life, and good thermal stability. At the same time, it has a wide range of raw materials and low prices. It is a cathode material that coexists with ternary materials for a long time. At present, most of the industrial production of lithium iron phosphate uses the precursor synthesis method, that is, anhydrous iron phosphate (FePO 4 ) is used as an iron source and a phosphorus source at the same time, mixed with a lithium source and a carbon source, and obtained by a high-temperature solid-state method to obtain lithium iron phosphate coated with a carbon layer on the surface. In this preparatio...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01B25/45C01B32/05H01M4/36H01M4/58H01M4/62H01M10/0525B82Y30/00
CPCC01B25/375C01B25/45C01B32/05H01M4/366H01M4/5825H01M4/62H01M10/0525B82Y30/00C01P2006/82Y02E60/10
Inventor 张友祥马晓玲
Owner 黄冈林立新能源科技有限公司
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