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Nano lithium iron phosphate and preparation method thereof

A nano-iron phosphate, ferric salt technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of irregular iron phosphate particles, poor performance of lithium iron phosphate, low tap density, etc. Achieve the effect of short hydrothermal time, shortened sample preparation time and high tap density

Active Publication Date: 2020-06-30
GUANGDONG BRUNP RECYCLING TECH +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production method of battery-grade lithium iron phosphate precursor iron phosphate is to oxidize ferrous ions to ferric ions, then directly mix it with phosphate, adjust the pH and then precipitate to obtain iron phosphate products. The iron phosphate obtained by this method is not Regular and large particles, low tap density, the performance of lithium iron phosphate directly prepared as a precursor is not good

Method used

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  • Nano lithium iron phosphate and preparation method thereof
  • Nano lithium iron phosphate and preparation method thereof
  • Nano lithium iron phosphate and preparation method thereof

Examples

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Effect test

Embodiment 1

[0038] A preparation method of nano iron phosphate, comprising the following steps:

[0039] (1) Weigh ferric chloride and ammonium phosphate in equimolar amounts, place them in a 50mL microwave digestion tank, stir for 10min and then ultrasonicate for 10min to obtain solution A;

[0040] (2) adding sodium dodecylbenzenesulfonate of ferric chloride mass 1% to solution A to obtain solution B;

[0041] (3) Stir the solution B for 30 minutes, then sonicate it for 30 minutes, place it in a microwave digestion apparatus, set the temperature at 110°C, and take it out for 8 minutes, and take it out after cooling to room temperature to obtain solid A;

[0042] (4) After several times of suction filtration with deionized water, put it in an oven and dry it at 60°C for 2 hours. After drying, place it in a tube furnace for calcination to improve the crystallinity of the material. After 1 hour, nitrogen gas was introduced as a protective gas during the calcination process, and then nanom...

Embodiment 2

[0045] A preparation method of nano iron phosphate, comprising the following steps:

[0046] (1) Weigh ferric chloride and ammonium phosphate in equimolar amounts, place them in a 50mL microwave digestion tank, stir for 10min and then ultrasonicate for 10min to obtain solution A;

[0047] (2) adding sodium dodecylbenzenesulfonate of ferric chloride mass 1% to solution A to obtain solution B;

[0048] (3) Stir the solution B for 30 minutes, then sonicate it for 30 minutes, place it in a microwave digestion apparatus, set the temperature at 90°C for 8 minutes, take it out after cooling to room temperature, and obtain solid A;

[0049] (4) Suction filter solid A several times with deionized water and dry it in an oven at 60°C for 2 hours. After drying, place it in a tube furnace for calcination to improve the crystallinity of the material. °C, time 1h, nitrogen gas is passed as a protective gas during the calcination process, and then nanometer iron phosphate is obtained.

[00...

Embodiment 3

[0052] A preparation method of nano iron phosphate, comprising the following steps:

[0053] (1) Weigh ferric chloride and ammonium phosphate in equimolar amounts, place them in a 50mL microwave digestion tank, stir for 10min and then ultrasonicate for 10min to obtain solution A;

[0054] (2) adding sodium dodecylbenzenesulfonate of ferric chloride mass 1% to solution A to obtain solution B;

[0055] (3) Stir the solution B for 30 minutes, then sonicate it for 30 minutes, place it in a microwave digestion apparatus, set the temperature at 130°C, and take it out for 8 minutes, and take it out after cooling to room temperature to obtain solid A;

[0056] (4) Suction filter solid A several times with deionized water and dry it in an oven at 60°C for 2 hours. After drying, place it in a tube furnace for calcination to improve the crystallinity of the material. °C, time 1h, nitrogen gas is passed as a protective gas during the calcination process, and then nanometer iron phosphate...

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Abstract

The invention belongs to the field of material chemistry, and discloses a preparation method of nano iron phosphate, which comprises the following steps: (1) adding a ferric salt and a phosphate intowater to obtain a solution A; (2) adding a surfactant into the solution A to obtain a solution B; (3) stirring the solution B, carrying out ultrasonic treatment, and carrying out a microwave hydrothermal reaction in a microwave digestion instrument to obtain a solid C; and (4) drying and calcining the solid C to obtain the nano iron phosphate. A microwave hydrothermal method is adopted, the methodhas the advantages of being high in heating speed, uniform in heating, free of temperature gradient and the like, a conventional hydrothermal reaction needs 2-8 h, microwave hydrothermal reaction only needs 3-15 min, and the sample preparation time is greatly shortened. The iron phosphate prepared by the invention is nanoscale, has the particle size of 20-30nm, uniform particle size, no agglomeration phenomenon and high tap density, can be used as a precursor of battery-grade lithium iron phosphate, and has the advantages of simple preparation process, high production efficiency, high productpurity and good dispersion performance.

Description

technical field [0001] The invention belongs to the field of material chemistry, and in particular relates to a nano-lithium iron phosphate and a preparation method thereof. Background technique [0002] Ferric phosphate is an important chemical raw material. It is widely used in steel, wastewater treatment, food additives, ceramic glass and other fields due to its low price, environmental friendliness and abundant resources. In recent years, with the rapid development of electric vehicles, lithium iron phosphate has been widely used as a reliable cathode material for lithium-ion batteries, and iron phosphate has also been widely used as a precursor for the synthesis of lithium iron phosphate. High-purity nano Iron phosphate is of great significance to the synthesis of lithium iron phosphate with excellent performance. [0003] The existing ferric phosphate synthesis methods include high-temperature roasting method, co-precipitation method and sol-gel method. The tradition...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58B82Y30/00H01M10/0525
CPCC01B25/45H01M4/5825B82Y30/00C01P2004/03C01P2004/64C01P2006/80C01P2006/11C01P2004/32H01M10/0525Y02E60/10
Inventor 杜少林谢英豪余海军张学梅明帮来候彭
Owner GUANGDONG BRUNP RECYCLING TECH
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