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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  • Summary
  • 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

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

Experimental program
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Example Embodiment

[0037] Example 1

[0038] A preparation method of nanometer iron phosphate includes the following steps:

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

[0040] (2) Add sodium dodecylbenzene sulfonate with 1% ferric chloride mass to solution A to obtain solution B;

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

[0042] (4) After suction filtration with deionized water for several times, it is dried in an oven at a baking temperature of 60°C for 2 hours. After drying, it is calcined in a tube furnace to increase the crystallinity of the material. The calcining temperature is 300°C. After 1 h, nitrogen was introduced as a protective gas during the c...

Example Embodiment

[0044] Example 2

[0045] A preparation method of nanometer iron phosphate includes the following steps:

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

[0047] (2) Add sodium dodecylbenzene sulfonate with 1% ferric chloride mass to solution A to obtain solution B;

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

[0049] (4) Use deionized water to filter the solid A several times and place it in an oven for drying at a baking temperature of 60°C for 2 hours. After drying, place it in a tube furnace for calcination to increase the crystallinity of the material. The calcination temperature is 300. ℃, time 1h, nitrogen as a protective gas during the calcination proce...

Example Embodiment

[0051] Example 3

[0052] A preparation method of nanometer iron phosphate includes the following steps:

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

[0054] (2) Add sodium dodecylbenzene sulfonate with 1% ferric chloride mass to solution A to obtain solution B;

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

[0056] (4) Use deionized water to filter the solid A several times and place it in an oven for drying at a baking temperature of 60°C for 2 hours. After drying, place it in a tube furnace for calcination to increase the crystallinity of the material. The calcination temperature is 300. ℃, time 1h, nitrogen as a protective gas during the ca...

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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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