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A low-cost high-purity green nanocrystalline battery grade anhydrous fepo 4 the preparation method of

A green and environmentally friendly nanocrystalline technology, applied in nanotechnology, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of equipment investment, high cost of sewage treatment, complicated co-precipitation process, large investment in equipment, etc., and achieve low price , fine workmanship and small investment in equipment

Active Publication Date: 2020-08-25
深圳中芯能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the vast majority of iron phosphate on the market is based on ferrous sulfate (FeSO 4 ·7H 2 O), phosphate, PH regulator, oxidant, etc. are prepared as raw materials by co-precipitation, and need to be filtered and washed with a large amount of water. The requirements for water treatment after suction and washing are very high, so the investment in equipment is very high. , the cost of sewage treatment is also high
The co-precipitation process is more complicated, there are more supporting production equipment, and the equipment capital investment is large, so the cost is relatively high

Method used

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  • A low-cost high-purity green nanocrystalline battery grade anhydrous fepo <sub>4</sub> the preparation method of
  • A low-cost high-purity green nanocrystalline battery grade anhydrous fepo <sub>4</sub> the preparation method of
  • A low-cost high-purity green nanocrystalline battery grade anhydrous fepo <sub>4</sub> the preparation method of

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A low-cost, high-purity, green and environmentally friendly nanocrystalline battery-grade anhydrous FePO 4 The preparation method, described method comprises the following steps:

[0034] (1) 115 grams of 85% H 3 PO 4 1. Dissolve 60g of oxalic acid in pure water, add 56g of Fe powder with a particle size of less than 100μm under nitrogen protection, stir and soak for 20 hours, then add the soaked raw materials to a high-energy mill and grind for 45 hours. Stirring speed: 450 rpm, nitrogen volume 90ml per minute.

[0035] (2) The ground material is spray-dried in a centrifugal sprayer to obtain spherical particles of 15-35 μm.

[0036] (3) The spray-dried spherical particle powder is fed into pure oxygen (purity is 99%-99.99% pure oxygen, and the flow rate of pure oxygen is 90ml per minute) at 400°C for calcination treatment, and heat preservation for 13 hours;

[0037] (4) The above-mentioned calcined material is subjected to airflow pulverization to obtain a spheri...

Embodiment 2

[0039] A low-cost, high-purity, green and environmentally friendly nanocrystalline battery-grade anhydrous FePO 4 The preparation method, described method comprises the following steps:

[0040] (1) 120 grams of 85% H 3 PO 4 1. Dissolve 65g of oxalic acid in pure water, add 58 g of Fe powder with a particle size of less than 100μm under nitrogen protection, stir and soak for 24 hours, then add the soaked raw materials into a high-energy mill and grind for 48 hours. Stirring speed: 650 rpm, nitrogen The volume is 100ml per minute.

[0041] (2) The ground material is spray-dried in a centrifugal sprayer to obtain spherical particles of 15-35 μm.

[0042] (3) The spray-dried spherical particle powder is calcined at 500° C. in a sintering furnace fed with pure oxygen (purity is 99%-99.99% pure oxygen, and the flow rate of pure oxygen is 110 ml per minute), and it is kept warm for 13 Hour;

[0043] (4) The above-mentioned calcined material is subjected to airflow pulverization t...

Embodiment 3

[0045] A low-cost, high-purity, green and environmentally friendly nanocrystalline battery-grade anhydrous FePO 4 The preparation method, described method comprises the following steps:

[0046] (1) 120 grams of H3PO with a concentration of 85% 4 Dissolve 70g of oxalic acid in pure water, add 60g of Fe powder with a particle size of less than 100μm under the protection of nitrogen to carry out ball milling reaction for 50h, stirring speed: 750 rpm, nitrogen volume 135ml per minute.

[0047] (2) The ground material is spray-dried in a centrifugal sprayer to obtain spherical particles of 35 microns.

[0048] (3) The spray-dried spherical particle powder is calcined at 600°C in a sintering furnace fed with pure oxygen (purity is 99%-99.99% pure oxygen, and the flow rate of pure oxygen is 170ml per minute), and it is kept warm for 13 Hour;

[0049] (4) The above-mentioned calcined material is subjected to airflow pulverization to obtain a spherical lithium iron phosphate precur...

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Abstract

The invention discloses a preparation method of low-cost high-purity environment-friendly nanocrystalline battery-grade anhydrous FePO4. According to the method, iron powder, phosphoric acid and oxalate dihydrate are used as raw materials, the raw materials are added into purified water, nitrogen is introduced for soaking reaction, then a reactant is transferred into a high energy mill for ball milling treatment, after the iron powder is reacted completely, high-speed centrifugal spray granulation is conducted, a certain amount of oxygen is introduced into a ball material obtained through spray granulation, and after high temperature calcination and heat preservation are conducted in a furnace for a certain time, the nanocrystalline battery-grade anhydrous FePO4 is obtained. The preparation method of the low-cost high-purity environment-friendly nanocrystalline battery-grade anhydrous FePO4 is low in product cost, simple in process, high in safety, and worth application and popularization in the whole industry.

Description

technical field [0001] The invention discloses the technical field of lithium-ion battery material preparation, and in particular relates to a low-cost, high-purity, green and environmentally friendly nanocrystalline battery-grade anhydrous FePO4 preparation method, which is especially suitable for industrial production enterprises with strict environmental protection requirements. Background technique [0002] Lithium iron phosphate cathode material is currently one of the most promising cathode materials for lithium-ion batteries due to its good safety performance, low price, environmental protection, and long service life. Due to the poor electronic conductivity of lithium iron phosphate materials, if the primary particle size is not controlled, the ionic conductivity will increase, resulting in poor electrochemical performance. Reducing the single crystal size of lithium iron phosphate by using single crystal particle nano-sized raw materials, semi-wet process, low-tempe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37B82Y40/00
CPCB82Y40/00C01B25/375C01P2002/72C01P2004/32C01P2004/61
Inventor 李健梁浩
Owner 深圳中芯能科技有限公司
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