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A kind of preparation method of battery grade microporous spherical iron phosphate

An iron phosphate, battery-level technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems affecting the electrical conductivity and charge and discharge performance of lithium iron phosphate, many impurities in iron phosphate, and complex preparation processes, etc., to achieve The effect of fewer types of raw materials, uniform particle size distribution, and simple process

Active Publication Date: 2019-03-05
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the iron phosphate prepared by the current method contains more impurities, which affects the electrical conductivity and charge-discharge performance of the subsequent preparation of lithium iron phosphate, and the preparation process is complicated and the cost is high.

Method used

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  • A kind of preparation method of battery grade microporous spherical iron phosphate
  • A kind of preparation method of battery grade microporous spherical iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Step 1: Measure 15mol·L -1 21.00ml of phosphoric acid solution, add FeCl 3 ·6H 2 O14.00g, and 200ml deionized water, stir and heat at 100°C for 90 minutes, and concentrate to a volume of 100ml.

[0017] Step 2: After the above solution is slightly cold, add 40ml of concentrated nitric acid with a content of 65%-68%, add 0.32g of nano silica, dilute to 1L with deionized water, and stir at a constant temperature for 3h at 80°C. Nano-silica is the crystal nucleus, causing the iron phosphate crystals to precipitate out in the solution, and then centrifugal filtering, washing and drying the precipitate to prepare battery-grade iron phosphate.

[0018] Step 3: Put the iron phosphate prepared above into 100 ml of hydrofluoric acid with a concentration of 1% and soak for 40 minutes, filter with medium-speed quantitative filter paper, wash and dry to prepare a microporous spherical battery-grade iron phosphate material.

[0019] The carbon reduction high-temperature solid-phase method ...

Embodiment 2

[0021] Step 1: Measure 15mol·L -1 21.00ml of phosphoric acid solution, add FeCl3·6H2O14.00g, and 200.00ml deionized water, stir and heat at 100°C for 90 minutes, and concentrate to a volume of 100ml.

[0022] Step 2: After the above solution is slightly cold, add 20ml of 65%-68% nitric acid and 0.32g of nano silica, dilute to 1L with deionized water, and stir at a constant temperature for 3 hours at 75°C. Silicon is the crystal nucleus, causing iron phosphate crystals to precipitate out in the solution, and then the precipitate is centrifuged, washed, and dried to prepare battery-grade iron phosphate.

[0023] Step 3: Put the iron phosphate prepared above into 100 ml of 2% hydrofluoric acid and soak for 30 minutes, filter with medium-speed quantitative filter paper, wash, and dry to prepare a microporous spherical iron phosphate material.

[0024] The carbon reduction high-temperature solid-phase method is used to further prepare lithium iron phosphate battery-grade materials, and th...

Embodiment 3

[0026] Step 1: Measure 15mol·L -1 25.00ml of phosphoric acid solution, add FeCl 3 ·6H 2 O15.00g, and 200ml deionized water, stirred and heated at 100°C for 120 minutes, concentrated to a volume of 80ml.

[0027] Step 2: After the above solution is slightly cold, add 30ml of concentrated nitric acid with a content of 65%-68%, add 0.32g of nano-silica, dilute to 1L with deionized water, and stir for 2h at a constant temperature at 80°C. Nano-silica is the crystal nucleus, which causes iron phosphate crystals to precipitate out in the solution, and then the precipitate is centrifuged, washed, and dried to prepare battery-grade iron phosphate.

[0028] Step 3: Put the above-prepared iron phosphate into 100ml of hydrofluoric acid with a concentration of 3% and soak for 30 minutes, filter with medium-speed quantitative filter paper, then wash and dry to prepare a microporous spherical battery-grade iron phosphate material.

[0029] The carbon reduction high-temperature solid-phase method i...

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Abstract

The invention provides a preparation method of battery level microporous spherical iron phosphate. The preparation method comprises the following steps: mixing and heating a phosphoric acid solution and ferric iron salt, and reacting to form a concentrated solution; adding a 1-3 mol / L nitric acid solution, nano silicon dioxide of which the mass percent is 0.01-0.1% and deionized water into the concentrate at 75-85 DEG C to induce iron phosphate crystals to precipitate out by using the nano silicon dioxide as a crystal nucleus, filtering, washing, and drying to prepare a battery level iron phosphate material; and soaking the iron phosphate prepared in the previous step in hydrofluoric acid for 20-60 minutes, washing, and drying to finally prepare the microporous spherical iron phosphate material, wherein the iron phosphate product prepared in the previous step is etched due to the reaction of the hydrofluoric acid and the nano silicon dioxide. Thus, the electric conductivity and charging / discharging properties of subsequently prepared lithium iron phosphate can be further improved. The invention belongs to the technical field of iron phosphate preparation.

Description

Technical field [0001] The invention belongs to the field of iron phosphate preparation, and specifically relates to a method for preparing iron phosphate. Background technique [0002] Lithium iron phosphate has high theoretical capacity (170mAh / g), high working voltage (about 3.5V voltage platform), good cycle performance, no memory effect and other excellent properties, and it has the advantages of low price and environmental friendliness, so it can replace Higher cost LiCoO 2 It has become a new generation of lithium-ion battery cathode material, and has become an important material for large-scale energy storage batteries such as electric vehicles. The solid-phase reaction method is currently a widely used method in the production and research of lithium iron phosphate, and iron phosphate has gradually become an important precursor for the production of lithium iron phosphate in the carbothermal reduction method. In CN 101337666A, CN 15181537A, CN1635648A, CN 101559935A, CN...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/32C01P2004/61C01P2006/40
Inventor 肖仁贵柯翔廖霞
Owner GUIZHOU UNIV
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