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Preparation method of iron phosphate with high tap density

A technology of tap density and iron phosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as low tap density, high energy consumption, and fluctuations in carbon content, and achieve high tap density and specific The effect of small surface area and dense growth

Active Publication Date: 2019-07-12
王东升
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, in the preparation of lithium iron phosphate, most manufacturers use anhydrous iron phosphate as the precursor. This is because iron phosphate dihydrate contains 20% water, and a large amount of water vapor is generated during the calcination process, resulting in a high dew point in the calcination furnace, which is easy to causing fluctuations in carbon content
[0004] At present, the preparation of anhydrous ferric phosphate is to react phosphate with iron salt to obtain ferric phosphate dihydrate, and then undergo high-temperature calcination (generally at a temperature of 500-600°C) to remove two crystal waters to obtain anhydrous ferric phosphate. Due to high-temperature calcination, As a result, the specific surface area of ​​anhydrous iron phosphate decreases sharply, and the energy consumption in the calcination process is high. According to actual production, each ton of anhydrous iron phosphate consumes 3500-5500 kWh of electricity, and the equipment requirements are high, the process is cumbersome, and the sintering process will cause phosphorus Volatilization loss, resulting in impurity, and easy to cause product pollution, and there is also the problem of low tap density

Method used

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  • Preparation method of iron phosphate with high tap density
  • Preparation method of iron phosphate with high tap density
  • Preparation method of iron phosphate with high tap density

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Effect test

Embodiment 1

[0035] A method for preparing ferric phosphate with high tap density, which comprises the following steps: mixing red phosphorus and iron powder under an inert atmosphere, then adding alcohol and putting them into a ball mill for ball milling, and then calcining at high temperature in an atmosphere furnace under an inert atmosphere to obtain Phosphorus-iron alloy body; the molar ratio of red phosphorus to iron powder is 1.015:1.

[0036] The inert atmosphere is nitrogen, and the oxygen content in the inert atmosphere is lower than 50ppm.

[0037] In the ball milling process, the mass ratio of the material to the alcohol is 1:0.85. The inner ball of the ball mill is made of zirconia balls. After 3 hours, the calcination temperature is 580°C, and it is taken out after cooling to the temperature <50°C.

[0038] The detection data of iron powder are as follows:

[0039] project Fe Fsss particle size O C Ni co data 99.64% 1.2μm 0.09% 0.02% 23.1ppm ...

Embodiment 2

[0053] A method for preparing ferric phosphate with high tap density, which comprises the following steps: mixing red phosphorus and iron powder under an inert atmosphere, then adding alcohol and putting them into a ball mill for ball milling, and then calcining at high temperature in an atmosphere furnace under an inert atmosphere to obtain Ferrophosphorus alloy body;

[0054] Put the obtained phosphorus-iron alloy body into a rotary furnace for oxidative calcination through oxygen-enriched gas, the calcination time is 4.8h, and the calcination temperature is 640°C to obtain a calcined powder;

[0055] The calcined powder is pulverized by airflow to obtain a powder with a particle size of 1.2 μm, which is then screened and electromagnetically removed to obtain anhydrous ferric phosphate.

[0056] The purity of the red phosphorus is 99.58%, the purity of the iron powder is 99.61%, the Fsss particle size is 1.7 μm, Ni / Co≤50ppm, Zn / Cd / Pb≤30ppm, Ca / Mg / Na / K≤100ppm.

[0057] The mol...

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Abstract

The invention discloses a preparation method of iron phosphate with a high tap density. The preparation method comprises the following steps: red phosphorus and iron powder are mixed in an inert atmosphere, then alcohol is added, the obtained mixture is placed in a ball mill and is ball-milled, and the ball-milled mixture is calcined at a high temperature in an inert atmosphere in an atmosphere furnace to obtain a ferrophosphorus alloy; the ferrophosphorus alloy is placed in a rotary furnace, and is oxidatively calcined by an oxygen-rich gas at 500-650 DEG C for 4-5 h to obtain a calcined powder; and the calcined powder undergoes jet milling to obtain a powder with a particle size of 0.5-2 [mu]m, and the powder is screened, and undergoes electromagnetic iron removal to obtain anhydrous iron phosphate. The preparation method has the advantages of simple process and low cost, and the obtained iron phosphate has the advantages of high tap density, good sphericity and large particle size,and is suitable for preparing high-compactness lithium iron phosphate.

Description

technical field [0001] The invention relates to a method for preparing iron phosphate with high tap density, belonging to the field of lithium battery new energy materials. Background technique [0002] Iron phosphate, also known as ferric phosphate, Iron orthophosphate , the molecular formula is FePO 4 , is a white, off-white monoclinic crystal powder. The material containing crystal water is a white slightly powdery material, and the anhydrous iron phosphate is a white slightly yellow material. Its main purpose is to manufacture lithium iron phosphate battery materials, catalysts and ceramics. [0003] At present, in the preparation of lithium iron phosphate, most manufacturers use anhydrous iron phosphate as the precursor. This is because iron phosphate dihydrate contains 20% water, and a large amount of water vapor is generated during the calcination process, resulting in a high dew point in the calcination furnace, which is easy to causing fluctuations in carbon con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37C01B25/45
CPCC01B25/375C01B25/45C01P2004/61C01P2004/62C01P2006/11C01P2006/12C01P2006/80C01P2006/82
Inventor 王东升
Owner 王东升
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