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Method for preparing Li3PO4 and Fe2O3 by ferrophosphorus

A fe2o3, ferrophosphorus technology, applied in the field of materials, can solve the problems of reducing oxygen purity and oxygen accuracy, difficult oxygen control, equipment corrosion, etc., to achieve the effect of eliminating severe corrosion, shortening the utilization process, and lower requirements

Inactive Publication Date: 2011-03-30
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The idea of ​​the present application is to prepare Li 3 PO 4 and Fe 2 o 3 According to the composition of phosphorus and iron, different combinations of lithium-containing substances can be used, which reduces the temperature of the reaction, solves the serious corrosion problem of equipment caused by phosphorus, and reduces the requirements for the purity of oxygen and the accuracy of oxygen content. The generated Li 3 PO 4 and Fe 2 o 3 It can be used alone after separation by dissolution and filtration technology, or it can be mixed and used directly without separation, such as adding FePO under anaerobic conditions 4 and C and other raw materials to prepare LiFePO 4 and Li 3 Fe 2 (PO 4 ) 3 and other electrode materials, which can solve the difficult problem of oxygen control in the process of preparing electrode materials from ferrophosphorus

Method used

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  • Method for preparing Li3PO4 and Fe2O3 by ferrophosphorus

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Preparation of Li from FeP and LiOH by reactive pulverization method 3 PO 4 with Fe 2 o 3 , first crush ferrophosphorus to a certain particle size, use ferrophosphorus as the phosphorus source, and LiOH as the lithium source, the ratio of the two substances is 1:3, after ball milling for 5 hours, put it into a horse at 300-900°C Roasting in a Furnace for 0.5-10 hours, heating and cooling in the air, using oxygen in the air as an oxygen source, without controlling the amount of air, and without other protective atmospheres, to obtain Li 3 PO 4 with Fe 2 o 3 , the reaction equation is as follows:

[0022] 2FeP+6LiOH+4O 2 →2Li 3 PO 4 +Fe 2 o 3 +3H 2 o

Embodiment 2

[0024] Using the rheological phase method to obtain the by-product phosphorus iron Fe of the yellow phosphorus production plant 1.5 P as raw material to prepare Li 3 PO 4 with Fe 2 o 3 , first crush ferrophosphorus to a certain particle size with a ball mill, use ferrophosphorus as the phosphorus source, and use Li 2 CO 3 It is a lithium source, the ratio of the two substances is 2:3, and ethanol is used as a solvent. After being fully ball-milled or ground to form a rheological phase, it is put into a muffle furnace at 200-900°C for 1-25 hours and baked in the air. Heating and cooling, using oxygen in the air as an oxygen source, no need to control the amount of air, no other protective atmosphere, to get Li 3 PO 4 with Fe 2 o 3 , the reaction equation is as follows:

[0025] 8Fe 1.5 P+12Li 2 CO 3 +19O 2 →8Li 3 PO 4 +6Fe 2 o 3 +12CO 2

[0026] Among them, the by-product CO 2 Can be absorbed by LiOH solution to form Li 2 CO 3 Raw materials to achieve zero...

Embodiment 3

[0028] By-product Fe of calcium magnesium phosphate fertilizer production plant by spray drying method 2 P as raw material to prepare Li 3 PO 4 with Fe 2 o 3 , first crush ferrophosphorus to a certain particle size with a jet mill, use ferrophosphorus as the phosphorus source, and use LiH 2 PO 4 LiOH and LiOH are mixed lithium sources, and the ratio of the three substances is 1:1:5. After the precursor is atomized, it is placed in an oxygen atmosphere furnace at 200-900°C. It is not necessary to control the amount of oxygen, and it is not necessary to For other protective atmospheres, get Li 3 PO 4 with Fe 2 o 3 , the reaction equation is as follows:

[0029] 4Fe 2 P+4LiH 2 PO 4 +20LiOH+9O 2 →8Li 3 PO 4 +4Fe 2 o 3 +10H 2 o

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Abstract

The invention relates to a method for preparing Li3PO4 and Fe2O3 by ferrophosphorus belonging to the material field. The ferrophosphorus composed of FexPy has wide sources, in particular to minerals or smelting products thereof, and side products of phosphorus chemical industry or silicate chemical industry and the like to provide partial or whole phosphor sources for Li3PO4. Compared with the prior art, the method adopts lithium-containing substance with poor thermal stability to react with the ferrophosphorus, has rich raw material sources, and can adopt different combinations of the lithium-containing substances according to the composition of the ferrophosphorus, reduces reaction temperature, solves the problem of serious corrosion on equipment caused by high temperature phosphoric acid, reduces requirement on purity of oxygen and precision of oxygen amount, ensures that the formed Li3PO4 not only can be mixed with Fe2O3, but also can be independently used after being separated from Fe2O3 through dissolving if FePO4, C and other raw materials are added to prepare an electrode material LiFePO4 or Li3Fe2(PO4)3 and the like. Through the designing on the reaction and the absorption reaction of the side products, green and environmental-friendly process of zero emission can be realized, which is not concerned in the process for preparing Na3PO4 by the ferrophosphorus at present. The method has low requirement on equipment, simple process, short production flow, small investment, good benefit, and good application value.

Description

technical field [0001] The present invention relates to the preparation of Li by ferrophosphorus 3 PO 4 and Fe 2 o 3 The method belongs to the field of materials. Background technique [0002] Ferrophosphorus is an intermetallic compound formed by the reaction of phosphorus and iron. It is rich in resources and has a wide range of sources. It can be ferrophosphorus ore or its smelting products, or it can be produced by thermal phosphorus or calcium magnesium phosphate fertilizer and other phosphorus chemical and silicate chemical industries. It is a kind of by-product, which can also be self-made. It is gray in color, has a slight metallic luster, a large specific gravity, a relative density of 5.6-6.0, and a large output. The current market price is not high. For example: in the process of producing yellow phosphorus by electrothermal method, A small amount of iron and phosphorus in phosphate rock are reacted at high temperature in an electric furnace to form ferrophosp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/30C01G49/06
Inventor 王贵欣闫康平陈妙刘睿
Owner SICHUAN UNIV
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