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Low-cost preparation method of anhydrous iron phosphate

An anhydrous phosphoric acid, low-cost technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of reduced specific surface area of ​​anhydrous iron phosphate, high energy consumption in the calcination process, and high dew point of the calciner. Short, low cost, high purity effect

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

AI Technical Summary

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 the reaction of phosphate and iron salt to obtain ferric phosphate dihydrate, and then undergoes 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 of the calcination process is high. According to actual production, each ton of anhydrous iron phosphate consumes 3500-5500 kWh of electricity, and the requirements for equipment are high, the process is cumbersome, and the sintering process will cause phosphorus Volatilization loss, resulting in impurity, and easy to cause product pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A kind of preparation method of low-cost anhydrous ferric phosphate, it is the following steps: get the iron oxide red waste material that steelworks produces, and its detection data is as follows:

[0039] project main content BET Cl- D50 value 99.04% 21.1m2 / g 650ppm 0.27μm Ni mn Zn Cr Cd 26.5ppm 110.5ppm 19.5ppm 27.5ppm 0.2ppm

[0040] Add the above iron oxide red waste into sulfuric acid solution to slurry, and at the same time raise the temperature to 72°C, stir for 55 minutes, then use a slurry pump to transport it to a filter press for filtration, and wash it with hot pure water at a temperature of 45°C until the washing water is dry. The pH is 4.9, and then the filtered and washed filter residue is dried and then air-flow crushed until the particle size of the material is 0.13 μm, and then the iron oxide red material is obtained through an electromagnetic separator. The test data is as follows:

[0041] ...

Embodiment 2

[0053] A method for preparing low-cost anhydrous ferric phosphate, which comprises the following steps: adding iron oxide red waste produced in a steelmaking plant to a sulfuric acid solution to make slurry, simultaneously raising the temperature to 72°C, stirring for 50 minutes, and then transporting with a slurry pump Filter through a filter press, wash with hot pure water at a temperature of 45°C until the pH of the washing water is 5.2, then dry the filtered residue and then air-flow pulverize until the particle size of the material is 0.15μm, and then pass through Electromagnetic iron remover to obtain iron oxide red material;

[0054] Add phosphoric acid to the iron oxide red material obtained, then add absolute alcohol and stir until the solid content is 45%, then transport it into the spray dryer through a high-pressure pump, use hot nitrogen as the heat source, and maintain the inlet temperature of the hot nitrogen at 240°C , the discharge temperature is 125°C to obta...

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Abstract

The invention discloses a low-cost preparation method of anhydrous iron phosphate. The method comprises the following steps: adding iron oxide red wastes produced in a steelmaking plant to a sulfuricacid solution, performing pulpifying, heating and reacting the obtained slurry, filtering the reacted slurry, washing the obtained filter residues with hot pure water, drying the washed filter residues, carrying out jet milling, and allowing the milled filter residues to go through an electromagnetic iron remover to obtain an iron oxide red material; adding the iron oxide red material to phosphoric acid, adding anhydrous alcohol, performing stirring, conveying the obtained solution into a spray dryer through a high-pressure pump, and using hot nitrogen as a heat source to obtain a dry material; and adding the dry material to anhydrous alcohol, washing the dry material, stopping washing when the content of free phosphoric acid in the dry material is less than 20 ppm, and drying the washed material to obtain the anhydrous iron phosphate. The method has the advantages of simple process and low cost, and the obtained anhydrous iron phosphate has the advantages of good dispersibility, highpurity, few impurity phases, large specific surface area, and easiness in subsequent grinding.

Description

technical field [0001] The invention relates to a preparation method of low-cost anhydrous iron phosphate, which belongs 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 FePO4, is a white, off-white monoclinic crystal powder. is iron saline solution and sodium phosphate The role of the salt, the iron in which is positive trivalent. 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 content [0004] At present, the prep...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/62C01P2006/12C01P2006/80C01P2006/82
Inventor 王东升
Owner 王东升
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