Method for preparing nano iron phosphate

A nano-ferric phosphate and phosphoric acid technology, which is applied in the fields of nanostructure manufacturing, nanotechnology, nanotechnology, etc., achieves the effects of simple equipment, low preparation cost and small size

Inactive Publication Date: 2010-04-14
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, no patents and articles on the preparation of nano-iron phosphate using this reactor have been reported.

Method used

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  • Method for preparing nano iron phosphate
  • Method for preparing nano iron phosphate
  • Method for preparing nano iron phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Adjust the rotational speed of the rotating packed bed to 500r·min -1 , the 0.1mol·L -1 Mixed solution of ferric nitrate and phosphoric acid in 0.1L·min -1 The speed is input into the rotating packed bed through the metering pump, and at the same time, 0.22mol L is input with the metering pump -1 The ammonia solution is used to control the pH value of the reaction system to 1.70, and the reaction temperature is 60°C. The raw material solution is quickly and fully mixed under the action of large centrifugal force, and the reaction crystallizes to form nano-iron phosphate particles. After the reaction, the mixed solution is discharged from the rotating packed bed. The outlet is discharged, and the nano-scale ferric phosphate is obtained through post-treatment processes such as filtration, washing, and drying.

Embodiment 2

[0033] Adjust the rotational speed of the rotating packed bed to 2000r·min -1 , the 0.5mol·L -1 Ferric sulfate and sodium dihydrogen phosphate and 0.05g·L -1 The mixed solution of sodium dodecylsulfonate at 0.2L·min -1 The speed is input into the rotating packed bed through the metering pump, and at the same time, 2.0mol L is input with the metering pump -1 The sodium hydroxide solution is used to control the pH value of the reaction system to 3.00, and the reaction temperature is 15°C. The raw material solution is quickly and fully mixed under the action of a large centrifugal force, and the reaction crystallizes to form nano-iron phosphate particles. It is discharged from the discharge port, and the nano-scale ferric phosphate is obtained through post-treatment processes such as filtration, washing, and drying.

Embodiment 3

[0035] Adjust the rotational speed of the rotating packed bed to 1500r·min -1 , the 1.0mol·L -1 Iron acetate and phosphoric acid 0.1g·L -1 The mixed solution of polyethylene glycol and 1.0L·min -1 The speed is input into the rotating packed bed through the metering pump, and at the same time, 2.0mol L is input with the metering pump -1Potassium hydroxide solution is used to control the pH value of the reaction system to 5.80, and the reaction temperature is 45°C. The raw material solution is quickly and fully mixed under the action of large centrifugal force, and the reaction crystallizes to form nano-iron phosphate particles. It is discharged from the discharge port, and the nano-scale ferric phosphate is obtained through post-treatment processes such as filtration, washing, and drying.

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Abstract

The invention relates to a method for preparing nano iron phosphate, belonging to the technical field of the preparation of lithium ion battery cathode materials. The method is characterized by comprising the following steps: inputting an alkaline aqueous solution and a mixed solution formed by one of phosphoric acid or a soluble phosphate solution, one of a water-soluble ferrous salt solution and an oxidant or a ferric salt solution and a water-soluble dispersing agent into a rotating packed bed layer by a metering pump at a certain feeding speed; regulating the rotating speed of the rotating packed bed and controlling the pH value of the reaction system by an alkaline solution; discharging nano iron phosphate particles generated by reaction crystallization from a discharge hole of the rotating packed bed along with the mixed solution; and filtering, washing and drying the nano iron phosphate particles to obtain nano iron phosphate (FePO4.2H2O) powder. The method is simple and has easy operation and high efficiency, and the prepared iron phosphate reaches the nano grade, has uniform particle size and narrow distribution range and is suitable for industrialized production. The nano iron phosphate is a good precursor material for preparing lithium iron phosphate which is used as a cathode material of high-power type lithium ion batteries.

Description

technical field [0001] The invention relates to a new preparation method of nano-iron phosphate, in particular to a method for preparing nano-iron phosphate by using a rotating packed bed reactor. The nano-iron phosphate is an excellent precursor material for preparing lithium iron phosphate, a cathode material of a high-power lithium-ion battery. Background technique [0002] Iron phosphate is a chemical product widely used in pigments, ceramics, food additives and other fields. In recent years, it has been widely used in the preparation of lithium iron phosphate, the positive electrode material of lithium ion batteries. [0003] Lithium iron phosphate (LiFePO4) is a new type of cathode material developed in recent years. It has good safety performance, long cycle life (more than 2000 times), wide source of raw materials (lithium, iron, phosphorus), cheap price, and no environmental pollution. It is recognized by the industry as the preferred cathode material for a new ge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37B82B3/00
Inventor 蒲薇华任建国武玉玲何向明王莉李建军高剑杨峪生万春荣姜长印
Owner TSINGHUA UNIV
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