Preparation method of nanometer iron phosphate

A technology of nano-iron phosphate and phosphoric acid, applied in the direction of nanotechnology, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of low product purity, large product particle size, and difficulty in controlling product particle size, and achieve high product purity and high production efficiency , good effect of monodispersity

Active Publication Date: 2012-04-11
TSINGHUA UNIV
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Problems solved by technology

These methods have disadvantages such as long reaction time, difficult control of product particle size, and difficult guarantee of product purity.
For example, the oxidation method has strict requirements on the reaction system, ferrous salt is easily oxidized, and inert gas protection is required during the reac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Prepare raw material A by preparing an aqueous solution containing 0.05 mol / L of ferric nitrate and 0.05 mol / L of phosphoric acid. A 0.1 mol / L ammonium phosphate aqueous solution was prepared to obtain raw material B. 1 L of raw material A and 1 L of raw material B were rapidly mixed using a membrane dispersion micro-mixer to obtain slurry C. Slurry C was subjected to atmospheric pressure hydrothermal treatment for 0.2 hours at a treatment temperature of 100°C. Filtrate the precipitate from the slurry C, wash and dry the precipitate to obtain nanometer iron phosphate with an average particle size of about 80nm.

Embodiment 2

[0022] Prepare raw material A by preparing an aqueous solution containing 0.1 mol / L of ferric chloride and 0.02 mol / L of phosphoric acid. A 0.1 mol / L ammonium phosphate aqueous solution was prepared to obtain raw material B. 1 L of raw material A and 1 L of raw material B were rapidly mixed using a micro-mesh micro-mixer to obtain slurry C. Slurry C was subjected to atmospheric pressure hydrothermal treatment for 2.0 hours at a treatment temperature of 120°C. Filtrate the precipitate from the slurry C, wash and dry the precipitate to obtain nanometer iron phosphate with an average particle size of about 120nm.

Embodiment 3

[0024] Prepare raw material A by preparing an aqueous solution containing 1.0 mol / L of iron nitrate and 2.0 mol / L of phosphoric acid. Prepare a 0.5 mol / L ammonium phosphate aqueous solution to obtain raw material B. 1 L of raw material A and 2.5 L of raw material B were rapidly mixed using a co-current micro-tank micro-mixer to obtain slurry C. Slurry C was subjected to atmospheric pressure hydrothermal treatment for 1.0 hour at a treatment temperature of 110°C. Filtrate the precipitate from the slurry C, wash and dry the precipitate to obtain nano-iron phosphate with an average particle size of about 100 nm.

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Abstract

The invention discloses a preparation method of nanometer iron phosphate, which belongs to the field of chemistry and chemical engineering. The method comprises the following steps of: previously adding proper amount of ferric iron salt water solution of phosphoric acid as iron source; taking phosphate water solution as phosphorus source; using micro mixer to quickly mix the iron source with the phosphorus source to obtain iron phosphate precursor with better monodispersity in a state of nanometer particle; and using normal pressure hydrothermal method to directly process product slurry to obtain nanometer iron phosphate material with high purity and average particle size of about 100nm. The method has the advantages of simple preparation process, high production efficiency, high product purity, uniform particle size, good monodispersity and easy industrial amplification.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to a method for preparing nano-iron phosphate by combining liquid-phase precipitation reaction and hydrothermal treatment. Background technique [0002] Iron phosphate is an important iron-based material. It is cheap, rich in raw materials, non-toxic and harmless. It was originally used in agriculture, ceramic glass, steel and surface passivation and other fields. In recent years, researchers have found that iron phosphate has unique catalytic properties, ion exchange capacity and electrochemical performance, and has broad application prospects in the fields of catalysis and lithium-ion battery electrode materials. At present, the commonly used methods for preparing ferric phosphate are mainly divided into two types: oxidation method and precipitation method. The oxidation method is to mix soluble ferrous salt and phosphate and add an oxidizing agent to...

Claims

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Application Information

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IPC IPC(8): C01B25/37B82Y40/00
Inventor 吕阳成张同宝骆广生
Owner TSINGHUA UNIV
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