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A kind of method of low temperature preparation containing fexpo4 material by ferrophosphorus

A ferrophosphorus and low-temperature technology, which is applied in the field of low-temperature preparation of FexPO4-containing substances from ferrophosphorus, can solve the problems of large influence on product particle size, high water consumption, and high energy consumption, and achieve the elimination of slow gas-solid reaction speed and energy consumption High and low cost effect

Active Publication Date: 2019-04-16
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, when preparing ferric phosphate directly from ferrophosphorus, the particle size of the product is greatly affected by the particle size of the raw material of ferrophosphorus
[0005] Here, the present invention proposes to utilize ferrophosphorus to prepare Fe-containing x PO 4 A new process route to overcome the current Fe x PO 4 Insufficiency of the production process, using the magnetic properties of ferrophosphorus to physically purify it, solve the problem of preparing Fe from ferrophosphorus x PO 4 When the ferrophosphorus raw material consumes a lot of water, high energy consumption, and the type and content of impurities are uncertain, it is difficult to fully purify impurity elements and Fe x PO 4 To solve the technical problem of difficult control of product particle size and shape, simplify the preparation process, reduce energy consumption and waste discharge, the present invention proposes a new process method completely different from the above invention: reacting ferrophosphorus and oxidizing substances under low temperature conditions Preparation of Fe x PO 4 , Fe can be obtained directly through raw material selection and process control x PO 4 Finished products, which can be further used as raw materials for the production of other materials, and the types of by-products are controllable

Method used

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  • A kind of method of low temperature preparation containing fexpo4 material by ferrophosphorus
  • A kind of method of low temperature preparation containing fexpo4 material by ferrophosphorus
  • A kind of method of low temperature preparation containing fexpo4 material by ferrophosphorus

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Effect test

Embodiment 1

[0023] Ferrophosphorus Fe by solvothermal method 1.5 Preparation of Iron Hydroxyphosphate Fe from P 5 (PO 4 ) 4 (OH) 3 , the ferrophosphate slag Fe 1.5 P is crushed until the particle size is above 400 mesh. According to the magnetic difference between ferrophosphorus and impurities, the high-purity ferrophosphorus is transferred into a clean container by magnetic flotation, thereby improving the purity of the raw material ferrophosphorus. In the hydrothermal kettle with pressure valve, add phosphoric acid and hydrogen peroxide in proportion, and add water or other solvents as needed, and react at 50ºC to 300ºC for 5 to 75 hours to obtain Fe 5 (PO 4 ) 4 (OH) 3 Aqueous solution, the morphology and particle size of the product are controlled through the concentration process, and spherical Fe with a particle size of 20-30 nm can be obtained after drying. 5 (PO 4 ) 4 (OH) 3 finished product, process such as figure 1 Shown, the XRD of product is as figure 2 shown. T...

Embodiment 2

[0027] Using an external magnetic field to strengthen the transfer process and reaction process, made of phosphorus iron Fe 2 Preparation of iron phosphate FePO from P 4 , the iron phosphorus Fe 2 P is crushed until the particle size is above 1000 mesh, and then mixed with supplementary phosphorus source P 2 o 5 The powder is mixed evenly in proportion in a dry atmosphere, and then transferred into a closed heating container with a pressure reducing valve, and a certain amount of air is introduced to make the powder reach a boiling state, and an external magnetic field of 1T~10T is used to strengthen the ferrophosphorus powder in the reaction container. The transfer process and reaction in , react at 100ºC ~ 500ºC for 10 ~ 35 h, get FePO 4 finished product. The reaction equation is as follows:

[0028]

[0029] In this reaction, P 2 o 5 To supplement the phosphorus source, O in the air 2 As an oxidant, the product is only iron phosphate FePO 4 , no other by-product...

Embodiment 3

[0031] Preparation of iron phosphate FePO from iron phosphorus FeP by plasma method 4 , the plasma generator is composed of aluminized stainless steel as the anode, the stainless steel tank wall as the cathode, and distilled water as the electrolyte. Put iron phosphorus FeP into a titanium basket and place it in the anode area where the plasma is generated for oxidation for 0.5~5 h , regulate the voltage and current of the plasma power supply to regulate the composition of oxidation products, adjust the composition of the solution to regulate the solubility of phosphate oxidation products, use the solubility of phosphate to purify the products, adjust the particle size and shape by concentration, and dry FePO 4 finished product. In addition, ferrophosphorus can be modified by in-situ doping by adjusting the electrolyte.

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Abstract

A method for low temperature manufacturing of a FexPO4-containing material using a ferrophosphorus, wherein x is a number determined by a chemical composition. The method uses the ferrophosphorus as a raw material, and comprises the following steps: mixing the ferrophosphorus with an oxidizing material, performing phosphorus or iron replenishment according to the composition of the ferrophosphorus, performing a low temperature reaction, and obtaining a FexPO4-containing material.

Description

technical field [0001] The invention relates to a low-temperature preparation of Fe-containing x PO 4 The material method overcomes the influence of impurities in raw materials, and the product has high purity, fine particle size, easy control of shape, and simple process. It can be applied to the comprehensive utilization of chemical solid waste and the low-cost clean production of high-end phosphate materials. Background technique [0002] As a phosphate of iron, containing Fe x PO 4 There are many kinds of substances, common ones are ferric phosphate, ferrous phosphate, ferric hydroxyphosphate, ferrous hydroxyphosphate, ferric carbonate phosphate, ferrous carbonate phosphate, which are widely used in energy materials, catalysts, ceramics, food additives and other fields . In the field of energy materials, containing Fe x PO 4 The substance itself can be used not only as an electrode material, but also as a material for preparing LiFePO 4 , LiFeP 2 o 7 and Li 3 F...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/37
Inventor 王贵欣许飞邹江东闫康平
Owner SICHUAN UNIV
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