Method for preparing LixFeyPzO4 from ferrophosphorous

A technology of ferrophosphorus and phosphorus sources, applied in chemical instruments and methods, phosphorus compounds, nanotechnology for materials and surface science, etc. The content is uncertain and other problems, so as to overcome the difficulty of raw material ratio, eliminate the easy corrosion of equipment, and easy to control the appearance.

Active Publication Date: 2016-11-09
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently commercial Li x Fe y P z o 4 The outstanding problems that still exist in the preparation process are: the use of expensive (sub) iron salts, the high energy consumption of high-temperature roasting, the difficulty of uniform mixing of solid precursors, etc., the strict limitation on the amount of oxygen, and the lack of utilization of oxygen-containing substances. Oxygen provides an oxygen source for the product, and the cost of raw materials and preparation is relatively high
In the invention patent 201010126920.X, although the one-step method is used to prepare LiFePO from phosphorus iron 4 , but using solid phase reaction, the reaction temperature is higher
[0005] In order to overcome the current Li x Fe y P z o 4 The deficiencies in the production process solve the problem of preparing Li by ferrophosphorus x Fe y P z o 4 Uncertain impurity types and contents in ferro

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  • Method for preparing LixFeyPzO4 from ferrophosphorous
  • Method for preparing LixFeyPzO4 from ferrophosphorous
  • Method for preparing LixFeyPzO4 from ferrophosphorous

Examples

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Example Embodiment

[0023] Example 1

[0024] Using solid-liquid low-temperature reaction 1.5 P preparation of lithium iron phosphate LiFePO 4 , The phosphorus iron slag Fe 1.5 P is pulverized to a particle size above 700 meshes. According to the different magnetic properties of ferrophosphorus and impurities, the high-purity ferro-phosphorus is transferred into a clean container by magnetic flotation to eliminate the influence of impurity elements in the raw materials of ferro-phosphorus on the product. Put it into a hydrothermal kettle lined with PTFE, according to LiFePO 4 The molar ratio of total lithium element, total iron element and total phosphorus element is 1.0:1.0:1.0. Phosphoric acid and lithium hydroxide are added. Hydrogen peroxide is added according to the composition of raw materials and products. An external magnetic field can be used to strengthen the reaction and transfer process. If necessary, water or ethanol solvents can be added, or some substances that dope, coat or compound t...

Example Embodiment

[0027] Example 2

[0028] Preparation of lithium iron phosphate LiFePO from ferrophosphorus FeP by solvothermal method 4 , The ferro-phosphorus powder with a particle size greater than 1000 meshes is purified by flotation of density and magnetic difference, and the high-purity ferro-phosphorus FeP is transferred into a reactor lined with fluorine rubber, and then combined with lithium phosphate Li 3 PO 4 , Phosphoric acid H 3 PO 4 , Iron oxide Fe 2 O 3 Press LiFePO 4 The molar ratio of the total lithium element, the total iron element and the total phosphorus element is 1.0:1.0:1.0 for batching. A certain amount of hydrogen peroxide can be added according to the composition of the raw material and product, and a certain amount of ethanol can be added as a solvent. More than 2 / 3 of the volume of the reactor, heated with molten salt, reacted at 150℃~350℃ for 20~40h to obtain LiFePO 4 The precursor aqueous solution is concentrated and granulated to control the morphology and particle ...

Example Embodiment

[0031] Example 3

[0032] An electrolytic cell is added to the low-temperature reactor, and the atomic oxygen generated in the anode is used to directly oxidize the phosphorus element in the ferrophosphorus, and the pressure generated by the system is used to accelerate the reaction. The hydrogen generated by the electrolysis of water is extracted as the clean heating raw material for the reactor, and it is adjusted Raw materials and process parameters to achieve LiFePO 4 The in-situ synthesis of the product, the specific operation process is as follows: the high-purity ferrophosphorus Fe 1.5 P, lithium carbonate, phosphoric acid according to LiFePO 4 The molar ratio of total lithium element, total iron element and total phosphorus element is 1.0:1.0:1.0 for batching. The total amount of reaction materials does not exceed 3 / 4 of the volume of the reactor. Put the graphite anode of the electrolytic cell into the reaction In the kettle, the anode chamber and the cathode chamber are ...

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Abstract

The invention relates to a method for preparing LixFeyPzO4 from ferrophosphorous at a low temperature in a closed system. A raw material is purified through physical and chemical reaction processes, oxygen in an oxidation raw material provides an oxygen source for the above product, and the self material balance reaction and the self-produced pressure driving reaction of reactants are realized through raw material selection and technology regulation to solve the disadvantages of traditional ferrophosphorous high temperature reactions, the reaction temperature is low, the energy consumption and the water consumption are low, device corrosion is light, byproducts can only be water, and energy saving , emission reduction and clean production are realized. The method utilizes a convenient operating technology, and promotes the reaction by using the pressure generated in the reaction process, so the product has the advantages of high purity, small granularity, easy morphology control and easy reaction control, and the preparation method has the advantages of simplicity, high resource utilization rate, low cost, less investment, good benefit, cleanness and environmental protection, easy industrialization, and suitableness for high-value comprehensive utilization of chemical engineering byproducts and large-scale industrial low-cost clean production of high-end phosphates.

Description

technical field [0001] The invention relates to a low-cost preparation of Li by ferrophosphorus x Fe y P z o 4 The method overcomes the influence of impurities in raw materials, reduces water consumption and energy consumption, 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 high-end phosphate energy materials with special shapes. low-cost production. Background technique [0002] As an alloy formed of phosphorus and iron, ferrophosphorus has a slight metallic luster, a large proportion, rich resources, and a wide range of sources (such as: minerals or their smelting products, yellow phosphorus or calcium magnesium phosphate fertilizers, etc. produced by phosphorus chemical industry and silicate chemical industry. By-products, self-made, etc.), the output is relatively large (only in the process of producing phosphorus by the electric furnace met...

Claims

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Application Information

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IPC IPC(8): C01B25/45B82Y30/00
CPCC01B25/45C01P2002/72C01P2004/32C01P2004/64
Inventor 王贵欣许飞邹江东闫康平
Owner SICHUAN UNIV
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