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A kind of preparation of li from phosphorus iron x fe y p z o 4 Methods

A technology of ferrophosphorus and phosphoric acid, applied in chemical instruments and methods, phosphorus compounds, nanotechnology for materials and surface science, etc., can solve high water consumption and energy consumption, difficult uniform mixing of solid precursors, high reaction temperature, etc. question

Inactive Publication Date: 2021-09-14
SICHUAN UNIV
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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 ferrophosphorus raw materials lead to difficulty in comprehensive purification of impurity elements, high water consumption and energy consumption, Li x Fe y P z o 4 The technical problems of large particle size and uncontrollable shape of the product, simplify the preparation process, reduce water consumption and energy consumption, and reduce waste discharge. In this application, based on our original patent application and new experimental results, we use physical methods and chemical reactions The process purifies ferrophosphorus through simple flotation and filtration, and can granulate the product and its precursor. It creatively proposes a coupling physical purification and chemical process to reduce the impact of the content of impurity elements in ferrophosphorus on the product and reduce the impact of low temperature on the product. Preparation of Li x Fe y P z o 4 new technology

Method used

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  • A kind of preparation of li from phosphorus iron <sub>x</sub> fe <sub>y</sub> p <sub>z</sub> o <sub>4</sub> Methods
  • A kind of preparation of li from phosphorus iron <sub>x</sub> fe <sub>y</sub> p <sub>z</sub> o <sub>4</sub> Methods
  • A kind of preparation of li from phosphorus iron <sub>x</sub> fe <sub>y</sub> p <sub>z</sub> o <sub>4</sub> Methods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Using solid-liquid low-temperature reaction to produce iron and phosphorus Fe 1.5 Preparation of Lithium Iron Phosphate LiFePO by P 4 , the ferrophosphate slag Fe 1.5 P is crushed until the particle size is above 700 mesh. According to the magnetic difference between ferrophosphorus and impurities, the high-purity ferrophosphorus is transferred into a clean container by magnetic flotation to eliminate the influence of impurity elements in the raw material of ferrophosphorus on the product, and the high-purity ferrophosphorus Put it in a hydrothermal kettle lined with polytetrafluoroethylene, according to LiFePO 4 The molar ratio of total lithium, total iron and total phosphorus is 1.0:1.0:1.0. Phosphoric acid and lithium hydroxide are added, and hydrogen peroxide is added according to the composition of raw materials and products. The external magnetic field can be used to strengthen the reaction and transfer process, according to If necessary, water or ethanol solven...

Embodiment 2

[0028] Preparation of lithium ferrous phosphate LiFePO from ferrophosphorus FeP by solvothermal method 4 , the ferrophosphorus powder with a particle size greater than 1000 mesh is purified by density and magnetic difference flotation, and the high-purity ferrophosphorus FeP is transferred into a reactor lined with fluororubber, and then mixed with lithium phosphate Li 3 PO 4 , Phosphate H 3 PO 4 , Iron oxide Fe 2 o 3 by 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 is added according to the composition of raw materials and products, and a certain amount of ethanol can be added as a solvent. The total amount of reaction materials is not More than 2 / 3 of the volume of the reactor, heating with molten salt, reacting at 150°C-350°C for 20-40h, to obtain LiFePO 4 Precursor aqueous solution, through the process of concentration and granulation to...

Embodiment 3

[0032] An electrolytic cell is added to the low-temperature reaction kettle, and the atomic oxygen generated in situ by 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. 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 obtained by flotation 1.5 P, lithium carbonate, phosphoric acid according to 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, the total amount of reaction materials does not exceed 3 / 4 of the volume of the reactor, and the graphite anode of the electrolytic cell is put into the reaction In the kettle, the anode chamber and the cathode chamber are connected through a valve and a diaphragm-lined fluorine plastic 304 stainless steel tube. T...

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Abstract

The invention relates to the preparation of Li at low temperature in a closed system by ferrophosphorus x Fe y P z o 4 The method uses physical and chemical reaction processes to purify the raw materials, and uses the oxygen in the oxidizing raw materials to provide the oxygen source for the product. Through the selection of raw materials and process regulation, the material balance reaction and self-production pressure-driven reaction of the reactants are realized, which overcomes the traditional The disadvantages of high-temperature reaction of ferrophosphorus are low reaction temperature, low energy and water consumption, light equipment corrosion, and the by-product can be only water, so as to realize energy saving, emission reduction and clean production. The method utilizes a convenient operation method, uses the pressure generated in the reaction process to promote the reaction, the product has high purity, small particle size, easy control of shape, easy control of the reaction, simple preparation method, high resource utilization rate, low cost, and less investment. Good benefits, clean and environmentally friendly, easy to industrialize, suitable for high-value comprehensive utilization of chemical by-products and high-end phosphate scale industrialization and low-cost clean production.

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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Patent Type & Authority Patents(China)
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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