Nano iron fluoride-based composite material, and preparation method thereof

An iron fluoride-based, positive electrode material technology, applied in battery electrodes, electrical components, circuits, etc., can solve the problems of expensive graphene, harsh reaction conditions, and small specific surface area, and achieve easy industrial scale-up production and mild preparation conditions , the effect of uniform distribution of elements

Active Publication Date: 2017-05-17
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the existing preparation methods of introducing oxygen and carbon to prepare composite ferric fluoride materials and nano-sized ferric fluoride have complex processes, harsh reaction conditions, and high costs.
[0005] The preparation method of iron fluoride-based materials reported above still has at least the following problems: (1) carbon nanotubes and graphene are expensive and difficult to obtain, and the ball milling process consumes a lot of energy, making it difficult to apply to industrial production; (2) NH 4 HF 2 As a fluorinating reagent, there are also problems of high raw material prices and difficulty in large-scale production; (3) the hydrothermal / solvothermal reaction system has high temperature and high pressure, and there are fluorides in the system, which seriously corrodes equipment and is not suitable for industrial production; (4) The particle size of the obtained ferric fluoride is large, the specific surface area is small, and the electrical and catalytic activity is poor

Method used

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  • Nano iron fluoride-based composite material, and preparation method thereof
  • Nano iron fluoride-based composite material, and preparation method thereof
  • Nano iron fluoride-based composite material, and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1: Preparation of nanometer iron fluoride-based composite material

[0026] Dissolve 1.0M iron source in 50mL of polyol solvent, reflux at 30-80℃ for 6h, then add fluorinated reagent dropwise to the above solution under stirring, the dropwise addition time is 30min, after the dropwise addition is completed Reflux and stir at 140-200°C for 6 hours to obtain a suspension; then statically age at 100-160°C for more than 24 hours, and then wash and filter to obtain a solid; finally, calcinate at 200-350°C for more than 4 hours in an air atmosphere to prepare A nanocrystalline iron fluoride matrix composite material was obtained. The texture properties of iron fluoride prepared under different iron sources, polyol solvents, complexing agents, fluorinating reagents and calcination temperatures are shown in Table 1.

[0027] Table 1 Results of physicochemical properties of iron fluoride in Example 1

[0028]

Embodiment 2

[0029] Example 2: Preparation of nanometer iron fluoride-based composite material

[0030] Dissolve 1.0 M ferric nitrate and polyethylene glycol in 50 mL of ethylene glycol, reflux at 60 °C for 6 h with stirring, and then add HF aqueous solution (40 wt.%) dropwise to the above solution with stirring. The dropwise addition time is 30min, after the dropwise addition was completed, reflux and stirring at 160°C for 6h to obtain a suspension; then statically aged at 160°C for more than 24h, washed and filtered to obtain a solid; finally, calcined at 300°C for more than 4h to obtain a nanoparticle Crystalline iron fluoride. The ferric fluoride textures obtained with different amounts of polyethylene glycol are shown in Table 2.

[0031] Table 2 The results of physical and chemical properties of iron fluoride in Example 2

[0032]

Embodiment 3

[0033] Example 3: Preparation of nanometer iron fluoride-based composite material

[0034] Dissolve 1.0M ferric nitrate and polyethylene glycol (the mass ratio of Fe / complexing agent is 1:3) in 50 mL of ethylene glycol, reflux for 6 h under stirring at 60 °C, and then add HF aqueous solution dropwise to the mixture under stirring. In the above solution, the dropwise addition time was 30min. After the dropwise addition was completed, the solution was refluxed and stirred at 160°C for 6h to obtain a suspension; then statically aged at 160°C for more than 24h, washed and filtered to obtain a solid; finally, the solid was obtained at 300°C. Under roasting for more than 4h, nanocrystalline iron fluoride is obtained. The textures of iron fluoride prepared with different HF concentrations are shown in Table 3.

[0035] Table 3 The results of physical and chemical properties of iron fluoride in Example 3

[0036]

[0037]

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Abstract

The invention discloses a preparation method of a nano iron fluoride-based composite material, which aims to solve the problems of high raw material cost, complex synthetic process, difficulty in uniform mixing of iron fluoride and carbon and oxygen elements, and inability for effective grain size control of the conventional preparation method. The preparation method of nanocrystalline iron fluoride comprises the following steps: (1) preparing a solution consisting of an iron source precursor, a polyalcohol solvent, and a complexing agent, and carrying out refluxing at a temperature of 30-80 DEG C; (2) adding a fluorinating reagent to a solution obtained through (1) for fluorination, and carrying out refluxing and stirring at a temperature of 140-200 DEG C to obtain a suspension; and (3) carrying out aging of the suspension at a temperature of 100-160 DEGC, carrying out washing and filtering of the aged suspension to obtain a solid, and finally calcinating the solid at a temperature of 200-350 DEG C to obtain the nano iron fluoride.

Description

technical field [0001] The invention relates to a nano iron fluoride, in particular to a mild, simple and environment-friendly preparation method of a carbon-coated iron fluoride composite material. Background technique [0002] Ferric fluoride has low toxicity and high thermal stability, especially its high theoretical specific capacity and high discharge platform, making it one of the most potential new environmentally friendly and high-efficiency battery cathode materials for replacing existing lithium LiCoO, an expensive cathode material in batteries 2 , LiFePO 4 . In addition, the iron fluoride surface has moderate strength Lewis and Acids can be used as catalysts for the synthesis of various fine chemicals. For example, the isomerization of citronellal to isopulegol requires diacid catalysis. Because the iron fluoride-based catalyst has two acid sites, it has few side reactions and good stability in the above reaction, showing a good application prospect. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62
CPCH01M4/364H01M4/58H01M4/625Y02E60/10
Inventor 毛伟吕剑白彦波王伟王博杨志强郝志军杜咏梅亢建平石磊贾兆华
Owner XIAN MODERN CHEM RES INST
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