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AlF3, and preparation method and application thereof

A technology of aluminum fluoride and aluminum salt, which is applied in the direction of aluminum fluoride, aluminum halide, electrical components, etc., can solve the problems of unfavorable human health, product impurities, toxicity, etc., achieve excellent electrochemical performance, simple preparation process, The effect of mild reaction conditions

Active Publication Date: 2019-01-29
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the above methods generally have the following problems: 1. Use hydrofluoric acid or hydrogen fluoride as a raw material to prepare aluminum fluoride. Hydrogen fluoride and its aqueous solution are toxic and easily deform bones and teeth, and hydrofluoric acid can also penetrate through the skin. Mucous membrane, respiratory tract and gastrointestinal tract absorption, which is not conducive to human health; 2. The traditional synthesis method of aluminum fluoride first obtains A1F 3 ·3H 2 O, then by calcining A1F 3 ·3H 2 O obtains anhydrous aluminum fluoride after removal of crystallization water, however, when the calcination temperature is higher than 300 °C, it will lead to A1F 3 ·3H 2 Hydrolysis of O to produce alumina (2A1F 3 ·3H 2 O=Al 2 o 3 +6HF), resulting in more impurities in the product
[0004] In addition, fluorine has the highest electronegativity, and the theoretical specific capacity of aluminum fluoride formed by combining with lightweight aluminum elements can be as high as 957mAh / g. Too low is generally only suitable for the aluminum electrolysis industry as a cosolvent and regulator, and cannot be used as an active material in batteries

Method used

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  • AlF3, and preparation method and application thereof
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  • AlF3, and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0051] A preparation method of aluminum fluoride, comprising the steps:

[0052] 1) Weigh 10g of aluminum nitrate nonahydrate into 30mL of deionized water, stir evenly at 100°C, slowly add 2.96g of ammonium fluoride, and stir to obtain a mixed solution;

[0053] 2) The mixed solution was heated at 80°C for 2h, then transferred to room temperature to stand for crystallization for 10h, suction filtered and washed with ethanol for 3 times to obtain white crystals, and the white crystals were dried in a blast oven at 100°C for 10h to obtain the precursor;

[0054] 3) Place the precursor in a tube furnace, program the temperature to 400°C at 5°C / min, keep the temperature for 3 hours, and naturally cool to room temperature to obtain aluminum fluoride.

Embodiment 2

[0056] A preparation method of aluminum fluoride, comprising the steps:

[0057] 1) Weigh 10g of aluminum nitrate nonahydrate in 30mL of deionized water, stir evenly at 100°C, slowly add 3.94g of ammonium fluoride, and stir to obtain a mixed solution;

[0058] 2) The mixed solution was heated at 80°C for 2h, then transferred to room temperature to stand for crystallization for 10h, suction filtered and washed with ethanol for 3 times to obtain white crystals, and the white crystals were dried in a blast oven at 100°C for 10h to obtain the precursor;

[0059]3) Place the precursor in a tube furnace, program the temperature to 400°C at 5°C / min, keep the temperature for 3 hours, and naturally cool to room temperature to obtain aluminum fluoride.

Embodiment 3

[0061] A preparation method of aluminum fluoride, comprising the steps:

[0062] 1) Weigh 13g of aluminum nitrate nonahydrate into 30mL of deionized water, stir evenly at 100°C, slowly add 3.85g of ammonium fluoride, and stir to obtain a mixed solution;

[0063] 2) The mixed solution was heated at 80°C for 2h, then transferred to room temperature to stand for crystallization for 10h, suction filtered and washed with ethanol for 3 times to obtain white crystals, and the white crystals were dried in a blast oven at 100°C for 10h to obtain the precursor;

[0064] 3) Place the precursor in a tube furnace, program the temperature to 450°C at 5°C / min, keep the temperature for 3 hours, and naturally cool to room temperature to obtain aluminum fluoride.

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Abstract

The invention discloses AlF3, and a preparation method and an application thereof. The preparation method includes: 1) heating an aluminum salt solution and adding a fluoride salt to form a mixed solution; 2) heating and crystallizing the mixed solution to obtain a precursor; 3) calcining the precursor to obtain the AlF3, wherein the aluminum salt and fluoride salt are both soluble. The preparation method is abundant in raw material source, is low in cost, is simple and reliable, has gentle reaction conditions and is easy to carry out in large-scale industrial production. Secondly, the methodis free of HF, so that the method is more environment-friendly and safe. Meanwhile, the AlF3 has excellent electrochemical performance, so that when being applied to batteries as a cathode active material, the AlF3 can reach 2.8-3.1 V in initial voltage and is higher than 300 mAh / g in specific capacity. Finally, the AlF3 has a special globular flower appearance.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to an aluminum fluoride and a preparation method and application thereof. Background technique [0002] At present, the industrial production process of aluminum fluoride mainly includes: 1. Hydrofluoric acid method, including dry process and wet process, dry process obtains ɑ-A1F after high temperature calcination at 500-600 °C 3 ;Wet method is A1F first 3 ·3H 2 O crystal, and then calcined at high temperature to obtain A1F 3 , the raw materials are hydrogen fluoride and aluminum hydroxide; 2. Fluorosilicic acid method, using fluorosilicic acid and aluminum hydroxide to react to obtain aluminum fluoride products, the products are mainly square α-crystal form or hexagonal β-crystal form Aluminum fluoride monohydrate; 3. Aluminum salt method, which mainly uses aluminum chloride aqueous solution and hydrofluoric acid to heat to 400 ℃ to obtain aluminum fluoride products; secondl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/50H01M4/58C25C3/18
CPCC01F7/50C01P2002/72C01P2004/03C01P2004/32C01P2006/12C25C3/18H01M4/582Y02E60/10
Inventor 袁中直林锦芳朱立才何仲张琼文
Owner SOUTH CHINA NORMAL UNIVERSITY
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