Preparation method of magnesium fluoride with high specific surface area

A magnesium fluoride and magnesium source technology, applied in the direction of magnesium fluoride and magnesium halide, can solve the problems of low specific surface area of ​​magnesium fluoride, inconvenient operation and control, complicated preparation process, etc., achieve high specific surface area, easy control, The effect of simple equipment

Active Publication Date: 2014-10-01
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to address the disadvantages of low specific surface area, complex preparation process, high production cost, high environmental protection pressure, inconvenient operation and control, and great corrosion to devices of magnesium fluoride prepared by most existing methods. , to provide a method for preparing magnesium fluoride with high specific surface area with simple preparation method, low production cost, low environmental protection pressure, easy operation and control, and low corrosion to equipment

Method used

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  • Preparation method of magnesium fluoride with high specific surface area
  • Preparation method of magnesium fluoride with high specific surface area
  • Preparation method of magnesium fluoride with high specific surface area

Examples

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Effect test

Embodiment 1

[0036] Prepare 100ml equal volume of 2mol / L NH 4 F solution and 1mol / L Mg(CH 3 COO) 2 4H 2 O solution, and sucrose (containing C 0.4mol) was added to the magnesium acetate solution, and the sucrose was completely dissolved. Mix by positive addition, and turn on magnetic stirring at the same time, react at a temperature of 30 °C for 7 hours, then leave it for aging at a constant temperature for 2 hours, evaporate the resulting solution to dryness, and put it in an oven at 100 °C for pre-carbonization for 6 hours, and then Pre-carbonize in an oven at 160°C for 6 hours, then bake in a muffle furnace under a nitrogen atmosphere at 400°C for 4 hours to obtain charcoal-containing magnesium fluoride, and finally bake in a muffle furnace under an air atmosphere at 400°C for 4 hours to remove carbon Template, you can get magnesium fluoride with high specific surface area, its specific surface area is 184m 2 / g, the pore volume is 0.35cc / g, and the most probable pore size distribution...

Embodiment 2

[0039] Prepare each 100ml equal volume of 2mol / L NaF solution and 1mol / L Mg(CH 3 COO) 2 4H 2 O solution, and sucrose (containing C 0.1mol) was added to the magnesium acetate solution, and the sucrose was completely dissolved. Mix by positive addition, and turn on magnetic stirring at the same time, react at a temperature of 30 °C for 7 hours, then leave it for aging at a constant temperature for 2 hours, evaporate the resulting solution to dryness, and put it in an oven at 100 °C for pre-carbonization for 6 hours, and then Pre-carbonize in an oven at 160°C for 6 hours, then bake in a muffle furnace under a nitrogen atmosphere at 400°C for 4 hours to obtain carbon-containing magnesium fluoride, and finally bake in a muffle furnace under an air atmosphere at 400°C for 3 hours to remove carbon Template, you can get magnesium fluoride with high specific surface area, its specific surface area is 73m 2 / g.

Embodiment 3

[0041] Prepare 100ml equal volume of 2mol / L NH 4 F solution and 1 mol / L MgC 2 o 4 .2H 2 O solution, and sucrose (containing C 1mol) was added to the ammonium fluoride solution, and the sucrose was completely dissolved. Mix by reverse addition, and turn on magnetic stirring at the same time, react at a temperature of 30°C for 7 hours, then leave it for aging at a constant temperature for 2 hours, evaporate the resulting solution to dryness, and put it in an oven at 100°C for pre-carbonization for 6 hours, and then Pre-carbonize in an oven at 160°C for 6 hours, then bake in a muffle furnace under a nitrogen atmosphere at 400°C for 4 hours to obtain charcoal-containing magnesium fluoride, and finally bake in a muffle furnace under an air atmosphere at 400°C for 12 hours to remove carbon Template, you can get magnesium fluoride with high specific surface area, its specific surface area is 153m 2 / g.

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Abstract

The invention discloses a preparation method of magnesium fluoride with high specific surface area. The preparation method comprises the steps of: mixing a magnesium source water solution with a fluorine source water solution, wherein the obtained mixed solution contains a carbon source, the carbon source is one of or a mixture of several of saccharose, glucose, furfuryl alcohol, P123, polyvinyl alcohol and phenolic resin and the mole ratio of the carbon source to the magnesium source is 1-10: 1 based on C to Mg; stirring for full reaction and standing for ageing and removing moisture to obtain a carbon source-containing magnesium fluoride precursor; carrying out pre-carbonization on the carbon source-containing magnesium fluoride precursor and then carrying out carbonization in an inert atmosphere to obtain carbon-doped magnesium fluoride; finally carrying out high-temperature decarburization in an oxygen-bearing atmosphere to obtain the magnesium fluoride product. The preparation method is simple, low in production cost, small in environmental pressure, easy to operate and control and low in device corrosion, and has favorable economical, environmental and social benefits.

Description

technical field [0001] The invention relates to a preparation method of magnesium fluoride, in particular to a preparation method of magnesium fluoride with a high specific surface area. technical background [0002] Magnesium fluoride is an important raw material in industrial production, widely used in ceramics and glass manufacturing; as a flux in the metallurgical industry; as a coating, film material or fluorescent material in optics. Especially the hot-pressed magnesium fluoride material, due to its extremely high infrared transmittance in the mid-wave infrared band; high mechanical strength and thermal shock resistance; small dielectric constant and dielectric loss and isotropy And many other characteristics, it is a good mid-wave infrared window, fairing material and mid-wave infrared / millimeter wave (microwave) composite radome material, widely used in infrared guidance, infrared imaging guidance, infrared / millimeter wave (microwave) composite guidance and Infrared...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/28
Inventor 李瑛唐浩东牛怀成韩文峰刘化章
Owner ZHEJIANG UNIV OF TECH
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