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A kind of synthesis method of nanometer magnesium fluoride of high specific surface area

A synthesis method, magnesium fluoride technology, applied in nanotechnology for materials and surface science, magnesium fluoride, magnesium halide, etc., can solve the problem of low yield of magnesium fluoride on high specific surface, harsh production or reaction conditions, difficult Realize industrialization and other issues, achieve the effect of reducing economic waste and environmental pollution, suitable for promotion and application, and simple equipment

Active Publication Date: 2016-01-20
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the existing preparation methods of magnesium fluoride with high specific surface area have at least one of the following problems: (1) expensive raw materials: expensive organic magnesium sources are used, 2) harsh production or reaction conditions: in anhydrous The reaction is carried out in an oxygen-free environment, 3) The process is complicated: add an appropriate amount of pore-forming agent during the roasting process
4) Raw materials are highly corrosive: highly corrosive to experimental equipment
Therefore, the output of magnesium fluoride with high specific surface is small, it is difficult to scale up industrially, and it is difficult to realize industrialization

Method used

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  • A kind of synthesis method of nanometer magnesium fluoride of high specific surface area
  • A kind of synthesis method of nanometer magnesium fluoride of high specific surface area
  • A kind of synthesis method of nanometer magnesium fluoride of high specific surface area

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Experimental program
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Effect test

Embodiment 1

[0036] The production method of high specific surface area nano-magnesium fluoride in the present embodiment, comprises the following steps:

[0037] Prepare an equal volume of 3mol / L NH 4 F solution and 1mol / L Mg(CH 3 COO) 2 4H 2O solution, mixed by positive addition, and at the same time turned on the magnetic stirring, reacted at a temperature of 30 ° C for 7 hours, and then stood at a constant temperature for aging for 2 hours, suction filtered the obtained colloidal solution, took its filter cake, and placed it in After drying for 4 hours in the air flow at ℃, put it in an atmospheric oven at 110℃ and dry it for 17 hours, and finally bake it in a muffle furnace under an air atmosphere at 200℃ for 4 hours to obtain a transparent magnesium fluoride product. 153m 2 / g, the pore volume is 0.29cc / g, and the most probable pore size distribution is 31nm.

[0038] The high specific surface area magnesium fluoride nitrogen adsorption isotherm figure, pore size distribution fi...

Embodiment 2

[0040] The production method of high specific surface area nano-magnesium fluoride in the present embodiment, comprises the following steps:

[0041] Prepare an equal volume of 2mol / L NH 4 F solution and 1mol / L Mg(CH 3 COO) 2 4H 2 O solution, reacted by co-current co-precipitation method, and at the same time turned on the magnetic stirring, reacted at a temperature of 50 ° C for 5 hours, and then stood at constant temperature for aging for 1 hour, and suction-filtered the obtained solid-liquid mixture. After drying the cake in an air stream at 25°C for 6 hours, put it in an oven at 100°C and dry it for 20 hours, and finally bake it in a muffle furnace under a nitrogen atmosphere at 300°C for 3 hours to obtain magnesium fluoride powder. The specific surface area is 146m 2 / g, the pore volume is 0.31cc / g, and the most probable pore size distribution is 36nm. The XRD pattern of gained magnesium fluoride and image 3 similar.

Embodiment 3

[0043] The production method of high specific surface area nano-magnesium fluoride in the present embodiment, comprises the following steps:

[0044] Prepare an equal volume of 4mol / L NH 4 F solution and 2mol / L Mg(CH 3 COO) 2 4H 2 O solution, mixed by reverse addition, and at the same time turned on the magnetic stirring, reacted at a temperature of 70 ° C for 12 hours, and then stood at a constant temperature for aging for 3 hours, and suction-filtered the obtained colloidal solution, and took its filter cake. After drying in the air flow at ℃ for 1 hour, put it in an oven at 90 ℃ and dry it for 25 hours, and finally bake it in a muffle furnace under a nitrogen atmosphere at 500 ℃ for 2 hours to obtain a transparent magnesium fluoride product with a specific surface area of ​​139m 2 / g, the pore volume is 0.31cc / g, and the most probable pore size distribution is 34nm. The XRD pattern of gained magnesium fluoride and image 3 similar.

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Abstract

The invention discloses a synthetic method of nanometer magnesium fluoride with a high specific surface area. The method comprises the steps as follows: 1), magnesium salt is fully dissolved in deionized water, so that a reaction liquid A is obtained, wherein the magnesium salt adopts one or a combination of any of magnesium acetate, magnesium chloride and magnesium nitrate; and ammonium salt is dissolved in deionized water, so that a reaction liquid B is obtained, wherein the ammonium salt adopts ammonium fluoride or a combination of the ammonium fluoride and ammonium acetate; 2), the reaction liquid A and the reaction liquid B are mixed under stirring, and reaction is performed; 3), after reaction, stirring is stopped, and the mixture is stood for aging; 4), after aging, filtration or centrifugal separation is performed, and the mixture is dried; and 5), a dried sample is roasted, so that the nanometer magnesium fluoride is obtained. The nanometer magnesium fluoride prepared with the method has the high specific surface area, the synthetic method is simple, the production cost is low, the preparation period is short, operation and control are easy, and small corrosiveness is caused to a device.

Description

technical field [0001] The invention relates to a preparation method of magnesium fluoride, in particular to a simple synthesis method of nano-magnesium fluoride with high specific surface area. Background technique [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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F5/28B82Y30/00
Inventor 李瑛唐浩东牛怀成李雨臻韩文锋刘化章
Owner ZHEJIANG UNIV OF TECH
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