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Method for preparing nano-crystal magnesium fluoride with high specific surface area

A high specific surface area, crystalline magnesium fluoride technology, applied in the direction of magnesium fluoride, nanotechnology for materials and surface science, chemical instruments and methods, etc., can solve the problems of high energy consumption, complicated process and high cost of reflux reaction , to achieve the effect of easy material surface coating, mild preparation conditions and low corrosion

Active Publication Date: 2017-05-31
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above reported MgF 2 The preparation method still has the following problems at least: (1) the anhydrous sol-gel fluorination method is that the organic solvent of the metal source and anhydrous HF is the fluorine source with an expensive organic metal, and this method must be in anhydrous Under the condition of operation, the process is complicated, and it is difficult to apply to industrial production. At the same time, the obtained MgF 2 It has an amorphous structure, is unstable at high temperature, and is easy to crystallize into fluorides with low specific surface area; (2) Although the raw materials are easy to obtain in the carbonation and fluorination method, the process is complicated, and high-temperature carbonization and carbon removal processes need to be repeated, and the energy consumption is high. , and when the temperature is higher than 350℃, the specific surface area of ​​magnesium fluoride drops rapidly to 30m 2 / g or so; (3) Although the acetate method is easy to operate, the required acetate concentration is high, the consumption is large, and the cost is high, so it is not suitable for industrial production
(4) What reflux reaction adopts is the magnesium source that is insoluble in water, and product loss is serious, and the energy consumption of reflux reaction is higher

Method used

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  • Method for preparing nano-crystal magnesium fluoride with high specific surface area
  • Method for preparing nano-crystal magnesium fluoride with high specific surface area
  • Method for preparing nano-crystal magnesium fluoride with high specific surface area

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Embodiment 1

[0023] Embodiment 1: Preparation of high specific surface area, nanocrystalline magnesium fluoride

[0024] Dissolve 1.0M magnesium source in 50mL polyol solvent, reflux at 20-80°C for 6 hours, then add the fluorinated reagent dropwise to the above solution with stirring, the dropping time is 30min, after the dropping is completed, Stir for 6 hours to obtain a liquid sol; then statically age at 100-160°C for more than 24 hours to obtain a solid gel; then dry at 140-200°C for more than 24 hours, and finally roast at 350-450°C for more than 4 hours in an air atmosphere to obtain High specific surface area nanocrystalline magnesium fluoride at high temperature. The textural properties of magnesium fluoride prepared under different magnesium sources, polyol solvents, coagulants, fluorinating reagents, and calcination temperatures are shown in Table 1.

[0025] The magnesium fluoride physicochemical property result of table 1 embodiment 1

[0026]

[0027]

Embodiment 2

[0028] Embodiment 2: Preparation of high specific surface area nanocrystalline magnesium fluoride

[0029] Dissolve 1.0M magnesium nitrate and polyethylene glycol in 50mL of ethylene glycol, reflux at 30°C for 6h, then add HF aqueous solution (40wt.%) dropwise to the above solution while stirring, and the dropping time is After the dropwise addition, stir for 6 hours to obtain a liquid sol; then statically age at 100°C for more than 24 hours to obtain a solid gel; then dry at 140°C for more than 24 hours, and finally roast at 400°C for more than 4 hours to obtain a high-temperature High specific surface area nanocrystalline magnesium fluoride. The textures of magnesium fluoride obtained with different amounts of polyethylene glycol are shown in Table 2.

[0030] The magnesium fluoride physicochemical property result of table 2 embodiment 2

[0031]

Embodiment 3

[0032] Embodiment 3: Preparation of high specific surface area nanocrystalline magnesium fluoride

[0033] Dissolve 1.0M magnesium nitrate and polyethylene glycol (Mg / gelling agent mass ratio is 1:3) in 50mL of ethylene glycol, reflux at 30°C for 6h, then add HF solution dropwise to In the above solution, the dripping time is 30min, after the dripping is completed, stir for 6h to obtain a liquid sol; then statically age at 100°C for more than 24h to obtain a solid gel; then dry at 140°C for more than 24h, and finally dry at 400°C Calcining at lower temperature for more than 4 hours to prepare nanocrystalline magnesium fluoride with high specific surface area at high temperature. The textures of magnesium fluoride prepared with different HF concentrations are shown in Table 3.

[0034] The magnesium fluoride physicochemical property result of table 3 embodiment 3

[0035]

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Abstract

The invention discloses a method for preparing nano-crystal magnesium fluoride with a high specific surface area, which aims at solving the problems that magnesium fluoride preparation has small high-temperature specific surface area and poor stability and an existing preparation method is expensive and complicated and has heavy pollution. The method comprises the following steps: (1) preparing a solution containing magnesium-source precursor, polyhydric alcohol and coagulation accelerator, and refluxing at 20-80 DEG C; (2) fluoridizing the solution obtained in the step (1) with a fluoridizing reagent, and aging at 100-160 DEG C to obtain liquid sol; and (3) drying the liquid sol at 140-200 DEG C to obtain solid gel, and roasting at 350-450 DEG C to obtain nano-magnesium fluoride.

Description

technical field [0001] The invention relates to a magnesium fluoride with high specific surface area, in particular to a mild, simple and environment-friendly preparation method of nanocrystalline magnesium fluoride with large specific surface area at high temperature. Background technique [0002] Magnesium fluoride (MgF 2 ) as an important chemical, optical and catalytic material has a wide range of uses. It can be used as an additive for electrolytic aluminum, a flux for smelting metal magnesium, a coating agent for titanium pigments, and a fluorescent material for cathode ray screens. At the same time, it is also a colorless and transparent infrared optical material with a wide transmission range and high transmittance, and is used to make optical components in infrared optical systems. In addition, MgF 2 It is a catalytic material that can exist stably for a long time under corrosive HF and HCl atmospheres. More importantly, its surface is weak in acid and alkali, an...

Claims

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Application Information

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IPC IPC(8): C01F5/28B01J27/138B82Y30/00B82Y40/00
CPCB01J27/138B82Y30/00B82Y40/00C01F5/28C01P2002/72C01P2004/51C01P2004/64C01P2006/12C01P2006/17
Inventor 毛伟吕剑白彦波王伟杨志强王博郝志军秦越马辉何飞徐强贾兆华
Owner XIAN MODERN CHEM RES INST
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