Method for preparing ultrafine magnesium fluoride

A technology of fine magnesium fluoride and sodium fluoride, applied in the field of preparation of ultra-fine magnesium fluoride, can solve the problem of uneven particle size of MgF2, failure to reach the main content of ultra-fine magnesium fluoride not less than 99%, and difficult washing Filter to remove impurities and other problems, to avoid gelation, reduce reaction supersaturation, and solve the effect of easy gelation

Active Publication Date: 2018-08-21
湖南新晶富新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since this document uses high temperature conditions, NaF solution and MgCl 2 The solution directly reacts in the liquid-liquid phase without adding any seed crystals, so the generated MgF 2 The particles are extremely fine, only 1-2 μm, and it is difficult to wash and filter to remove impurities, resulting in high impurity content, which cannot meet the requirement that the main content of ultra-fine magnesium fluoride products should not be less than 99%.
[0006] In addition, although the purity of the existing high-purity magnesium fluoride can reach more than 99.9%, it has no requirement on the particle size of the product, and the obtained MgF 2 The particle size is uneven, and it cannot meet the requirements of D50 between 5 and 15 μm and D97 less than 30 μm

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  • Method for preparing ultrafine magnesium fluoride
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Embodiment 1

[0023] The preparation method of the present invention comprises the following steps:

[0024] (1) Preparation of saturated sodium fluoride solution: Add 42 g of granular sodium fluoride with a particle size of 0.5 to 0.8 mm into 360 mL of water, place it in a constant temperature water bath at 10°C, and stir until the sodium fluoride solid no longer dissolves, that is, Obtain a saturated sodium fluoride solution, which also contains undissolved sodium fluoride solid;

[0025] (2) Synthetic reaction: in step (1) gained saturated sodium fluoride solution, slowly drip 475g mass fraction into the magnesium chloride solution of 10%, the time of dropping is 1h, stir constantly, control stirring speed 300r / min, after feeding finishes Continue to react for 1 h to obtain a suspension;

[0026] (3) Washing and drying: filter and wash the suspension obtained in step (2), and dry at 70° C. for 9 hours to obtain ultrafine magnesium fluoride powder that is easy to disperse and has uniform...

Embodiment 2

[0028] The preparation method of the present invention comprises the following steps:

[0029] (1) Preparation of saturated sodium fluoride solution: Add 42 g of granular sodium fluoride with a particle size of 0.5 to 0.8 mm into 360 mL of water, place it in a constant temperature water bath at 15°C, and stir until the solid sodium fluoride no longer dissolves, that is, Obtain a saturated sodium fluoride solution, which also contains undissolved sodium fluoride solid;

[0030] (2) Synthetic reaction: Slowly add 316.7g of magnesium chloride solution with a mass fraction of 15% in the saturated sodium fluoride solution obtained in step (1), the time for the addition is 1h, keep stirring, control the stirring speed at 350r / min, and the feeding ends Then continue to react for 2h to obtain a suspension;

[0031] (3) Washing and drying: filter and wash the suspension obtained in step (2), and dry at 80° C. for 8 hours to obtain ultrafine magnesium fluoride powder that is easy to di...

Embodiment 3

[0033] The preparation method of the present invention comprises the following steps:

[0034] (1) Preparation of saturated sodium fluoride solution: Add 42 g of granular sodium fluoride with a particle size of 0.2 to 0.5 mm into 324 mL of water, place it in a constant temperature water bath at 20°C, and stir until the solid sodium fluoride no longer dissolves, that is, Obtain a saturated sodium fluoride solution, which also contains undissolved sodium fluoride solid;

[0035] (2) Synthetic reaction: Slowly add 237.5g of magnesium chloride solution with a mass fraction of 20% in the saturated sodium fluoride solution obtained in step (1), the time for the addition is 1h, keep stirring, control the stirring speed at 300r / min, and the feeding ends Then continue to react for 1 h to obtain a suspension;

[0036] (3) Washing and drying: filter and wash the suspension obtained in step (2), and dry at 65° C. for 10 hours to obtain ultrafine magnesium fluoride powder that is easy to di...

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Abstract

The invention discloses a method for preparing ultrafine magnesium fluoride. The method includes steps of firstly, dissolving excessive sodium fluoride with the particle size of 0.2-1.0 mm in water toobtain solution, placing the solution in constant-temperature water bath kettles and carrying out water bath at the water bath temperature of 5-20 DEG C under the control to obtain saturated sodium fluoride solution with undissolved sodium fluoride particles; secondly, completely dropwise adding, by weight, 10-25% of magnesium chloride solution into the saturated sodium fluoride solution in 1-2 h, continuously stirring the magnesium chloride solution and the saturated sodium fluoride solution, and continuously carrying out reaction for 1-2 h after the magnesium chloride solution is completelydropwise added into the saturated sodium fluoride solution so as to obtain suspension; thirdly, filtering, washing and drying the suspension to obtain the ultrafine magnesium fluoride. A molar ratioof magnesium chloride to sodium fluoride is 0.5:1. The method has the advantages that the purity of the ultrafine magnesium fluoride prepared by the aid of the method is higher than 99.0%, the impurity content of the ultrafine magnesium fluoride is lower than 0.01%, the D50 particle size of the ultrafine magnesium fluoride is 5-15 micrometers, and the D97 particle size of the ultrafine magnesium fluoride is smaller than 30 micrometers.

Description

technical field [0001] The invention relates to a preparation process of magnesium fluoride, in particular to a preparation method of ultrafine magnesium fluoride. Background technique [0002] The infrared transmittance of the magnesium fluoride polycrystal can reach more than 90% in the mid-wave infrared band of 3-5 μm and the thickness of 2 mm, which is the highest among the existing infrared materials. Magnesium fluoride polycrystalline also has many characteristics such as high mechanical strength, strong thermal shock resistance, chemical corrosion resistance and isotropy, and its dielectric constant and dielectric loss are small, so it is a good medium-wave infrared window and dome Materials and mid-wave infrared / millimeter wave (microwave) composite radome materials are widely used in infrared guidance, infrared imaging guidance, infrared / millimeter wave (microwave) composite guidance, and infrared tracking, detection, and guidance of aircraft infrared pods and photo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/28
CPCC01F5/28C01P2004/61C01P2006/80
Inventor 罗小平陈新文
Owner 湖南新晶富新材料有限公司
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