Preparation method of ultrapure magnesium oxide powder

A technology of magnesium oxide powder and sodium hydroxide, applied in magnesium oxide, magnesium hydroxide and other directions, can solve the problems of low economic and technical competitiveness.

Active Publication Date: 2014-05-14
GANSU KETE OPTICAL TECHNIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the existing high-purity MgO preparation methods include vacuum volatilization method, solvent evaporation method, inert gas evaporation method, liquid phase precipitation method, sol-gel method, alkoxide decomposition method and vapor phase deposition method, etc., and the product purity is usually 98%. -- Between 99.9%, although the organic magnesium salt decomposition method can obtain ultra-pure magnesium oxide, but the economic and technical competitiveness is not strong

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  • Preparation method of ultrapure magnesium oxide powder
  • Preparation method of ultrapure magnesium oxide powder
  • Preparation method of ultrapure magnesium oxide powder

Examples

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Effect test

Embodiment 1

[0025] Add magnesium sulfate heptahydrate into pure water with a conductivity of 1.0 μs / cm to completely dissolve, and prepare a 1.5 mol / L magnesium sulfate solution, filter to remove mechanical impurities and insoluble substances; add 0.0000675 mol / L oxalic acid and keep stirring until complete After the reaction produces calcium oxalate precipitate, let it stand and separate until the upper layer becomes a clear liquid, then filter; add 0.00006mol / L hydrogen peroxide dropwise while stirring continuously, and finish adding dropwise within 0.5h, then continue to react for 1h, and stir fully at the same time And acidify, control pH = 4; add 2mol / L sodium hydroxide and keep stirring, after complete reaction, let it stand for 24 hours, extract the supernatant, add it to the polytetrafluoroethylene reactor, keep stirring and heat up After reaching 68°C, add 3.0 mol / L ammonia water dropwise and keep stirring, and the dropwise addition is completed within 4 hours to obtain a magnesiu...

Embodiment 2

[0027] Add magnesium sulfate heptahydrate into pure water with a conductivity of 1.0μs / cm to dissolve completely, and prepare a 2.0mol / L magnesium sulfate solution, filter to remove mechanical impurities and insoluble substances; add 0.0009mol / L oxalic acid and keep stirring until completely After the reaction produces calcium oxalate precipitate, let it stand and separate until the upper layer becomes clear liquid, then filter; add 0.00008mol / L hydrogen peroxide dropwise under constant stirring, finish adding dropwise within 0.8h, then continue to react for 1.5h, and fully Stir and acidify, control pH = 4; add 2.5mol / L sodium hydroxide and keep stirring, let stand for 48 hours after complete reaction, extract the supernatant, add to the polytetrafluoroethylene reactor, keep stirring and After heating up to 70°C, add 4.0 mol / L ammonia water dropwise and keep stirring, and the dropwise addition is completed within 4 hours to obtain a magnesium hydroxide suspension; after the pro...

Embodiment 3

[0029] Add magnesium sulfate heptahydrate into pure water with a conductivity of 1.0 μs / cm to dissolve completely, and prepare a 2.5mol / L magnesium sulfate solution, filter to remove mechanical impurities and insoluble substances; add 0.0001125mol / L oxalic acid and keep stirring until completely After the reaction produces calcium oxalate precipitate, let it stand and separate until the upper layer becomes clear liquid, then filter; add 0.0001 mol / L hydrogen peroxide dropwise under constant stirring, and finish adding dropwise within 1 hour, then continue to react for 2 hours, at the same time fully stir and Acidification, control pH = 4; add 3mol / L sodium hydroxide and keep stirring, after complete reaction, let it stand for 36 hours, extract the supernatant, add it to the polytetrafluoroethylene reactor, keep stirring and heat up to After 72°C, add 5.0 mol / L ammonia water dropwise and keep stirring, and the dropwise addition is completed within 4 hours to obtain a magnesium h...

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Abstract

The invention discloses a preparation method of ultrapure magnesium oxide powder. The preparation method comprises the following steps of A. dissolving magnesium sulfate heptahydrate in pure water to prepare a magnesium sulfate solution and filtering to remove mechanical impurities and insoluble impurities; B. adding oxalic acid with continuously stirring, ageing repeatedly and carrying out suction filtration to remove calcium impurity; C. dropwise adding hydrogen peroxide into the solution with calcium removed with continuously stirring; D. adding a sodium hydroxide aqueous solution with continuously stirring; standing for stratification after reaction is completed, extracting a supernatant liquid, and removing impurities by a multi-stage precipitation and multi-stage filtration under a normal pressure; and E. putting the filtered clear liquid into a polytetrafluoroethylene reaction kettle, dropwise adding ammonium hydroxide with continuously stirring to obtain a pure magnesium hydroxide turbid liquid, separating a turbid liquid product through centrifugation, washing, filtering, drying, sintering for at least 5 h, and thus ultrapure magnesium oxide powder with a purity of 99.999% can be obtained.

Description

technical field [0001] The invention belongs to the category of inorganic materials in the category of new materials, and specifically relates to a preparation method of ultrapure magnesium oxide powder. Background technique [0002] In China, high-purity magnesium oxide generally refers to W （MgO） ≥98% (weight percent) products, so most of them are used in silicon steel sheet coating, high-temperature insulating materials, advanced ceramics, etc. MgO protective layer plating as the key part of plasma display PDP device is a bottleneck on the plasma display production line. High-purity magnesium oxide (MgO) is widely used in many fields such as electronic components and advanced ceramic materials, especially in the new generation of plasma flat panel display (PDP), its performance directly affects the working characteristics and life of PDP. At present, the purity of MgO mass-produced in China is usually below 99.9%, and the content of impurities such as iron, silicon, cal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/08
CPCC01F5/08C01F5/22C01P2006/80
Inventor 杨松涛张煊铭李洁徐玉江
Owner GANSU KETE OPTICAL TECHNIC MATERIAL
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