CN103787376B - A kind of preparation method of ultra pure magnesium oxide powder - Google Patents

A kind of preparation method of ultra pure magnesium oxide powder Download PDF

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CN103787376B
CN103787376B CN201210423413.1A CN201210423413A CN103787376B CN 103787376 B CN103787376 B CN 103787376B CN 201210423413 A CN201210423413 A CN 201210423413A CN 103787376 B CN103787376 B CN 103787376B
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magnesium oxide
oxide powder
pure
preparation
constantly stirring
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CN103787376A (en
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杨松涛
张煊铭
李洁
徐玉江
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GANSU KETE OPTOELECTRONICS TECHNOLOGY MATERIALS Co Ltd
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GANSU KETE OPTOELECTRONICS TECHNOLOGY MATERIALS Co Ltd
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Priority to PCT/CN2013/085531 priority patent/WO2014067403A1/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/14—Magnesium hydroxide
    • C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a kind of preparation method of ultra pure magnesium oxide powder.It comprises the steps: A, is added in pure water by magnesium sulfate heptahydrate and dissolve completely, is mixed with Adlerika, crosses and filters mechanical impurity and insoluble substance; B, while constantly stirring, add oxalic acid, after reaction aging, suction filtration removing impurity calcium; C, the solution after deliming is dripped hydrogen peroxide while constantly stirring, D, while constantly stirring, add aqueous sodium hydroxide solution, after complete reaction after stratification, extract supernatant liquid, at ambient pressure, adopt multi stage precipitation, cascade filtration method, remove impurity; E, the clear liquid after filtering is entered in tetrafluoroethylene reactor, drip ammoniacal liquor and constantly stir, obtaining pure cerium hydroxide magnesium suspension liquid; After this suspension liquid product centrifugation, after washing and filtering, dry, calcine at least 5h, obtain the ultra pure magnesium oxide powder of 99.999%.

Description

A kind of preparation method of ultra pure magnesium oxide powder
Technical field
The invention belongs to the inorganic materials class in novel material class, specifically a kind of preparation method of ultra pure magnesium oxide powder.
Background technology
At home, high-purity magnesium oxide generally refers to W (MgO)>=98%(weight percent) product, thus the overwhelming majority is applied in the aspects such as coating for silicon steel sheet, high temperature insulating material, advanced ceramic.It is a bottleneck on plasma panel production line that MgO protective layer as plasma panel PDP device critical part is coated with.High purity magnesium oxide (MgO) is widely used in multiple field such as electronic devices and components, advanced ceramic materials, and especially in plasma panel display of new generation (PDP), its performance directly has influence on performance characteristics and the life-span of PDP.The MgO purity of current domestic batch production is usually all below 99.9%, and the foreign matter content severe overweights such as Qi Zhongtie, silicon, calcium, sodium, how low cost prepares high-purity Mg0 becomes the gordian technique that it affects high-end applications.At present, the high-purity MgO preparation method that oneself has has vacuum volatilization method, flux method of evaporation, inert gas evaporation method, liquid-phase precipitation method, sol-gel method, alkoxide decomposition method and vapour deposition process etc., product purity is usually between 98%--99.9%, although organic-magnesium salt decomposition method can obtain ultra pure magnesium oxide, economy and technological competitiveness are not strong.
The existing method preparing ultra pure magnesium oxide powder adopts MAGNESIUM METAL or magnesium alloy to be raw material, it is put into reactor together with a kind of solvent, have auxiliary agent exist and lower than 100 DEG C of conditions under react, the generating rate of presoma is controlled by controlling solid-to-liquid ratio, temperature of reaction, auxiliary dosage and reaction times, gained presoma obtains magnesium oxide product after recovery auxiliary agent, and purity reaches 99.99%.
Another method adopts magnesium chloride as main raw material, adds sodium hydroxide and generate magnesium hydroxide, and obtain magnesium oxide powder after drying calcining, purity reaches 99.99%.
Method for producing high-purity magnesium oxide by whiske selective method is had to be a kind of employing method for producing high-purity magnesium oxide by whiske selective method again, it generates magnesium sulfate with magnesian light burnt powder and sulfuric acid, water reaction, magnesium sulfate reacts generation alkali magnesium sulfate crystal whisker under certain condition with alkaline matter again after refining, again by generating high purity magnesium hydroxide with alkali substance reaction after separation, after high-temperature calcination, obtain high-purity magnesium oxide, purity reaches 99.9%.
Summary of the invention
The object of this invention is to provide the preparation method that a kind of purity is the magnesium oxide powder of 99.999%.
Technical scheme of the present invention is as follows: a kind of preparation method of ultra pure magnesium oxide powder comprises the steps:
A, magnesium sulfate heptahydrate added in pure water and dissolves completely, be mixed with the Adlerika of 1.5 ~ 2.5mol/L, cross and filter mechanical impurity and insoluble substance;
B, while constantly stirring, add the oxalic acid of 0.0000675 ~ 0.0001125mol/L, after reaction aging, suction filtration removing impurity calcium;
C, the solution after deliming is dripped 0.00006 ~ 0.00010mol/L hydrogen peroxide, by Fe while constantly stirring 2+and Ni 2+be converted into Fe 3+and Ni 3+, drip in 0.5 ~ 1h, then continue reaction 1 ~ 2h, fully stir and acidifying, control pH=4 simultaneously;
D, while constantly stirring, add 2 ~ 3mol/L aqueous sodium hydroxide solution, after complete reaction, after complete reaction, after stratification, extract supernatant liquid, at ambient pressure, adopt multi stage precipitation, cascade filtration method, remove Fe respectively 3+, Ni 3+, Mn 2+, Cr 3+, Al 3+impurity;
E, the clear liquid after filtering is entered in tetrafluoroethylene reactor, constantly to stir and after being heated to 68 DEG C-72 DEG C, drip the ammoniacal liquor of 3.0 ~ 5.0mol/L and constantly stirring, drip in 4 ~ 5h, obtain pure cerium hydroxide magnesium suspension liquid; After this suspension liquid product centrifugation, with pure water to pH=8, then use BaCl 2indicator detects without SO 4 2-, with after the tetrafluoroethylene filter paper filtering of 0.1 μm after adopting afterwards, enter baking oven dry 3h at 105 DEG C-115 DEG C, then high-temperature calcination at least 5h at 900 ~ 1000 DEG C, obtains pure zirconia magnesium powder.
As a further improvement on the present invention, in described steps A, pure electrical conductivity of water is 1.0 μ s/cm.
As a further improvement on the present invention, described step C acidifying acid used is dilute sulphuric acid.
As a further improvement on the present invention, described step D adds stratification 24 ~ 48h after aqueous sodium hydroxide solution.
The present invention adopts the magnesium sulfate heptahydrate meeting Chinese Pharmacopoeia to be main raw material, through dedoping step removing calcium, iron, manganese, nickel such as overpickling, oxidation, alkali cleanings, chromium, the impurity such as aluminium, then add precipitation agent and surpassed (height) purity magnesium hydroxide by controlling the condition elements such as stirring velocity, temperature of reaction, reaction times, pH value, again by it after centrifugation, washing, drying, surpassed (height) pure zirconia magnesium powder through high-temperature calcination.
The present invention develops W (MgO)>=99.999%(weight percent) super (height) pure zirconia magnesium powder mainly as the protective layer of plasma panel PDP, PDP MgO material, its impurities affect the brightness of PDP, sharpness and life-span.MgO film is as the medium protective layer of plasma panel; not only can tolerate the shock of plasma sputter, extend the working life of PDP, and firing voltage and the ME for maintenance of glow discharge in cavity can be reduced; improve its luminous intensity, play an important role in PDP working process.In addition, super (height) pure zirconia magnesium also can be used as optical filming material, semiconductor material, high temperature material, high-temperature superconducting thin film substrate, accompanying drawing explanation
Fig. 1 is Institute of Analysis of Lanzhou University examining report front cover;
Fig. 2 is Institute of Analysis of Lanzhou University examining report page 1;
Fig. 3 is Institute of Analysis of Lanzhou University examining report page 2;
Fig. 4 is that Chinese Academy of Space Technology's starting material ensure central branch analysis report.
Embodiment
The following examples can further illustrate the present invention, but do not limit the present invention in any way.
Embodiment 1:
Magnesium sulfate heptahydrate being added specific conductivity is dissolve completely in 1.0 μ s/cm pure water, is mixed with the Adlerika of 1.5mol/L, crosses and filters mechanical impurity and insoluble substance; Add 0.0000675mol/L oxalic acid and constantly stir, after complete reaction oxalic calcium deposit, stratification to upper strata is filter after clear liquid; Dripping the hydrogen peroxide of 0.00006mol/L when constantly stirring, dripping in 0.5h, after then continuing reaction 1h, fully stir and acidifying, control pH=4 simultaneously; Add the sodium hydroxide of 2mol/L and constantly stir, stratification 24h after complete reaction, extract supernatant liquid, be added in tetrafluoroethylene reactor, continuous stirring after being heated to 68 DEG C, drip the ammoniacal liquor of 3.0mol/L and constantly stir, dripping in 4h, obtain magnesium hydroxide suspension liquid; After this suspension liquid product centrifugation, with deionized water wash to about pH=8, then use BaCl 2indicator detects without SO 4 2-, the tetrafluoroethylene filter paper filtering of rear use 0.1 μm, enters baking oven dry 3h at 105 DEG C, and then high-temperature calcination 6h at 900 DEG C.
Embodiment 2:
Magnesium sulfate heptahydrate being added specific conductivity is dissolve completely in 1.0 μ s/cm pure water, is mixed with the Adlerika of 2.0mol/L, crosses and filters mechanical impurity and insoluble substance; Add 0.0009mol/L oxalic acid and constantly stir, after complete reaction oxalic calcium deposit, stratification to upper strata is filter after clear liquid; Dripping the hydrogen peroxide of 0.00008mol/L when constantly stirring, dripping in 0.8h, after then continuing reaction 1.5h, fully stir and acidifying, control pH=4 simultaneously; Add the sodium hydroxide of 2.5mol/L and constantly stir, stratification 48h after complete reaction, extract supernatant liquid, be added in tetrafluoroethylene reactor, continuous stirring after being heated to 70 DEG C, drip the ammoniacal liquor of 4.0mol/L and constantly stir, dripping in 4h, obtain magnesium hydroxide suspension liquid; After this suspension liquid product centrifugation, with deionized water wash to about pH=8, then use BaCl 2indicator detects without SO 4 2-, the tetrafluoroethylene filter paper filtering of rear use 0.1 μm, enters baking oven dry 3h at 112 DEG C, and then high-temperature calcination 5.5h at 950 DEG C.
Embodiment 3:
Magnesium sulfate heptahydrate being added specific conductivity is dissolve completely in 1.0 μ s/cm pure water, is mixed with the Adlerika of 2.5mol/L, crosses and filters mechanical impurity and insoluble substance; Add 0.0001125mol/L oxalic acid and constantly stir, after complete reaction oxalic calcium deposit, stratification to upper strata is filter after clear liquid; Dripping the hydrogen peroxide of 0.0001mol/L when constantly stirring, dripping in 1h, after then continuing reaction 2h, fully stir and acidifying, control pH=4 simultaneously; Add the sodium hydroxide of 3mol/L and constantly stir, stratification 36h after complete reaction, extract supernatant liquid, be added in tetrafluoroethylene reactor, continuous stirring after being heated to 72 DEG C, drip the ammoniacal liquor of 5.0mol/L and constantly stir, dripping in 4h, obtain magnesium hydroxide suspension liquid; After this suspension liquid product centrifugation, with deionized water wash to about pH=8, then use BaCl 2indicator detects without SO 4 2-, the tetrafluoroethylene filter paper filtering of rear use 0.1 μm, enters baking oven dry 3h at 110 DEG C, and then high-temperature calcination 5h at 1000 DEG C.
Purity detecting is tested
One, carry out relevant purity detection to embodiment 1, conclusion is as follows:
Adopt JY/T1996 to feel lotus root plasma emissioning light method general rule of diving and detect calcium, iron level, conclusion is as follows:
ω Ca=2.6mg／kg(0.00026%)
ω Fe=0.9mg／kg(0.0000097%)
JY/T015-1996 feels lotus root plasma emission spectroscopy method general rule and detects manganese, nickel, chromium, aluminium content, and conclusion is as follows:
Mn0.15mg／kg(0.000015%)
Ni≤0.34mg／kg(0.000034%)
Cr≤0.38mg／kg(0.000038%)
Al≤0.44mg／kg(0.000044%)
Obtain according to above detection: foreign matter content is 0.00083%, and magnesia powder body burden is 99.99917%.
Two, carry out relevant purity detection to embodiment 2, conclusion is as follows:
Adopt JY/T1996 to feel lotus root plasma emissioning light method general rule of diving and detect calcium, iron level, conclusion is as follows:
ω Ca=2.4mg／kg(0.00024%)
ω Fe=0.99mg／kg(0.0000099%)
JY/T015-1996 feels lotus root plasma emission spectroscopy method general rule and detects manganese, nickel, chromium, aluminium content, and conclusion is as follows:
Mn0.16mg／kg(0.000016%)
Ni≤0.35mg／kg(0.000035%)
Cr≤0.35mg／kg(0.000035%)
Al≤0.42mg／kg(0.000042%)
Obtain according to above detection: foreign matter content is 0.000377%, and magnesia powder body burden is 99.99962%.
Three, carry out relevant purity detection to embodiment 3, conclusion is as follows:
Adopt JY/T1996 to feel lotus root plasma emissioning light method general rule of diving and detect calcium, iron level, conclusion is as follows:
ω Ca=2.5mg／kg(0.00025%)
ω Fe=1.0mg／kg(0.00001%)
JY/T015-1996 feels lotus root plasma emission spectroscopy method general rule and detects manganese, nickel, chromium, aluminium content, and conclusion is as follows:
Mn0.15mg／kg(0.000015%)
Ni≤0.37mg／kg(0.000037%)
Cr≤0.35mg／kg(0.000035%)
Al≤0.43mg／kg(0.000043%)
Obtain according to above detection: foreign matter content is 0.00039%, and magnesia powder body burden is 99.99961%.
product of the present invention is detected by Institute of Analysis of Lanzhou University of the Ministry of Education of the state, and front cover and page 1 content are shown in Fig. 1, Fig. 2.
Institute of Analysis of Lanzhou University examining report page 2 content is shown in Fig. 3.
Chinese Academy of Space Technology's starting material ensure that central branch analysis report content is shown in Fig. 4.

Claims (4)

1. a preparation method for ultra pure magnesium oxide powder, is characterized in that it comprises the steps:
A, magnesium sulfate heptahydrate added in pure water and dissolves completely, be mixed with the Adlerika of 1.5 ~ 2.5mol/L;
B, while constantly stirring, add the oxalic acid of 0.0000675 ~ 0.0001125mol/L, after reaction aging, suction filtration removing impurity calcium;
C, the solution after deliming is dripped 0.00006 ~ 0.00010mol/L hydrogen peroxide while constantly stirring, drip in 0.5 ~ 1h, then continue reaction 1 ~ 2h, fully stir and acidifying, control pH=4 simultaneously;
D, while constantly stirring, add 2 ~ 3mol/L aqueous sodium hydroxide solution, after complete reaction after stratification, extract supernatant liquid, at ambient pressure, adopt multi stage precipitation, cascade filtration method, remove Fe respectively 3+, Ni 3+, Mn 2+, Cr 3+, Al 3+impurity;
E, the clear liquid after filtering is entered in tetrafluoroethylene reactor, constantly to stir and after being heated to 68 DEG C-72 DEG C, drip the ammoniacal liquor of 3.0 ~ 5.0mol/L and constantly stirring, drip in 4 ~ 5h, obtain pure cerium hydroxide magnesium suspension liquid; After this suspension liquid product centrifugation, with pure water to pH=8, then use BaCl 2indicator detects without SO 4 2-, after adopting the tetrafluoroethylene filter paper filtering of 0.1 μm afterwards, enter baking oven dry 3h at 105 DEG C-115 DEG C, then high-temperature calcination at least 5h at 900 ~ 1000 DEG C, obtains pure zirconia magnesium powder.
2. the preparation method of a kind of ultra pure magnesium oxide powder according to claim 1, is characterized in that: in described steps A, pure electrical conductivity of water is 1.0 μ s/cm.
3. the preparation method of a kind of ultra pure magnesium oxide powder according to claim 1 and 2, is characterized in that: described step C acidifying acid used is dilute sulphuric acid.
4. the preparation method of a kind of ultra pure magnesium oxide powder according to claim 3, is characterized in that: described step D adds stratification 24 ~ 48h after aqueous sodium hydroxide solution.
CN201210423413.1A 2012-10-30 2012-10-30 A kind of preparation method of ultra pure magnesium oxide powder Active CN103787376B (en)

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PCT/CN2013/085531 WO2014067403A1 (en) 2012-10-30 2013-10-20 Method for preparing ultrapure magnesia powder

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CN104386718A (en) * 2014-11-03 2015-03-04 苏州市泽镁新材料科技有限公司 Method for preparing magnesium hydrate
CN104709927B (en) * 2014-12-30 2017-02-01 上海实业振泰化工有限公司 Preparation method of silicon-steel grade magnesium oxide
CN112661178A (en) * 2020-12-25 2021-04-16 山东信能达工程科技有限公司 Preparation and production process of high-purity magnesium oxide

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CN102398911A (en) * 2010-09-13 2012-04-04 北京有色金属研究总院 Preparation method for high purity magnesium oxide powder
CN102275957A (en) * 2011-07-18 2011-12-14 南京航空航天大学 Process for producing high purity magnesium oxide with dolomite
CN102701240A (en) * 2012-05-10 2012-10-03 昆明理工大学 Method for preparing silicon-steel-grade magnesium oxide from magnesium sulfate waste liquor

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