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WO2020195721A1 - Poudre de spinelle - Google Patents

Poudre de spinelle Download PDF

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Publication number
WO2020195721A1
WO2020195721A1 PCT/JP2020/009766 JP2020009766W WO2020195721A1 WO 2020195721 A1 WO2020195721 A1 WO 2020195721A1 JP 2020009766 W JP2020009766 W JP 2020009766W WO 2020195721 A1 WO2020195721 A1 WO 2020195721A1
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Prior art keywords
mass
purity
spinel
less
powder
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PCT/JP2020/009766
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English (en)
Japanese (ja)
Inventor
善久 大崎
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Tateho Chemical Industries Co Ltd
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Tateho Chemical Industries Co Ltd
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Priority to JP2021508948A priority Critical patent/JP7585191B2/ja
Priority to CN202080034405.0A priority patent/CN113784923B/zh
Priority to KR1020217033898A priority patent/KR102886992B1/ko
Publication of WO2020195721A1 publication Critical patent/WO2020195721A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C04B35/443—Magnesium aluminate spinel
    • 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
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
    • 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
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/162—Magnesium aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/30—Three-dimensional structures
    • C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • 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

Definitions

  • the present invention relates to spinel powder.
  • the present invention relates to magnesium aluminate spinel powder.
  • Magnesium aluminate spinel which chemical composition is represented by MgAl 2 O 4 (MgO-Al 2 O 3 spinel, hereinafter referred to as "spinel") is a sintered ceramic having excellent thermal stability and chemical stability As a body, it is used in various fields. Examples of applications of ceramic sintered bodies using this spinel include optical materials, heat-resistant containers, insulating materials, catalyst carriers, adsorbents, supports, and coating materials.
  • a ceramic sintered body using spinel is obtained by sintering spinel powder. It is known that trace elements contained in spinel powder affect the characteristics of ceramic sintered bodies used in various applications.
  • Patent Document 1 The Kohyo 2018-501178 (Patent Document 1), MgO and at least 0.1 wt% of the dopant, and a Al 2 O 3, sintering total impurities content of less than 0.7 wt% Ceramic components are disclosed.
  • Patent Document 2 proposes fusion particles consisting of a matrix of magnesium aluminum oxide MgAl 2 O 4 and / or Mg O-Mg Al 2 O 4 eutectic mixture having a spinel structure. More than 95.0% of the weight of the fused particles shows the chemical composition of Al 2 O 3 and Mg O, and the cumulative content of CaO and ZrO 2 is less than 4000 mass ppm.
  • Patent Document 3 discloses a gas nozzle including a main body made of a spinel sintered body. This spinel sintered body contains 90% by mass or more and 99.9% by mass or less of magnesium aluminate as a main component, and 0.1% by mass or more and 10% by mass or less of Ca, Mg or Zr as a sintering aid. Includes.
  • WO2013 / No. 038916 Patent Document 4
  • Zn and K content of each ZnO and K 2 magnesium aluminate total in terms of 30ppm or 500ppm or less in O sintered body have been proposed. Patent Document 4 describes that the total contents of Si, Ca and P are controlled to 500 ppm or more and 2500 ppm or less in terms of SiO 2 , Ca O and P 2 O 5 , respectively.
  • Patent Document 5 The JP 62-72556 (Patent Document 5), and calcining the coprecipitate obtained by alkoxide coprecipitation obtain highly pure MgAl 2 O 4 material purity of 99.9% or more techniques Is disclosed.
  • Patent Document 6 a slurry obtained by adding a pH-adjusted alumina dispersion to an aqueous dispersion of a magnesium compound is dried and then calcined to produce magnesium aluminate spinel. Technology has been proposed.
  • Patent Document 7 describes a magnesium oxide-containing spinel powder having a step of mixing magnesium source particles having a predetermined particle size and aluminum source particles and then calcining them at 900 to 1400 ° C. The manufacturing method is disclosed.
  • Patent Documents 5 and 6 have a problem that the operation becomes complicated and it is difficult to control the particle size. Further, since the method of Patent Document 5 uses an expensive alkoxide, there is a problem in terms of cost.
  • the obtained spinel is highly purified by using high-purity magnesium source particles and aluminum source particles as raw materials.
  • trace elements which are impurities, promote the formation of MgAl 2 O 4 by calcination.
  • a raw material having a purity of 99.95% by mass or more is used, this accelerating effect cannot be obtained, so that sufficient spinelization is difficult at a firing temperature of about 900 to 1400 ° C.
  • Spinelization may proceed by firing at a high temperature of 1600 ° C.
  • An object of the present invention is to provide a spinel powder having high purity and not deteriorating activity due to high-temperature firing, and a method for producing the same.
  • the purity of the spinel powder according to the present invention is 99.95% by mass or more.
  • the spinel powder, the content of Mg and Al represented by oxide conversion is less 78 mass% 9 mass% or more as MgO, is for Al 2 O 3 22 wt% or more 91 wt% or less.
  • the purity of this spinel powder is 99.99% by mass or more.
  • the Ca content of this spinel powder is less than 30 ppm, and the Si content is less than 30 ppm.
  • the total content of elements other than Mg, Al and O in this spinel powder is less than 500 ppm.
  • a magnesium source having a purity of 99.95% by mass or more and an aluminum source having a purity of 99.95% by mass or more are subjected to a solid phase reaction at a reaction temperature of 1500 ° C. or less. It is a powder made of aluminum.
  • the present invention relates to a method for producing this spinel powder.
  • This production method is a mixing step of (1) mixing a magnesium source having a purity of 99.95% by mass or more and an aluminum source having a purity of 99.95% by mass or more to obtain a mixed powder.
  • the magnesium source and the aluminum source are powders composed of a large number of particles, respectively.
  • the ratio D50 (1) / D50 (2) of the volume-based cumulative 50% particle diameter D50 (1) of this magnesium source to the volume-based cumulative 50% particle diameter D50 (2) of this aluminum source is 0. It is 2 or more and 5.0 or less.
  • this pulverization step is performed by wet pulverization.
  • the purity of the spinel powder according to the present invention is 99.95% by mass or more.
  • This spinel powder is obtained by a method of mixing a magnesium source and an aluminum source and then firing at a temperature of 1500 ° C. or lower.
  • This spinel powder does not decrease in activity due to high-temperature firing and has a sufficiently low content of impurity elements, so that it is suitably used for various applications requiring high purity.
  • spinel is a magnesium aluminate spinel having a chemical composition of MgAl 2 O 4 , and is a two-component compound of Mg O-Al 2 O 3 .
  • the spinel powder according to the present invention does not have a magnesium oxide matrix and an aluminum oxide matrix separated as in a simple mixture of magnesium oxide and aluminum oxide, but a composite of magnesium and aluminum in whole or in part. Oxides are formed and it has a more uniform composition.
  • the purity of the spinel powder according to the present invention is 99.95% by mass or more, preferably 99.99% by mass or more.
  • the purity refers to a value obtained by subtracting the content of impurities contained in the spinel powder from 100%.
  • the spinel powder having a purity of 99.95% by mass or more contains elements other than Mg, Al and O, that is, impurities, which are sufficiently smaller than those of the conventional spinel powder. According to this spinel powder, the variation in the coefficient of thermal expansion of the obtained ceramic sintered body is reduced. Further, by using this spinel powder, a highly transparent ceramic sintered body can be obtained. This spinel powder is suitably used for various applications in which high purity of 99.95% by mass or more is required.
  • the content of Mg and Al represented by oxide conversion is less 78 mass% 9 mass% or more as MgO, are for Al 2 O 3 22 wt% or more 91 wt% or less .
  • the ceramics sintered body obtained by using the spinel powder within this range can be imparted with various properties required for various uses.
  • the content of Mg and Al is preferably not more than 70 wt% or more 12 wt% as MgO, Al 2 O 3 as not more than 30 wt% or more 88 wt%, more preferably, a MgO It is 14% by mass or more and 61% by mass or less, and 39% by mass or more and 86% by mass or less as Al 2 O 3 .
  • the stoichiometric ratio of Mg to Al in this spinel powder is in the range of 9: 1 to 2: 8.
  • the coefficient of thermal expansion increases as the proportion of Mg increases, and the spalling resistance tends to decrease. If the proportion of Mg is low, the corrosion resistance may decrease. Further, as the proportion of Al increases, the hardness of the spinel powder increases, so that the possibility of impurities being mixed during pulverization increases. The method for measuring the content of Mg and Al will be described later in Examples.
  • the spinel powder may contain elements other than Mg, Al and O as long as the effects of the present invention are not impaired.
  • elements other than Mg, Al and O contained in the spinel powder include Ca, Si, Fe, Mn, Ni, Cu, Zn and Na.
  • P, S, B, Ti, Zr, Ba and the like may be included.
  • the Ca content of this spinel powder is less than 30 ppm, and the Si content is less than 30 ppm.
  • the Ca content is more preferably 25 ppm or less, further preferably 20 ppm or less.
  • the Si content is more preferably 25 ppm or less, further preferably 20 ppm or less.
  • the total content of elements other than Mg, Al and O in this spinel powder is less than 500 ppm.
  • the total content of elements other than Mg, Al and O is in this range, a high purity of 99.95% by mass or more is achieved.
  • the total content of elements other than Mg, Al and O is more preferably 100 ppm or less, further preferably 70 ppm or less.
  • the total content is determined as the total content of elements other than Mg, Al and O.
  • the type of this "other element” is not particularly limited, and elements other than Mg, Al and O detected by the measurement method described later in the examples are used as "other elements” in the calculation of the total content. Be done.
  • Specific examples of the "other element” include Ca, Si, Fe, Mn, Ni, Cu, Zn, Na, P, S, B, Ti, Zr, Ba and the like.
  • this spinel powder is prepared by mixing a magnesium source having a purity of 99.95% by mass or more as a raw material and an aluminum source having a purity of 99.95% by mass or more and then subjecting them to a solid phase reaction at a temperature of 1500 ° C. or less. It is a product. In a solid phase reaction at 1500 ° C. or lower, strong sintering of the obtained spinel powder is suppressed.
  • This spinel powder avoids the inclusion of impurities due to strong crushing and crushing after firing. Further, since this spinel powder is not subjected to excessive high temperature treatment, activities such as sinterability can be maintained.
  • This manufacturing method includes a mixing step, a crushing step, and a firing step.
  • the mixing step is a step of mixing a magnesium source having a purity of 99.95% by mass or more and an aluminum source having a purity of 99.95% by mass or more to obtain a mixed powder.
  • the pulverization step is a step of pulverizing the mixed powder to obtain a precursor.
  • the firing step is a step of firing this precursor at a temperature of 1500 ° C. or lower.
  • This manufacturing method may include a particle size adjusting step after the firing step. As long as the object of the present invention is achieved, this manufacturing method may include further other steps.
  • the purity of the magnesium source used as a raw material is 99.95% by mass or more.
  • a magnesium source of this purity high purity of the obtained spinel powder is achieved.
  • the purity of the preferred magnesium source is 99.99% by mass or more.
  • the type of magnesium source is not particularly limited as long as the effect of the present invention is not inhibited.
  • Specific examples of the magnesium source include magnesium hydroxide, magnesium oxide, magnesium carbonate, basic magnesium carbonate, magnesium nitrate, magnesium acetate, magnesium sulfate and the like.
  • Magnesium hydroxide and magnesium oxide are preferable, and magnesium hydroxide is more preferable.
  • Magnesium hydroxide changes to magnesium oxide with a high specific surface area during calcination. The presence of this high specific surface area of magnesium oxide around the aluminum source promotes the formation reaction of MgAl 2 O 4 , and sufficient spinelization is achieved in a relatively low calcination temperature region.
  • the method for producing a magnesium source having a purity of 99.95% by mass or more is not particularly limited.
  • a method for producing magnesium hydroxide having a purity of 99.95% by mass or more an alkaline aqueous solution such as ammonia, calcium hydroxide, or sodium hydroxide is added to a magnesium chloride-containing aqueous solution, reacted, and then dried.
  • a method of obtaining magnesium hydroxide powder can be mentioned.
  • the magnesium oxide powder obtained by calcining the magnesium hydroxide powder thus obtained and then pulverizing it to a desired particle size can also be used as a magnesium source.
  • a method of obtaining magnesium oxide powder by a vapor phase method of burning and oxidizing metallic magnesium can be mentioned.
  • the magnesium source is preferably a powder composed of a large number of fine particles.
  • the cumulative 50% particle diameter D50 (1) on a volume basis is 0.1 ⁇ m or more and 1.0 ⁇ m or less.
  • the volume-based cumulative 50% particle size D50 (1) of the magnesium source is more preferably 0.2 ⁇ m or more and 0.9 ⁇ m or less, and further preferably 0.2 ⁇ m or more and 0.8 ⁇ m or less. The method for measuring the cumulative 50% particle diameter D50 (1) based on the volume of the magnesium source will be described later in Examples.
  • the purity of the aluminum source used as a raw material is 99.95% by mass or more.
  • the purity of the preferred aluminum source is 99.99% by mass or more.
  • the type of aluminum source is not particularly limited as long as the effect of the present invention is not impaired.
  • Specific examples of the aluminum source include aluminum hydroxide, aluminum oxide, aluminum carbonate, aluminum nitrate, aluminum acetate, aluminum sulfate and the like.
  • a preferred aluminum source is aluminum oxide.
  • the method for producing an aluminum source having a purity of 99.95% by mass or more is not particularly limited.
  • a method for producing aluminum hydroxide having a purity of 99.95% by mass or more for example, bauxite is reacted with an aqueous sodium hydroxide solution under pressure and heating, and then the obtained solution is filtered to be aluminum.
  • a method of obtaining aluminum hydroxide by extracting a sodium hydroxide solution and cooling it can be mentioned.
  • aluminum oxide obtained by firing the aluminum hydroxide thus obtained and then pulverizing it to a desired particle size can also be used as an aluminum source.
  • the aluminum source is preferably a powder composed of a large number of fine particles.
  • the cumulative 50% particle diameter D50 (2) on a volume basis is 0.1 ⁇ m or more and 1.0 ⁇ m or less.
  • the volume-based cumulative 50% particle diameter D50 (2) of the aluminum source is more preferably 0.2 ⁇ m or more and 0.9 ⁇ m or less, and further preferably 0.2 ⁇ m or more and 0.8 ⁇ m or less. The method for measuring the cumulative 50% particle diameter D50 (2) based on the volume of the aluminum source will be described later in Examples.
  • the ratio D50 (1) / D50 (2) of the particle size D50 (1) of the magnesium source to the particle size D50 (2) of the aluminum source is 0.2 or more and 5.0 or less.
  • the mixing step by mixing the magnesium source and the aluminum source having a ratio of D50 (1) / D50 (2) within this range, a mixed powder having a relatively uniform particle size distribution is obtained.
  • the particle size distribution of the precursor (mixture before firing) obtained by pulverizing this mixed powder is also uniform.
  • the reaction between the magnesium source and the aluminum source proceeds at a relatively low firing temperature, and the formation of a spinel phase is promoted.
  • the ratio D50 (1) / D50 (2) is more preferably 0.4 or more and 4.0 or less, and particularly preferably 0.3 or more and 3.0 or less.
  • the blending ratio of the magnesium source and the aluminum source to be mixed in the mixing step is adjusted so that the content of Mg and Al (also referred to as composition ratio) of the obtained spinel powder is within the above-mentioned range.
  • the method of mixing the magnesium source and the aluminum source is not particularly limited, and a known mixing device is appropriately selected and used. Specific examples thereof include a container rotary mixer such as a V-type mixer, a ribbon mixer, a Henschel mixer, a professional share mixer, a super mixer, a dry ball mill and the like. It is preferable to mix as uniformly as possible.
  • the mixed powder obtained in the mixing step is crushed to a predetermined particle size in the powder step before firing. This grinding step further promotes the formation of spinel phases in the relatively low firing temperature range.
  • the method for pulverizing the mixed powder is not particularly limited, and wet pulverization or dry pulverization may be used. Wet pulverization is preferable from the viewpoint that a more uniform particle size distribution can be easily obtained.
  • the mixed powder is pulverized in a state of being dispersed in a solvent. Examples of the solvent used include water and alcohol. Water and alcohol may be mixed and used.
  • crushers used in the crushing process include jaw crushers, cone crushers, impact crushers, roll crushers, cutter mills, stamp mills, ring mills, jet mills, hammer mills, pin mills, ball mills, vibration mills, bead mills, cyclone mills, etc. Can be mentioned.
  • the crushing conditions are not particularly limited.
  • a desired particle size distribution can be achieved by appropriately adjusting the pulverization time, rotation speed, etc. according to the particle size of the mixed powder, the type of pulverization apparatus used, and the like.
  • the mixed powder after pulverization is subjected to the firing step as a precursor (mixture before firing).
  • the particle size of the precursor used in the firing step is not particularly limited.
  • the cumulative 50% particle size (D50) based on the volume as the particle size of the precursor is 0.1 ⁇ m or more. It is preferably 0 ⁇ m or less, more preferably 0.2 ⁇ m or more and 0.9 ⁇ m or less, and further preferably 0.2 ⁇ m or more and 0.8 ⁇ m or less.
  • the particle size of the precursor is measured by the same method as for the magnesium source and the aluminum source.
  • a pulverized product slurry containing the mixed powder after pulverization and the solvent can be obtained.
  • the pulverized slurry is dried to remove the solvent, and the dry powder is used as a precursor in the firing step.
  • the method for drying the pulverized slurry is not particularly limited, and a known dryer such as a vacuum dryer, a spray dryer, or a freeze dryer is appropriately selected and used.
  • the drying method is also not particularly limited, and is adjusted according to the drying apparatus to be used and the properties of the pulverized slurry.
  • the temperature at which the precursor is fired in the firing step is 1500 ° C. or lower.
  • a spinel raw material in which magnesium oxide and aluminum oxide are compounded can be obtained.
  • the firing temperature is 1500 ° C. or lower, strong sintering does not occur after firing, so that the possibility of foreign matter being mixed during the crushing operation is reduced.
  • the firing temperature is preferably 1500 ° C. or lower, more preferably 1470 ° C. or lower, and even more preferably 1450 ° C. or lower.
  • the preferred firing temperature is 1400 ° C. or higher.
  • the firing time is appropriately adjusted according to the firing temperature. For example, when the temperature is 1450 ° C. or higher and 1500 ° C. or lower, the preferable firing time is 1 hour or more and 12 hours or less, and when the temperature is 1400 ° C. or higher and 1450 ° C. or lower, the preferable firing time is 3 hours or more and 18 hours or less. By setting the firing time within this range, the spinel phase is sufficiently formed and strong sintering is avoided.
  • a firing container is usually used for firing the precursor.
  • the type of the firing container is not particularly limited, and general members such as an alumina saggar and a magnesia saggar are used.
  • the top surface of the firing container into which the precursor is charged is covered with a lid.
  • the material of the firing container and the lid is preferably high-purity magnesia having a purity of 99.99% by mass or more.
  • the device used for firing is not particularly limited as long as it can be fired at 1500 ° C. or lower.
  • Known firing furnaces such as a box furnace, a stove furnace, a tube furnace, a tunnel furnace, a vacuum furnace, a bottom elevating furnace, a resistance heating furnace, an induction heating furnace, and a direct electric furnace can be used.
  • Spinel powder may be obtained by crushing or crushing the spinel raw material obtained in the firing step to adjust the particle size and particle size distribution.
  • crushing or crushing for example, jaw crusher, gyre crusher, cone crusher, impact crusher, roll crusher, cutter mill, stamp mill, ring mill, roller mill, jet mill, hammer mill, rotary mill, vibration mill, planetary A crusher such as a mill, a ball mill, or a cyclone mill can be used.
  • the crushing or crushing conditions are not particularly limited, and are appropriately adjusted according to the type of equipment used, the composition and particle size of the precursor, the firing conditions, and the like. For example, by adjusting the number of revolutions during crushing and crushing, the processing time, and the like, contamination of impurities is avoided and the purity of the spinel powder is maintained. As a result, a high-purity spinel powder having a desired particle size and particle size distribution can be obtained. For example, when crushing using a dry ball mill, the preferable crushing time is 24 hours, and the preferable rotation speed is 80 rpm.
  • composition ratio of spinel powder The composition of the spinel powder was analyzed by the glass bead method using a multi-element simultaneous fluorescent X-ray analyzer (trade name "Simultex 12" manufactured by Rigaku Co., Ltd.). The contents of Al and Mg were calculated in terms of oxides, and the composition ratio of MgO and Al 2 O 3 was determined.
  • Magnesium oxide and aluminum oxide were measured using a multi-element simultaneous fluorescent X-ray analyzer (trade name "Simultex 12" manufactured by Rigaku Co., Ltd.). The purity of magnesium oxide and aluminum oxide was determined by converting the total content (ppm) of the detected elements other than Mg, Al and O into% and subtracting it from 100%.
  • the main elements other than the detected Mg and Al were Ca, Si, Fe, Mn, Ni, Cu, and Zn.
  • Example 1 A magnesium chloride aqueous solution adjusted to have a Mg ion concentration of 2.0 mol / L and a sodium hydroxide aqueous solution adjusted to a concentration of 2.7 mol / L are sent to a reaction vessel by a metering pump, respectively, and combined. The reaction was carried out. The reaction rate of sodium hydroxide with magnesium chloride was controlled to be 90 mol%. The obtained reaction slurry was overflowed from the reaction tank with a residence time of 30 minutes and recovered. This reaction slurry (magnesium hydroxide slurry) was filtered, washed with water, and dried to obtain a dry magnesium hydroxide powder. The purity of the obtained dry magnesium hydroxide powder was 99.99% or more, and the cumulative 50% particle size (D50) on a volume basis was 0.58 ⁇ m.
  • magnesium hydroxide dry powder obtained by the above method aluminum hydroxide powder having a purity of 99.99% or more and a volume-based cumulative 50% particle diameter (D50) of 0.20 ⁇ m is added to the composition ratio of Mg and Al.
  • D50 volume-based cumulative 50% particle diameter
  • the obtained mixed powder and solvent (industrial alcohol) were filled in a pot mill (filling rate 35%) so as to have a mass ratio of 1: 1 and wet pulverized by a ball mill (rotation speed 80 rpm / 24 hours). .. Then, the slurry of the contents was recovered and sufficiently dried in an explosion-proof dryer to obtain a pre-baking mixture (precursor).
  • This pre-baking mixture was filled in a square alumina saggar, fired at 1400 ° C. for 3 hours, and then cooled to obtain a spinel raw material.
  • the spinel raw material and the solvent (industrial alcohol) were filled in a pot mill (filling rate 35%) so as to have a mass ratio of 1: 1 and wet pulverized by a ball mill (rotation speed 80 rpm / 24 hours).
  • the slurry of the contents was collected, passed through a 500 mesh sieve, and then dried in an explosion-proof dryer to obtain the spinel powder of Example 1.
  • Table 1 The composition ratio, particle size and purity of the spinel powder of Example 1 are shown in Table 1 below.
  • the contents and total contents of various elements in this spinel powder are shown in Table 2 below.
  • Comparative Example 1 A spinel powder of Comparative Example 1 was obtained in the same manner as in Example 1 except that an aluminum hydroxide powder having a purity of 99.99% or more and a cumulative 50% particle diameter (D50) on a volume basis of 8.3 ⁇ m was used. It was.
  • the composition ratio, particle size and purity of the spinel powder of Comparative Example 1 are shown in Table 1 below.
  • the contents and total contents of various elements in this spinel powder are shown in Table 2 below.
  • Example 1 a spinel powder having a purity of 99.95% by mass or more and an extremely low impurity content was obtained.
  • the contents of Ca and Si in this spinel powder were both less than 30 mm.
  • Comparative Example 1 the purity was less than 99.95% by mass, and the contents of Ca and Si were both 30 ppm or more. From this evaluation result, the superiority of the present invention is clear.
  • the spinel powder described above is suitably used in various fields where a high-purity ceramic sintered body is required.

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  • Compositions Of Oxide Ceramics (AREA)

Abstract

Poudre de spinelle ayant une pureté de 99,95 % en masse ou plus. Dans cette poudre de spinelle, la teneur en Mg en termes d'oxyde (MgO) est compris entre 9 à 78 % en masse et la teneur en Al en termes d'oxyde (Al2O3) est compris entre 22 à 91 % en masse. Un procédé de fabrication de cette poudre de spinelle comprend : une étape de mélange pour mélanger une source de magnésium, qui a une pureté de 99,95 % en masse ou plus, avec une source d'aluminium, qui a une pureté de 99,95 % en masse ou plus, pour obtenir une poudre mélangée; une étape de broyage pour broyer la poudre mélangée afin de donner un précurseur; et une étape de cuisson pour cuire le précurseur à une température de 1500°C ou moins.
PCT/JP2020/009766 2019-03-28 2020-03-06 Poudre de spinelle Ceased WO2020195721A1 (fr)

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CN113198471A (zh) * 2021-05-21 2021-08-03 晋中学院 一种甲醇重整制氢的铜铝尖晶石催化剂及其制法和应用
CN115582120A (zh) * 2022-09-16 2023-01-10 福州大学 一种助剂改性负载型Ru和/或Ni基催化剂的制备方法
JP2023120508A (ja) * 2022-02-18 2023-08-30 デンカ株式会社 粉末及び粉末の製造方法

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CN115582120B (zh) * 2022-09-16 2023-12-19 福州大学 一种助剂改性负载型Ru和/或Ni基催化剂的制备方法

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TW202102460A (zh) 2021-01-16
KR20210144777A (ko) 2021-11-30

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