JP2008280246A - Apparatus for manufacturing high purity magnesium oxide fine powder and method for manufacturing high purity magnesium oxide fine powder using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a technique for continuously manufacturing high purity magnesium oxide fine powder having a uniform particle diameter. <P>SOLUTION: An apparatus for manufacturing high purity magnesium oxide fine powder is a magnesium oxidation apparatus provided with a magnesium vapor jetting port at the bottom part, an oxygen-containing gas jetting port at the side face and a magnesium oxide fine powder take-out port at the upper part. The apparatus for manufacturing high purity magnesium oxide fine powder includes a magnesium oxidation apparatus which is provided with a window for observing the inside disposed at the side part and a grinding apparatus installed parallel to the bottom part and for grinding metal magnesium or a magnesium compound deposited on the magnesium vapor jetting port, or includes a magnesium oxidation apparatus which has a heater for heating the surroundings of the magnesium vapor jetting port and is installed on the bottom part. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a high-purity magnesium oxide fine powder production apparatus and a method for producing a high-purity magnesium oxide fine powder using this apparatus.

  A gas phase synthesis method is known as a method for producing a high-purity magnesium oxide fine powder. This vapor phase synthesis method is a method in which magnesium metal is heated to generate magnesium vapor, and this magnesium vapor and an oxygen-containing gas are brought into contact with each other to oxidize magnesium to produce magnesium oxide fine powder. .

  An apparatus for producing a magnesium oxide fine powder by a vapor phase synthesis method generally oxidizes magnesium by bringing a magnesium vapor generating apparatus that generates metallic magnesium vapor into contact with the magnesium vapor and an oxygen-containing gas. It consists of a magnesium oxidizer that produces magnesium oxide fine powder.

  As a magnesium vapor generating apparatus, a metal magnesium melting pot (also referred to as a melting pot) for heating and melting metal magnesium and a magnesium evaporation pot for heating and evaporating molten magnesium are heat-resistant pipes ( 2. Description of the Related Art A metal magnesium melting / evaporating apparatus connected by a connecting pipe is also known (see Patent Document 1).

  As a magnesium oxidation apparatus, a magnesium oxidation apparatus having a magnesium vapor injection port at the bottom and an oxygen-containing gas injection port at a side is known (see Patent Document 2).

JP-A-2-307822 JP-A-7-101722

It has been found that there are some problems when the present inventors actually produce magnesium oxide fine powder by using the above-described metal magnesium melting and vaporizing apparatus and magnesium oxidizing apparatus. One of them, when manufacturing magnesium oxide fine powder continuously over a long period of time, metal magnesium and magnesium compounds (eg magnesium oxide) adhere and deposit around the magnesium vapor injection port of the magnesium oxidizer. Since the amount of magnesium vapor introduced from the magnesium vapor injection port into the magnesium oxidizer is likely to fluctuate, there is a problem that the particle diameter of the obtained magnesium oxide fine powder may be non-uniform.
Accordingly, an object of the present invention is to provide a technique that makes it possible to continuously produce high-purity magnesium oxide fine powder having a uniform particle size.

  The present invention relates to a metal magnesium melting pot having a metal magnesium inlet at the top and a molten magnesium supply port at the bottom of the side, a heat resistant pipe connected to the molten magnesium supply port of the melting pot, and the heat resistant pipe The molten magnesium inlet is connected to the other end of the metal at the lower part of the side, and the upper part is a magnesium magnesium evaporating apparatus comprising a magnesium evaporating pot provided with a magnesium vapor outlet, and the magnesium of the evaporating pot at the bottom. It consists of a magnesium vapor injection port connected to the vapor blow-out port, an oxygen-containing gas injection port on the side surface, and a magnesium oxidation device with a magnesium oxide fine powder take-out port on the top. Metal magnesium with windows and parallel to the bottom of the magnesium vapor Or in the high-purity magnesium oxide fine powder production apparatus characterized by grinding apparatus scraping magnesium compound it is attached. A heater for heating the periphery of the magnesium vapor injection port may be attached to the bottom of the magnesium oxidizer.

  The present invention further uses the above-described high-purity magnesium oxide fine powder production apparatus to generate magnesium vapor in a metal magnesium melting and evaporating apparatus, and then in the magnesium oxidizing apparatus, the magnesium vapor is emitted from a magnesium vapor injection port into an oxygen-containing gas. Each of the oxygen-containing gases is injected from the injection port, and the magnesium vapor and the oxygen-containing gas are brought into contact with each other to produce fine magnesium oxide powder. While observing the periphery of the magnesium vapor injection port from the internal observation window, the magnesium vapor There is also a method for producing high-purity magnesium oxide fine powder, characterized in that metal magnesium or a magnesium compound deposited around the injection port is scraped off by a grinding device.

  The present invention also provides a metal magnesium melting pot having a metal magnesium inlet at the top and a molten magnesium supply port at the lower side, a heat resistant pipe connected to the molten magnesium supply port of the melting pot, and the heat resistance. A molten magnesium inlet that is connected to the other end of the pipe is provided at the lower part of the side, and a magnesium magnesium evaporating apparatus comprising a magnesium evaporating pot provided with a magnesium vapor outlet at the upper part, and the evaporating pot at the bottom. It consists of a magnesium vapor injection port connected to the magnesium vapor discharge port, an oxygen-containing gas injection port on the side surface, and a magnesium oxidation device with a magnesium oxide fine powder take-out port on the top. Magnesium vapor injection at the bottom of the magnesium oxidation device A high-purity acid characterized by a heater that heats around the mouth Some magnesium fine powder production apparatus.

  The present invention further uses the above-described high-purity magnesium oxide fine powder production apparatus to inject metal magnesium from the metal magnesium inlet of the metal magnesium melting evaporator, and to inject magnesium vapor from the magnesium vapor outlet of the magnesium oxide apparatus. In addition, by introducing the oxygen-containing gas from the oxygen-containing gas injection port of the magnesium oxidation apparatus, the magnesium vapor and the oxygen-containing gas are brought into contact with each other to generate magnesium oxide fine powder, and the magnesium vapor injection port of the magnesium oxidation apparatus There is also a method for producing a high-purity magnesium oxide fine powder characterized in that the surroundings are heated by a heater.

  By using the high-purity magnesium oxide fine powder production apparatus of the present invention, a high-purity magnesium oxide fine powder having a uniform particle diameter can be produced continuously over a long period of time.

  A high-purity magnesium oxide fine powder production apparatus and a high-purity magnesium oxide fine powder production method using the apparatus of the present invention will be described with reference to the accompanying drawings.

  FIG. 1 is a diagram showing an example of the configuration of a high-purity magnesium oxide fine powder production and recovery device using the high-purity magnesium oxide fine powder production device according to the present invention, and FIG. 2 shows the high-purity magnesium oxide fine powder of FIG. It is the figure which expanded the peripheral part of the magnesium vapor injection port of the magnesium oxidation apparatus which is the feature point of a manufacturing apparatus.

  In FIG. 1, a high purity magnesium oxide fine powder production and recovery device includes a high purity magnesium oxide fine powder production device comprising a metal magnesium melt evaporation device 10 and a magnesium oxidation device 26, a heat exchanger 41, a bag filter 42, and a hopper 43. And a high-purity magnesium oxide fine powder recovery device.

  The metallic magnesium melting / evaporating apparatus 10 includes a lid 13 having an inlet 11 for metallic magnesium and an inlet 12 for an antioxidant gas for preventing oxidation of metallic magnesium, and a molten magnesium outlet 14 at the lower side of the side. A metal magnesium melting pan 16 comprising a pan portion 15 provided, a heat-resistant pipe 17 connected to the molten magnesium outlet of the melting pan, and a molten magnesium inlet 18 connected to the other end of the heat-resistant pipe are provided on the lower side of the side. A magnesium evaporating pan 23 comprising a pan portion 19 provided with a lid portion 22 provided with a magnesium vapor outlet 20 and an inert gas inlet 21 for preventing magnesium metal from oxidizing and diluting magnesium vapor. It is configured.

  Use of sulfur hexafluoride gas, carbon dioxide gas, neon gas, argon gas, krypton gas, xenon gas, and radon gas as the antioxidant gas introduced into the melting pot from the antioxidant gas inlet 12 of the melting pot lid Can do. Among these gases, sulfur hexafluoride gas is particularly preferable. This antioxidant gas is always introduced into the melting pot when magnesium vapor is generated.

  Helium gas, neon gas, argon gas, krypton gas, xenon gas, and radon gas can be used as the inert gas introduced into the evaporation pot from the inert gas inlet 21 of the evaporation pot lid. Among these gases, argon gas is particularly preferable. This inert gas is always introduced into the evaporation pan when magnesium vapor is generated.

  Magnesium vapor is generated as follows. First, metal magnesium 24 as a raw material is charged into the melting pot 16 from the metal magnesium inlet 11, and the metal magnesium is heated to its melting temperature in the melting pot to obtain molten magnesium 25. The molten magnesium passes through the heat resistant pipe 17 and is stored in the evaporation pot 23. The molten magnesium 25 is further heated to a temperature equal to or higher than its boiling point in the evaporating pot 23 to generate magnesium vapor. This magnesium vapor is discharged from the magnesium vapor outlet 20 of the evaporation pot as a mixed gas with the inert gas introduced into the evaporation pot from the inert gas inlet 21.

  When magnesium vapor is generated continuously over a long period of time, impurities in metal magnesium (especially, high-boiling heavy metals such as iron, nickel, chromium, etc.) gradually accumulate in the evaporating pan, and impurities increase as the amount of accumulation increases. May be mixed with magnesium vapor, and the purity of the obtained fine powder of magnesium oxide may be reduced. For this reason, in the metal magnesium melting and evaporating apparatus of FIG. 1, the distance from the molten magnesium introduction port 18 of the evaporating pot 23 to the bottom is made longer than the distance from the molten magnesium take-out port to the bottom of the evaporating pot. By staying at the bottom side of the evaporating pan, the amount of impurities mixed into the magnesium vapor can be reduced over a long period of time.

  The magnesium oxidizer 26 has a magnesium vapor injection port 27 connected to the magnesium vapor outlet 20 of the evaporation pan at the bottom, an oxygen-containing gas injection port 28 on the side surface, and a magnesium oxide fine powder take-out port 29 on the top. Yes.

  The magnesium vapor injection port 27 is formed so that a mixed gas of magnesium vapor and an inert gas is injected vertically upward. The oxygen-containing gas injection port 28 is disposed so as to inject the oxygen-containing gas substantially perpendicular to the traveling direction of the mixed gas injected from the magnesium vapor injection port 27. The magnesium oxide fine powder outlet 29 is arranged vertically above the magnesium vapor injection port so that the produced magnesium oxide fine powder can be taken out on the flow of an inert gas introduced together with the magnesium vapor.

  As the oxygen-containing gas, air is usually used. However, the oxygen-containing gas is not limited to air. For example, oxygen can be used alone, and further, an inert gas (usually argon gas) is added to oxygen or air. It is also possible to do.

  The internal temperature of the magnesium oxidizer 26 (that is, the oxidation reaction temperature of magnesium) is preferably 1200 to 2000 ° C. However, since the oxidation reaction of magnesium is an exothermic reaction, the magnesium oxidation is accompanied with the production of the magnesium oxide fine powder. The internal temperature of the device tends to increase. Therefore, the periphery of the portion where the magnesium vapor and the oxygen-containing gas are in contact with each other is covered with a cooling outer pipe 32 having a cooling air inlet 30 and a cooling air outlet 31, and cooling air introduction By introducing cooling air from the mouth, the internal temperature of the magnesium oxidizer can be adjusted.

  In the magnesium oxidizer of FIG. 1, an internal observation window 33 is provided on the side, and a grinding device 34 for scraping off metallic magnesium or a magnesium compound deposited on the magnesium vapor injection port is provided in parallel with the bottom. The grinding device 34 is composed of an arm 36 having a grinding plate 35 at the tip, and a cylinder 37 for pulling the arm parallel to the bottom of the magnesium oxidation device. In the magnesium oxidation apparatus of FIG. 1, the internal observation window 33 and the grinding apparatus 34 are integrally incorporated in a hollow housing 38, but the internal observation window 33 and the grinding apparatus 34 There is no particular limitation on the arrangement.

  As shown in FIG. 2, the grinding device 34 scrapes off the metal magnesium or magnesium compound deposited around the magnesium vapor injection port 27 by the grinding plate 35 by pulling out the arm 36 in the direction of the arrow. The metallic magnesium and magnesium compound scraped off by the grinding device 34 can be taken out to the outside through an opening (cleaning window) 39 provided on the side of the magnesium oxidation device.

  The internal observation window 33 is a window for visually observing the deposition state of metallic magnesium or a magnesium compound around the magnesium vapor injection port 27. The operating speed of the arm 36 of the grinding device 34 is appropriately adjusted in consideration of the magnesium oxide deposition state observed in the internal observation window.

  In the magnesium oxidation apparatus of FIG. 1, magnesium vapor is injected from the magnesium vapor injection port 27, oxygen-containing gas is injected from the oxygen-containing gas injection port 28, and the magnesium vapor and the oxygen-containing gas are brought into contact with each other. 40, and the magnesium oxide deposited around the magnesium vapor injection port can be scraped off by the grinding device 34 while observing the periphery of the magnesium vapor injection port through the internal observation window 33. Accordingly, the amount of magnesium vapor introduced from the magnesium vapor injection port into the magnesium oxidizer is stabilized over a long period of time.

  The magnesium oxide fine powder 40 generated by the magnesium oxidation apparatus is sent to the heat exchanger 41 through the magnesium oxide fine powder take-out port 29. The magnesium oxide fine powder cooled by the heat exchanger 41 is collected by the bag filter 42 and temporarily stored in the hopper 43.

  Magnesium oxide fine powder produced by gas phase synthesis has high activity and may adsorb carbon dioxide and water vapor in the air when in contact with air. For this reason, it is preferable to re-fire the magnesium oxide fine powder stored in the hopper at a temperature of 500 to 1100 ° C. before shipment.

  FIG. 3 is a diagram showing another example of the configuration of a high-purity magnesium oxide fine powder production and recovery device using the high-purity magnesium oxide fine powder production device according to the present invention, and FIG. 4 is a diagram showing the high-purity magnesium oxide of FIG. It is the figure which expanded the peripheral part of the magnesium vapor injection port of the magnesium oxidation apparatus which is the feature point of a fine powder manufacturing apparatus.

  In FIG. 3, the high-purity magnesium oxide fine powder production and recovery apparatus includes a high-purity magnesium oxide fine powder production apparatus composed of a metal magnesium melt evaporation apparatus 10 and a magnesium oxidation apparatus 26, a heat exchanger 41, as in FIG. The high-purity magnesium oxide fine powder recovery device including the bag filter 42 and the hopper 43 is configured.

  Also in the high-purity magnesium oxide fine powder production apparatus of FIG. 3, the metal magnesium melting and evaporating apparatus 10 includes a lid provided with a metal magnesium inlet 11 and an antioxidant gas inlet 12 for preventing the metal magnesium from being oxidized. Part 13, a metal magnesium melting pot 16 comprising a pan part 15 provided with a molten magnesium outlet 14 at the lower side, a heat resistant pipe 17 connected to the molten magnesium outlet of the melting pot, and the other of the heat resistant pipes A pan portion 19 provided with a molten magnesium inlet 18 connected to the end portion at the lower side of the side, a magnesium vapor outlet 20 and an inert gas inlet 21 for preventing oxidation of metallic magnesium and diluting magnesium vapor It is comprised from the magnesium evaporating pot 23 which consists of the cover part 22 provided with.

  Also in the high purity magnesium oxide fine powder production apparatus of FIG. 3, the magnesium oxidation apparatus 26 includes a magnesium vapor injection port 27 connected to the magnesium vapor discharge port 20 of the evaporation pan at the bottom, and an oxygen-containing gas injection port 28 on the side surface. A magnesium oxide fine powder outlet 29 is provided at the top. The magnesium oxidizer of FIG. 3 is characterized in that a heater 44 is attached to the bottom thereof. As the heater 44, an induction heating type heater or a heating element type heater can be used.

  In the magnesium oxidizer of FIG. 3, magnesium vapor is injected from the magnesium vapor injection port 27 and oxygen-containing gas is injected from the oxygen-containing gas injection port 28, and the magnesium vapor and the oxygen-containing gas are brought into contact with each other. 40, and the surroundings of the magnesium vapor injection port 27 are heated by the heater 44 to a temperature not lower than the boiling point of the metal magnesium (preferably 1200 to 2000 ° C.), so that the metal magnesium or the magnesium compound is heated to the magnesium vapor injection port. It can be made difficult to adhere to the surroundings. Accordingly, the amount of magnesium vapor introduced from the magnesium vapor injection port into the magnesium oxidizer is stabilized over a long period of time.

  In the magnesium oxidizer shown in FIG. 3, the heater 44 is disposed so as to surround the magnesium vapor jet port as shown in FIG. 4, but the magnesium vapor jet port 27 of the magnesium oxidizer shown in FIG. A heater may be attached to the periphery of the steel plate so long as the operation of the grinding device 34 is not hindered, and the grinding of the deposit by the grinding device and the heating of the periphery of the magnesium vapor injection port by the heater may be performed simultaneously.

It is a figure which shows an example of a structure of the high purity magnesium oxide fine powder manufacture collection apparatus using the high purity magnesium oxide fine powder manufacturing apparatus according to this invention. It is the figure which expanded the peripheral part of the magnesium vapor injection port of the magnesium oxidation apparatus which is the feature point of the high purity magnesium oxide fine powder manufacturing apparatus of FIG. It is a figure which shows another example of a structure of the high purity magnesium oxide fine powder manufacture collection | recovery apparatus using the high purity magnesium oxide fine powder manufacturing apparatus according to this invention. It is the figure which expanded the peripheral part of the magnesium vapor injection port of the magnesium oxidation apparatus which is the feature point of the high purity magnesium oxide fine powder manufacturing apparatus of FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Metal magnesium fusion | evaporation apparatus 11 Metal magnesium inlet 12 Antioxidation gas inlet 13 Lid part 14 Molten magnesium outlet 15 Pot part 16 Molten pot 17 Heat resistant pipe 18 Molten magnesium inlet 19 Pot part 20 Magnesium vapor outlet 21 Not Active gas inlet 22 Lid portion 23 Evaporation pan 24 Metal magnesium 25 Molten magnesium 26 Magnesium oxidizer 27 Magnesium vapor jet 28 Oxygen-containing gas jet 29 Magnesium oxide fine powder outlet 30 Cooling air inlet 31 Cooling air exhaust 31 32 Cooling outer tube 33 Internal observation window 34 Grinding device 35 Grinding plate 36 Arm 37 Cylinder 38 Housing 39 Opening (cleaning window)
40 Magnesium oxide fine powder 41 Heat exchanger 42 Bag filter 43 Hopper 44 Heater

Claims (5)

  A metal magnesium melting pot having a metal magnesium inlet at the top and a molten magnesium outlet at the bottom of the side, a heat resistant pipe connected to the molten magnesium outlet of the melting pot, and the other end of the heat resistant pipe The molten magnesium inlet connected to the part is provided in the lower part of the side surface, the upper part is a magnesium magnesium melting evaporator comprising a magnesium evaporation pot provided with a magnesium vapor outlet, and the magnesium vapor outlet of the evaporation pot at the bottom. It consists of a magnesium vaporizer, a magnesium vaporizer that has an oxygen-containing gas jet on the side, and a magnesium oxide fine powder outlet on the top. The magnesium oxide has an internal observation window on the side. If the magnesium metal is deposited on the magnesium vapor jet, parallel to the bottom High purity magnesium oxide fine powder production apparatus characterized by grinding device scraping a compound of magnesium is attached is.   2. The high-purity magnesium oxide fine powder production apparatus according to claim 1, wherein a heater for heating the periphery of the magnesium vapor injection port is attached to the bottom of the magnesium oxidation apparatus.   Using the high-purity magnesium oxide fine powder production apparatus according to claim 1 or 2, magnesium vapor is generated by a metal magnesium melting evaporator, and then the magnesium vapor is oxygen-containing from a magnesium vapor injection port by the magnesium oxidation apparatus. Each of the oxygen-containing gases is injected from the gas injection port, and the magnesium vapor and the oxygen-containing gas are brought into contact with each other to produce a fine powder of magnesium oxide, and while observing the surroundings of the magnesium vapor injection port from the internal observation window, the magnesium A method for producing a high-purity magnesium oxide fine powder, characterized in that metal magnesium or a magnesium compound deposited around a steam injection port is scraped off by a grinding device.   A metal magnesium melting pot having a metal magnesium inlet at the top and a molten magnesium outlet at the bottom of the side, a heat resistant pipe connected to the molten magnesium outlet of the melting pot, and the other end of the heat resistant pipe The molten magnesium inlet is connected to the lower part of the side, and the upper part of the side is provided with a magnesium magnesium evaporating apparatus having a magnesium vapor outlet at the upper part, and the magnesium vapor outlet of the evaporating pot at the bottom. It consists of a magnesium vapor injection port connected to it, an oxygen-containing gas injection port on the side, and a magnesium oxide fine powder extraction port on the top. High-purity magnesium oxide characterized by having a heater for heating Beam fine powder production equipment.   5. The magnesium vapor is produced by a metal magnesium melting and evaporating apparatus using the high purity magnesium oxide fine powder producing apparatus according to claim 4, and then the magnesium vapor is injected into the magnesium vapor from a magnesium vapor injection port by the magnesium oxidizing apparatus. High-purity oxidation characterized by injecting oxygen-containing gas from the mouth, bringing magnesium vapor and oxygen-containing gas into contact to produce fine magnesium oxide powder, and heating the periphery of the magnesium vapor injection port with a heater Manufacturing method of magnesium fine powder.

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